LC–UV Method
Development for
Cannabinoid ProfilingèState-of-the-Art
Formulation Technology
in the Cannabis Industryè

A Guide to Reducing
Contamination and Eliminating
Error in the Laboratory

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Tips for

Reducing

Cultivation
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4

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Learn more at thermoﬁsher.com/cannabiscanada© 2018 Thermo Fisher Scientiﬁc Inc. All rights reserved. All trademarks are the property of Thermo Fisher Scientiﬁc and its subsidiaries
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6

Table of Con
ntentts

CANNABIS SCIENCE AND TECHNOLOGY|

VOL 1 • NO 4w w w.CannabisScienceTech.com

CANNABIS ANALYSIS

12 Error, Accuracy,
and Precision
Brian C. Smith
Find out if you know the difference
between accuracy and precision

CULTIVATION CLASSROOM

18

Curbing the
Cannabis Industry’s
Appetite for Energy
Roger Kern
A look at energy consumption in thecannabis industry and suggestions on
how cultivator’s can reduce those costs.

FEATURES

22

Setting the Standard:
Considerations When
Handling DEA-Exempt
Cannabinoid ReferenceStandard Preparations Used
for Potency Determination
Catharine E. Layton
and Andrew J. Aubin
Reference standard qualifications are
discussed and techniques for qualifying incoming reference standards aresuggested.

50

Rapid Screeningof Cannabinoids in
Edibles Using Thermal
Desorption-GC–MS

30

30 Leveraging Selectivity
and Efficiency to Takethe Strain Out of LC–UV
Method Development for
Cannabinoid Profiling
Justin Steimling
Here the LC–UV separation of 16 cannabinoids of interest was performed
while the potential impact from minor
cannabinoids and terpenes on reported potency values was monitored.

36 Certified Reference
Material Manufacturing
Challenges
Don Shelly
What to consider when creating or using certified reference materials

TUTORIALS

Rojin Belganeh and William Pipkin
A look at how TD-GC–MS analysis
eliminates conventional sample preparation regimes and can be used as agood rapid screening technique.

56

5
6 Major Engine of
Growth in the Cannabis
Industry: State of the Art
Formulation Technology
for Product Innovation andExpanded Applications
Andreas M. Papas
Which formulation choices will support safety, efficacy, stability, andconsumer acceptance

CANNABIS CROSSROADS

60

40

40

Holding Data to a
Higher Standard,Part II: When Every PeakCounts—A Practical Guide
to Reducing Contaminationand Eliminating Error in
the Analytical Laboratory
Patricia Atkins
In this guide, we look at the mostcommon sources of contaminationand error in an analytical process.

Professor Jack Henion
Shares Insights on Cannabis
Research, Academia, andthe Expanding Role ofMass Spectrometry
Joshua Crossney
Professor Jack Henion shares his insights on cannabis research, including challenges and opportunities inmoving cannabis science forward.

DEPARTMENTS

10 Caannabiss Newss Foocuus
on the cover:Canna Obscura/Shutterstock.com

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

62 Ap
pplication
n No
otes
63 Suupplier Prrofilees
VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

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ǖ ǘǗ-&"11"-1BSUT $POTVNBCMFTt"UMBOUJD"WF 3BMFJHI /$ttXXXQBMQBSUTDPN

8

Editorial Ad
dviso
ory Board

EDITORIAL ADVISORY BOARD MEMBERS
Susan Audino, S.A.Audino & Associates, LLC

Sandy Mangan, SPEX SamplePrep LLC

Bob Clifford, Shimadzu Scientific Instruments

David (Dedi) Meiri, Laboratory of Cancer
Biology and Cannabinoid Research,
Technion Israel Institute of Technology

Ashlee Gerardi, Restek Corporation
Jacklyn Green, Agate Biosciences
Zac Hildenbrand, Inform Environmental, LLC

Kevin Schug, Department of Chemistry &Biochemistry, The University of Texas at Arlington

Karan Kapoor, Avana Canada Inc.

Brian Smith, Big Sur Scientific

Autumn Karcey, Cultivo, Inc.

Katherine Stenerson, MilliporeSigma

Julie Kowalski, Trace Analytics

Cannabis Science and Technology’s Editorial Advisory Board is a group of distinguished individuals assembled
to help the publication fulfill its editorial mission to educate the legal cannabis industry about the science andtechnology of analytical testing and quality control. With recognized expertise in a wide range of areas, board
members perform various functions, such as suggesting authors and topics for coverage, reviewing manuscripts,
and providing the editor with general direction and feedback. We are indebted to these individuals for theircontributions to the publication and to the cannabis community as a whole.

CANNABIS
science and technology

Connect with us on Social Media
Join your colleagues in conversation and stay up-to-dateon breaking news, research, and trends associated with thelegal cannabis industry. “Like” and follow us on Facebook,
LinkedIn, Twitter, and Instagram today!
facebook.com/CannSciTech

linkedin.com/groups/12090641

twitter.com/CannabisSciTech

instagram.com/CannabisScienceTechnology

Andrei Verner/ Shutterstock.com

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Know
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www.hamiltoncompany.com/microlab600©2018 Hamilton Company. All rights reserved.

Cannabis Newss Focus

Cannabis Science and Technology
Announces Editorial Advisory Board
Cannabis Science and Technology is pleased to announce the launch of its editorial advisory board (EAB).
The distinguished members of the EAB will play a crucial role in defining the editorial direction and maintaining a high level of editorial quality and integrity.
The official charter of the advisory board for Cannabis Science and Technology is to support the publication in identifying the most significant developmentsin the cannabis science field, and in ensuring the relevance and technical accuracy of our content. In doing
this work, board members support our mission to educate the legal cannabis industry about the science andtechnology of analytical testing and quality control. We
are pleased to announce the following board members:• Susan Audino, S.A. Audino & Associates, LLC• Bob Clifford, Shimadzu Scientific Instruments• Ashlee Gerardi, Restek Corporation• Jacklyn Green, Agate Biosciences• Zac Hildenbrand, Inform Environmental, LLC• Karan Kapoor, Avana Canada Inc.
• Autumn Karcey, Cultivo, Inc.
• Julie Kowalski, Trace Analytics• Sandy Mangan, SPEX SamplePrep LLC• David (Dedi) Meiri, Laboratory of Cancer Biology
and Cannabinoid Research, Technion Israel
Institute of Technology• Kevin Schug, Department of Chemistry &Biochemistry, The University of Texas at Arlington• Brian Smith, Big Sur Scientific• Katherine Stenerson, MilliporeSigma
For more information about our esteemed board
members, please see the full announcement on our
website: www.cannabissciencetech.com/news/cannabis-science-and-technology-announces-editorial-advisory-board.

University of Connecticut toOffer Cannabis Horticulture Course
The University of Connecticut (UConn, Storrs, Connecticut) announced plans to offer a class on cannabis horticulture through the Department of Plant Science andLandscape Architecture (1).

The course will be called “Horticulture of Cannabis:
From Seed to Harvest” and will be taught by Gerald“Gerry” Berkowitz, a professor of plant science, and experts working in the cannabis industry today such as
CEOs from successful business operations, for example, licensed cannabis growing facilities in Connecticut
and cannabis testing laboratories.
According to UConn Today, the course will have afirm focus in horticulture, serving as a gateway to theentire cannabis industry. The introductory course will
be open to all UConn students, regardless of their major, and has no prerequisites for enrollment. In addition
to Berkowitz, expert guest lecturers will present on topics such as cannabis genetics, seed selection, soil andtissue testing, plant hormones, and laboratory testingof harvests.
Berkowitz currently has the ability to work with low
tetrahydrocannabinol (THC) hemp cannabis plants,
which will be used as examples for class demonstrations. As reported by UConn Today, the plants will begrown in concert with the course to provide students
with hands-on examples of the range of horticultural methods applied to cannabis, such as propagatingclones through cuttings, transplanting, training plants
to alter canopy and flower architecture, culling males,
pest management, and more. The course will be offered in the Spring 2019 semester (2).

References
1) https://today.uconn.edu/2018/10/cannabiscourse-responds-industry-need/#.

2) http://www.plantscience.uconn.edu/.

Cannabis Science Conference
Announces East Coast Show
The organizers of the Cannabis Science Conference
announced a new east coast show for 2019. Cannabis Science Conference East will take place April 8–10,
2019, at the Baltimore Convention Center in Baltimore,
Maryland. The flagship conference in Portland, Oregon will take place September 4–6, 2019.
Oral and poster abstracts are now being accepted for Cannabis Science Conference East. Please visit www.cannabisscienceconference.com for more information on both events.

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

TOTEMART/SHUTTERSTOCK.COM

10

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12

Cann
nabis Annaly
ysis

Error, Accuracy, and Precision
In the science of analytical chemistry, we quantitate things such as weights and concentrations. All ofthese measurements generate a number, but to truly understand the quality of data we have to know
the size of the error in the measurement. Well known measures of data quality include accuracy andprecision. Do you know the difference between these two metrics? Do you know how to quantitate
them? And how does all of this apply to cannabis analysis? Please read on to find out more.

Any time a quantity is measured, be it your weight on abathroom scale, the speedof light, or potency of a cannabisbud, there will be error involved in
the measurement. Sources of error include environmental changes,
power fluctuations, electronics, andgood old fashioned human error. Error exists because human beings are
not gods and thus cannot control all
the variables all the time for any given measurement (1). Two of the mostimportant types of noise are random
noise and systematic noise. Let’s discuss random noise first.
Random Noise
Random error is caused by variables we cannot control as mentioned
above. The sign of random error is
random, that is, it is equally probableto be positive or negative. This is why
measurements are often times expressed as X±y, where X represents
the value of the measurement andy represents the amount of error in
the measurement. Error is sometimes
called noise, and the quality of data
can be expressed as a signal-to-noise
ratio (SNR) defined in equation 1.
SNR = (Signal)/(Noise)[1]

The SNR concept is perhaps best illustrated using a cell phone call. In
this case, the volume of the caller’s

voice is the signal and the static in theconnection is the noise. If the volumeof the caller’s voice is large comparedto the static, the connection has agood SNR and you can clearly hear
what the other person is saying. Alternatively, if the static in the connection is high, and the caller’s voice canbarely be heard above it, the SNR of
the call is low and you will have trouble understanding what your caller issaying. Note that a high SNR phone
call, or any high SNR data, will carry a
lot of information. Whereas a low SNR
phone call or low SNR data will carryvery little information. This is why SNR
is a measure of data quality.
In analytical chemistry error is often seen as “fuzz” in the baseline ofchromatographic and spectroscopic
measurements. An example of this isseen in Figure 1.
Figure 1 shows noise measured by
a Fourier transform-infrared (FT-IR)
spectrometer. Since the sign of random noise is random, the baseline
fluctuates up and down randomly.
The size of these wiggles is a measureof the noise (2). Note in Figure 1 thatthe size of the noise varies with wavenumber, which is typical of any spectrum measured using light (electromagnetic radiation).
The big peak at 2350 cm -1 in Figure 1 is an artifact, which is a peakor signal in your data that is not fromthe sample. This peak is from the

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

presence of unwanted atmospheric carbon dioxide inside the instrument. If you see a CO2 peak in an FTIR spectrum that you measure, it isan artifact.
A measurement of a signal-tonoise ratio, of course, needs a signal.
In chromatography, spectroscopy,
and other analytical techniques thesignal is the magnitude of the measurement made. This is illustrated in
Figure 2.
The y-axis in Figure 2 is in absorbance units (AU), which is a measure of the amount of light absorbed
by a sample. The size of the peakat 461 cm-1 in this case is the signal,
which has a magnitude of 0.0215 AU.
A measure of the error in a signal iscalled the peak-to-peak noise (PPN).
In Figure 2, this is calculated by taking a section of the baseline and taking the highest noise point, in thiscase 0.01388 AU, subtracting fromit the lowest noise point, which is
0.001144 AU, and obtaining a PPN of
0.00244 AU. The signal-to-noise ratiois then (0.0215) AU/(0.00244) AU for avalue of ~9. This is not a particularly
good SNR. Many laboratories measure what they call a limit of detection(LOD), which is typically calculated
as 3x the noise in a measurement oran SNR of 3. By calculating an LOD alaboratory is saying, “this is the minimum signal I can reliably measure.”
Many cannabis laboratory pesticide

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

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Cannnabis An
naly
ysis

14

the better SNR. Random error cannot be eliminated, but it can be minimized by controlling error sources
and averaging data.

100.4% Transmittance

100.2

100

99.8

99.6

99.4
3500

2000

2500

3000

1500

1000

500

Wavenumber (cm-1)

Figure 1: An example of noise in an infrared spectrum, seen as the random wiggles or“fuzz” in the baseline.

.022

.02

AbsorbancePeak-to-peak noise @440–420 cm-1
(0.01388 – 0.01144) =0.00244

Peak height(signal) = 0.0215@461 cm-1

.018

.016

.014

.012

500

480

460

Wavenumber (cm-1)

440

420

Figure 2: Measurement of a signal-to-noise ratio. In this case, the size of the peak is thesignal and the size of the random fluctuations in the baseline are the noise.

Systematic Error
Systematic error occurs when ameasurement is consistently wrong
by the same amount and in the same
direction. A classic example of systematic error is a clock that has been
not been set ahead for daylight savings time. This clock will always be
1 h behind whenever you look at it.
It is an example of systematic error
because it is always off by the sameamount, 1 h and in the same direction, always behind.
To detect systematic error, onemust have a true or reference value
with which to compare your observation. In the United States the reference time value is supplied by theatomic clock at the National Instituteof Standards and Technology (NIST)
in Gaithersburg, Maryland (3). Unlike
random error, systematic error can beeliminated, in this case by simply setting the clock forward 1 h.

above the limit of detection but below the limit of quantitation.
Random noise can be reduced byobserving the same quantity multiple
times and then averaging those readings. The SNR improves as the squareroot of the number of observations,N, averaged as such:
SNR ∝ (N)1/2[2]

where N is the number of observations averaged.
In essence, equation 2 works because random noise cancels itself as
N increases. Equation 2 is why we prefer to measure an average instead ofa single observation, the average has

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

Accuracy and precision are terms incommon use, and they are commonly confused. Some people seem tothink they are the same thing. They
are not. Precision is a measure of thescatter in a set of measurements. Accuracy is a measure of how far away a
set of measurements is from the true
values. This is illustrated in Figure 3.
Imagine you are tasked with weighing a 1.0 g standard weight on thesame scale seven times. Because oferror you will not get the same reading each time, but a spread of values. This is illustrated to the left in
Figure 3. The bullseye represents
the known value, 1.0 g, and the seven dots represent the seven readings

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

BLABLO101/SHUTTERSTOCK.COM

Accuracy and Precision
analysis reports, for example, contain an LOD that gives the minimum
amount of a pesticide whose presence can be reliably confirmed.
However, signals at or just above
the LOD are too noisy to give reliable quantitative results. So, many laboratories use a limit of quantitation(LOQ) of 10x the noise level or an SNRof 10. By calculating an LOQ a laboratory is saying, “this is the minimum
amount of signal with which I can givea reliable quantitative measure.” The
LOQ in a pesticide report from a cannabis analysis laboratory tells you theminimum amount of pesticide thatcan be reliably quantitated in a sample. Thus, the SNR of 9 in Figure 2 isCannabiis An
naly
ysis

you obtained. These readings are arandom scatter and they are not particularly close to the bullseye; thisdata set is imprecise because thereadings are widely scattered andnot reproducible. This data is inaccurate because of how far on average
the readings are from the bullseye,the true value. If your seven readings
are about the same value, let’s say
1.9 g, they would form the plot seenin the middle of Figure 3. The readings form a tight cluster in the upper right hand corner of the bullseye,but their center is far from the true
value of 1.0 in the center. This dataset is said to be precise but inaccurate. It is precise because the scatter in the data is small and the points
cluster tightly together. Precision is ameasure of the amount of random error in a dataset. It is found by measuring the same value on the same sample multiple times. Imprecise data
will give a wide scatter, like to the left
in Figure 3. Precise data will be tightly clustered as seen in the middle of
Figure 3. However, this data is clustered around 1.9 g, far away from thetrue value of 1.0 at the center of thebullseye. Thus, this data set is inaccurate because the points fall far fromthe true value. Precision is a usefulmeasure of data quality since it quantitates random error, but it ignores
systematic error so it is not a complete picture. The systematic error in
the middle of Figure 3 is the distance
between the center of the data cluster and the bullseye.
Accuracy is a measure of theamount of random and systematic error in a data set. If the seven weights
you measure all cluster tightly around
1.0 g, the diagram at the right in Figure
3 will be obtained. This data is precise
because the spread of the readings issmall, and it is accurate because thepoints cluster tightly around the true

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

value. This is the ideal situation. Accuracy is a better measure of data quality than precision since it incorporates
both random and systematic error.
Now, if one does not have a trueor reference value to compare to,15

let’s say you lose your 1.0 g standard
weight, repeated measurements onsome other sample can be made toobtain a precision value. For example, you might want take a pencil andmeasure its weight seven times. The

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naly
ysis

Imprecise andinaccurate

Precise andinaccurate

Precise andaccurate

Figure 3: An illustration of the concepts of accuracy and precision using bullseyes.

spread of these values will give you the precision of thebalance. This is not as good as an accuracy determination, but since we do not have a standard weight, and we
do not know the true weight of the pencil, the precision
is the best we can do. When reporting error size in theliterature, always make sure to disclose whether you arereporting an accuracy or a precision, and for an accuracy result always clearly state the source of the true value
used in the calculations.

Is True Accuracy Achievable in the
Cannabis Industry Right Now?
As mentioned above, obtaining an accuracy calculation
requires a sample with a known value to be measured.
For many industries, where plant material is processedsuch as tea, there exist NIST traceable standard reference materials (SRMs). For example, there exist SRMs fortea and tea extracts that can be used to give reference
values for accuracy calculations (4). Since cannabis is notlegal at the federal level in the United States, NIST, beinga Federal agency, cannot develop cannabis SRMs for anyof the materials that cannabis laboratories test. This has
left the industry in the difficult position of having to develop its own standards and analytical methods.
Now, for chromatographic methods there are purecannabinoid standards that can be used for calibration.
However, since there are no SRMs available for the actual types of samples analyzed, such as cannabis buds andextracts, the effect of sample preparation on the final
results is not reflected in the accuracy calculations performed. Thus, I have to conclude, perhaps controversially, that in the absence of the proper SRMs, true accuracy measurements in the cannabis analysis industry may
not be possible.
This issue is reflected in the problem of inter-laboratory variation. This has been documented before and continues to be an issue (5,6). In my view, part of the problem is the lack of industry standard methods for cannabis

analysis. Because of the lack of this guidance, laboratories have had to fend for themselves to develop their own
methods. Thus, different laboratories have developed
different ways of doing things, and this leads to different
results. In particular, I have observed that many laboratories prepare samples in completely different ways, leading to variations in the results obtained.
All of this is not to say that cannabis laboratories are
not precise, they are. They can get impressively reproducible data on a given sample. But until SRMs andstandard methods are available, the search for a true accuracy and a solution to the inter-laboratory variation issue will, I believe, be problematic. In the meantime, it
might be best for cannabis businesses to find a laboratory they trust, submit their samples to them, and only compare numbers from this chosen laboratory to themselves
going forward.
References
1) B.C. Smith, Quantitative Spectroscopy: Theory andPractice, (Elsevier, Boston, Massachusetts, 2002).
2) B.C. Smith, Fundamentals of Fourier Transform Infrared
Spectroscopy, (CRC Press, Boca Raton, Florida, 2011).
3) www.time.gov.
4) www.nist.gov.
5) M.O. Bonn-Miller, M.J.E. Loflin, B.F. Thomas,
J.P. Marcu, T. Hyke, and R. Vandrey, JAMA,
J. Am. Med. Assoc. 318, 1708 (2017).
6) B. Smith, P. Lessard, and R. Pearson,
manuscript in preparation.

About the Columnist
Brian C. Smith, PhD,
is Founder, CEO, and Chief Technical Officer of
Big Sur Scientific in Capitola, California. Dr. Smith
has more than 40 years of experience as an industrial analytical chemist having worked for suchcompanies as Xerox, IBM, Waters Associates,
and Princeton Instruments. For 20 years he ran Spectros
Associates, an analytical chemistry training and consulting
firm where he taught thousands of people around the world
how to improve their chemical analyses. Dr. Smith has written
three books on infrared spectroscopy, and earned his PhD inphysical chemistry from Dartmouth College.

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

BLABLO101/SHUTTERSTOCK.COM

16

18

Cultivationn Cla
assroom

Curbing the Cannabis Industry’s
Appetite for Energy
Cannabis cultivation has a problem, a big problem: the electric bill! Earlier in my cannabis career, I
heard growers complain about the cost of electricity eating into their profits—but now the situation
is much worse, while the stakes are far greater. Energy consumption is under greater scrutiny thanever by regulators because of concerns over fossil fuels hastening climate change and the cost of
expanding the grid. This means the cannabis industry better find solutions to cut down on its poweruse, or else the government will—and no one wants that.
Roger KernJ

ust how bad is the energy problem in the cannabis industry? Energy inputs are estimated by several studies to be perhaps as much as half of total indoor cannabis cultivation costs. Based on this estimate, let’s assume
2000 kW/h per pound of medicine and a typical energy costof $0.24 (1). For growing a single pound of cannabis, that’s$480 worth of energy! And just what is this energy used for?
It’s not just lighting; also sucking up power are air conditioners
and chillers, dehumidifiers, carbon and high-efficiency particulate air (HEPA) filters, fans, and system controllers. In a 2016
study done for investor-owned San Diego Gas & Electric, Evergreen Economics broke down the energy consumption forindoor cannabis production and found that lighting accounts
for 38% of the energy consumed, venting 30%, and air conditioning 21% (2). Furthermore, when one considers the current
means of energy production, the cultivation of 1 kg of cannabis results in the production of 4600 kg of carbon dioxide.
Clearly, there is plenty of room for improvement and, just
as fortunately, there are many ways to improve. For now, let’s
just talk about two: the cultivation structure and how it is illuminated. According to BOTEC Analysis, indoor cultivation
has the highest energy consumption levels with 4400 kWh,
6100 KWh/kg. Greenhouses have much lower energy demands with 6 kWh, 580 kWh/kg (3). (BOTEC’s study considers the energy consumption of outdoor cultivation to be minimal.) This is why I recommend to cultivators that they start
their site and structure selection process by giving serious
consideration to a greenhouse.
In California, my home state, the Department of Agriculture has projected the following trends: There will be a shift inproduction from the northern to the southern part of the state
while the use of controlled-environment agriculture (CEA) is
forecast to jump dramatically over 2–3 years from 16% to morethan 50% (4). I expect there will always be indoor, greenhouse,
and outdoor production, and there are advantages to all thesemethods. Still, I would like to see the percentage of greenhousefacilities increase for the reduction of energy use while still enabling a controlled environment for maximum yield and quality.

Light emitting diodes (LEDs) are finding their way into more
and more grows, despite skepticism by cultivators. Most of
the controversy centers around sufficient power during theflowering phase and the nonsolar nature of the spectrum.
Both concerns are not issues in the greenhouse, where LEDsserve to augment the solar spectrum during off-peak times ofsolar illumination such as early morning, late afternoon, wintermonths, and cloudy days. However, the energy benefits are realand substantial: Most manufacturers claim that their 600-W
fixture can replace a 1000-W high-intensity fixture, resulting
in a 40% reduction in lighting costs. This efficiency is further
compounded by energy savings associated with cooling because of the heat produced from lighting; therefore, thesepractices are being adopted by CEA vegetable growers on a
global scale. The reason is simple: LEDs save money by savingenergy in the CEA setting while increasing yield and quality.
As the acceptance of cannabis spreads across the nation
and world, it’s logical to assume more will be grown, which,of course, means an increasing demand for electricity. The industry would be wise to demonstrate its responsibility by acting now to cut back on power consumption. Because if cultivators don’t, strangers may be more than willing to act forthem—and when they do, they may not have the industry’s
wellbeing in mind.

An Expert’s Point of View
When looking for solutions to the cannabis industry’s high energy consumption, it’s necessary to have experts who are familiar with both cultivation and how utilities can help growers. Dan Duran has that knowledge, having worked for powercompanies and, as a professor, having researched cultivators’
use of power. Dan spoke with Cannabis Science and Technology magazine to share how the two sides can work together.
What has been your background and experience withthe cannabis sector?
Dan Duran: I am a veteran of 25 years in the corporate world,
where I led operations and marketing teams in the IT and

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VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Cultivation Classrooomenergy sectors, including stints with American Telephone
and Telegraph, Nippon Electric Corp., Southern California
Edison, and Sempra Energy. I decided, after the tragic eventson September 11, to move into academia and have been afaculty member at a California liberal arts college since then.
At Whittier College, I study domestic and international sustainable development with a focus on energy and renewable
resource management. I founded Energized Solutions, LLC,
in 2002 with the goal to provide real-world data and researchpertaining to sustainable development and renewable resource management to be used in and out of the classroom.
Dr. Cinzia Fissore, who joined Energized Solutions a few years
ago, and I have planned and executed several field-based
research projects pertaining to agriculture for the California Public Utilities Commission (CPUC) and California-based
electric, natural gas, and water utilities. We have conducted more than 200 field visits with a broad spectrum of growers, from row crops to dairy, nuts, and vineyards. Our goal is
to better understand current practices, help the utilities andother stakeholders learn more about their customers, anddevelop and deliver programs to improve energy–water efficiency and other sustainability-focused programs and technical services. Over the last few years, we have tightened our
focus on the urban agriculture sector and more specificallyon CEA and greenhouse operations, especially the growth inSouthern California.
You mentioned your energy–water work with utilities
and the agriculture sector. What are the utilities
thinking and doing with respect to the legalized andfast-growing cannabis business in California, andspecifically with the increasing focus on CEA andgreenhouse production by growers?
Duran: The good news is that a few utilities have recognized
the need and opportunity to work with CEA and greenhouse
growers, including those in urban areas. The case is that the
majority of the utilities have opted to take a “wait and see”
position. As a veteran manager of several utilities, the reality
is that utilities are far more risk-adverse than other firms in theprivate or public arena, and while most of them highlight theircommitment to serving customer needs, their primary goal
is to protect investors by heeding to the dictates and regulations of the CPUC or equivalent oversight agency. For example, while the major utilities in California have dedicatedagriculture account executives or service representatives thatwork with the large growers and post-harvest processors thathave significant energy and water needs, the unfortunate caseis that they rarely, if ever, interact, and know very little about
the needs of CEA and greenhouse growers. Another factor isthat many of those growers have operated in a “gray” area toelude the detection by utilities and most often take the “fast”
in–out operations way rather than a systems approach. I have
VOL 1 • NO 4 • NOVEMBER/DECEMBER 201819

spoken to several of the utilities and the large consulting firmsthat help them with strategic planning and program evaluation, and while there are a few field people who recognize
the need to learn and support growers, the senior management teams have almost consistently chosen to take limited
initiatives. This is not a good situation, as the growing number and size of CEA and greenhouse growers need to better
understand and take advantage of “Time of Use rates,” energy-efficiency programs and incentives, service planning infrastructure support, technical training on current and innovative technologies, and a broad spectrum of other services
and support provided to the traditional medium to big users.
Utilities increasingly want to be perceived as being environmentally responsible with strong corporate social responsibility agendas, but in this case, they have largely missed the opportunity to acknowledge the emergence of this new base ofcustomers that are producing a high-value crop with significant social and economic benefits.
What should current and hopeful growers expect fromthe utilities and what is the most effective approach touse in securing technical and financial support from them?
Duran: Utilities are typically organized by function, such as
distribution, energy–water efficiency, service planning, customer education, regulatory, and public relations. My firstpiece of advice is to do a bit of internet leg work and determine where the agriculture support team is situated and tocontact the local account executive or service representative.
While most of the utility agriculture teams are located in the
traditional rural locales, they are the most likely to respondto a request for information on services. Growers should also
identify the local or regional public affairs or equivalent representative because they are the most attuned to listening tousers and their professional association advocates. The public affairs folks are charged to be the face of the utility to the
local community and the local power structure, and they are
responsible for articulating problems and opportunities totheir utility management organization. While most of the midto larger utilities run education and training programs on efficiency strategies and new product offerings, they have yet
to develop and offer programs customized to the needs of
the CEA or greenhouse cannabis grower. With the exception of the recent 2017 Grower Report prepared by the Cannabis Conservancy for the Colorado Energy Office (5), there
is a lack of solid and current data on the energy spends andefficiency levels of different energy-intensive (for example,
lighting, heating, ventilation, and air conditioning [HVAC], andCO2 generation) and water-operating modes used for outdoor and indoor operations. Still, it is commonly stated andbelieved that the energy spend constitutes between 30–45%
of CEA-greenhouse grower operations. There is a real lack ofunderstanding regarding which specific energy-use areas can

www.CannabisScienceTech.com|

CANNABIS SCIENCE AND TECHNOLOGY

20

Cultivationn Cla
assroombe best addressed via more energy-efficient technologies
and what their impact is on the bottom line.
What should utilities put on their agenda to prepare andsupport the CEA-greenhouse growers?
Duran: The cannabis growers market has several key stakeholders, and the local energy, water, and waste utilities all
have important roles to play in helping this industry mature
with respect to energy efficiency, water management, andwaste practices. At the moment, I am in conversation with several Southern California utilities about how best to prepare
and support the CEA and greenhouse growers. The most important step is for the utilities to prepare and execute a datagathering plan that identifies and records the current energy, water, and waste practices—what we call a baseline study.
Utilities need to figure out where the near-future CEA-greenhouse growth will be with respect to their distribution systems, including both the electric and water distribution grids.
Electric utilities tend to be “grid-focused,” and it is critical thatthey understand where the electric load will grow and how tobest support it. The corollary need is for utilities to identify andwork with the growers to provide a spectrum of services andsupport, from infrastructure service planning to information
on how demand charges are calculated, the available time ofuse and other rate options, and the incentives and rebates for
current and innovative technologies, including LED and virtual management systems. I believe that utilities will be motivated to respond to the growers who can provide data on plantcycle growing needs, energy consumption by equipment andsystem, and operations practices. My hope is that the sustainably and profit-focused CEA sector and greenhouse growers
will work with the utilities, equipment and tech providers, andconsultants to plan and implement a triple bottom line strategy that generates value and simultaneously benefits people,
the planet, and profits. It is my impression that utilities are very
motivated to work with other sectors to promote leadershipin efficiency and design (LEED) buildings and facilities that areboth energy efficient and operationally advanced. My “call”
to growers is to work with their local utilities (gas, electric, water, and waste), equipment and technology providers, and experienced consultants to lay the foundation for LEED growing
operations that produce quality products using environmentally-responsible growing operations that increase bottomline profits and generate value for both consumers and thecities and counties in which they operate.

Conclusion
We are entering a new era of cooperation and coordination
between the cannabis industry and the public utilities. Reducing energy consumption and adopting more sustainable
practices should become a high priority for cultivators. This
will show the public and the utility companies that cannabis

cultivators have a strong commitment to the environment,
while still making a profit. This approach will generate a positive relationship with the utilities, create goodwill in the public eye, and demonstrate that cannabis cultivation is on the
cutting edge of sustainability. By being innovative in cultivation practices and becoming leaders in lowering energy usage, cannabis cultivators will show the world that they are excellent stewards of our natural resources and good partners
with public utilities.

References
1) J.P. Caulkins, “Estimated Cost of Production for Legalized
Cannabis” (RAND Drug Policy Research Center, 2012).
2) Evergreen Economics, “SDG&E Cannabis
Agriculture Energy Demand Study” (Prepared for
San Diego Gas & Electric Company, 2016).
3) M. O’Hare, D. Sanchez, and P. Alstone, “Environmental
Risks and Opportunities in Cannabis Cultivation” (BOTEC
Analysis Corporation internal publication, June 2013).
4) J. Remillard and N. Collins, “Trends and Observations ofEnergy Use in the Cannabis Industry” (ACEEE Summer
Study on Energy Efficiency in Industry, 2017).
5) Colorado Energy Office, “Energy Use in the
Colorado Cannabis Industry” (Fall 2018).

ABOUT THE INTERVIEWEEDr. Dan Duranis an Associate Professor at Whittier College where
he teaches sustainable development. He is also thefounder and principal of Energized Solutions, LLC, a
CPUC-certified minority-owned business (MBE). His
career includes senior planning and operations workwith energy utilities and water agencies. His ongoing researchand consulting focus is in the energy–water nexus, especially with
the California agriculture community. He has met with hundredsof agriculture producers to identify their sustainability and bestpractices, and he works with utilities to optimize the potential for
CEA cannabis production.

ABOUT THE GUEST COLUMNISTDr. Roger Kern
is a scientist and technologist who cares deeply
about the cultivation and health of plants in thecannabis industry. With his PhD in microbiology
from the University of California, Davis, Plant
Growth Laboratory, he solves the most challenging problems in hydroponics, from studying the root microbiome to developing nutrients and lighting systems to ensure
plant health and a disease-free lifecycle. He spent 22 years at
NASA’s Jet Propulsion Laboratory as a scientist, technologist,
and research leader before becoming the President of Agate
Biosciences, a consulting firm for project management, systems engineering, and science in CEA for the past eight years.
He leads developments to optimize sustainability, consistency, quality, and yield without compromising plant health.
Direct correspondence to: rkern@agatebiosciences.com

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VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

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22

FeatureSetting the Standard:
Considerations When Handling
DEA-Exempt Cannabinoid ReferenceStandard Preparations Used for
Potency Determination
With the growth of the cannabis market, significant investments have been made into the setup,
operation, and maintenance of cannabinoid potency testing laboratories. Results generated inthese laboratories are not only dependent upon the accuracy of the testing methods and sample
preparation, but on the quality of the reference standards from which batches of cannabis samples
are directly quantified. The quality, consistency, and reliability of reference standard solutions are not
only a priority for manufacturers, but it is in the best interest of testing laboratories to protect andmaintain the integrity of these formulations during use and storage. In this manuscript, reference
standard qualifications are discussed and techniques for qualifying incoming reference standards
are suggested. Additionally, in-laboratory handling of reference solutions is explored to promote
and preserve accuracy of the formulations during use.
Catharine E. Layton and Andrew J. Aubin

C

urrently in the United States,
cannabinoid isolates are classified as Schedule I controlled
substances under the Controlled
Substance Act (CSA) Title 21 Code ofFederal Regulations (CFR) Parts 1300
to 1308. The distribution of these isolates is controlled and monitored by
the Drug Enforcement Administration (DEA) division of the U.S. Department of Justice (1). Purchasing
and use of controlled substances
must adhere to the requirements of
the Controlled Substance Act andany state enforcement agency, as
well as the terms and conditions of
any Institutional Research or Analytical Licenses or Registrations issuedin accordance with proposed laboratory activities. Sanctioned DEA-exemptions are granted for cannabinoid preparations after approval by
the DEA and Local State Codes toregistered manufacturers that supply these solutions for laboratory or
scientific research purposes (2).

A reference standard is broadly described by the U.S. Food andDrug Administration (FDA) and U.S.
Pharmacopeia (USP) as a well characterized, highly purified compound that serves as a specimen or
performance calibrator from which
drug substances, excipients, impurities, degradation products, orcompendial reagents are identified
and quantified for purity and potency. Any material can be called a“reference standard,” but the degree to which that material is characterized defines if the reference
standard is an acceptable calibrator for the intended application.
Simply because DEA sanctions
have been provided to a particular reference standard manufacturer, it does not automatically ensurethat the reference standards produced by that manufacturer meetthe quality and reliability specifications for laboratories testing cannabis samples for potency.

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

Certified cannabis testing laboratories operate under International Organization for Standardization(ISO) and International Electrotechnical Commission (IEC) 17025 accreditations issued by the American Association for Laboratory Accreditation(A2LA) to provide confidence that results generated in these testing laboratories are high quality and consistent. Reference standards usedby these laboratories are held to thesame ISO quality standard, in addition to ISO 17034:2016, which focuses
specifically on an evaluation of process uncertainty. This value is associated with manufacturing as a whole,and is reported along with orthogonal testing results, in the reference
standard traceable documentation(certificate of analysis [CoA]) provided as per ISO 9001:2015. These ISO
accreditations offer a foundation of
integrity when selecting a manufactured cannabinoid reference standard material supplier.

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

PRO Scientific Inc. | Oxford, CT 06478 | 203.267.4600

Feature

24

0.018

0.018

CBD

0.016

0.014

Absorbance (AU)

0.012

0.012

0.010

0.010

0.008

0.008

0.006

0.006

0.004

0.004

0.002

0.002

0.000

0.000

0.50

Δ9 THC

0.016

0.014

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

Time (min)

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

Time (min)Figure 1: Overlay of DEA-nonexempt CBD and ∆9-THC isolate starting materials (black)with DEA-exempt ampouled reference standards from three manufacturers (green, red,blue) when separated using a validated chromatographic testing method for assay.

Evaluation of Incoming
Reference Standards
Accurate determination of chromatographic purity depends upon
the ability of an analytical method
to resolve the analyte from closely eluted impurities. Since cannabis testing methods have yet to
be standardized within the industry, the ability of chromatographic methods to separate the reference standard peak of interest fromthe impurities may not be consistent between laboratories. Becauseof this lack of standardization, chromatographic assay results determined for the reference standard
solution in a sample testing laboratory may be different than the chromatographic assay value (mg/mL)
reported in the CoA.
To demonstrate, three certified
DEA-exempt ampouled cannabidiol (CBD) and ∆9 -THC reference
standards formulated in methanol(1.0 mg/mL) were purchased fromdifferent certified manufacturers(sources withheld). The chromatographic profiles of the CBD and ∆9 THC DEA-nonexempt isolate starting materials were compared to
DEA-exempt ampouled reference

standards using the same chromatographic platform (Figure 1) (3).
The CBD, ∆9-THC isolate starting materials, and the ampouled reference standards were confirmed
to be spectrally pure by ultraviolet-photodiode array (UV-PDA) detection, and the mass was confirmed by mass spectrometry (MS)using the in-house validated chromatographic method. From the linear response of a CBD isolate reference standard, the concentrationof CBD in the DEA-exempt ampouled preparations was calculated
and compared to the CoA. Concentrations of CBD were 1.013 mg/mL,
1.001 mg/mL, and 1.001 mg/mL. All
values were within the concentration range specified by the manufacturer CoA at 1.002 ± 0.011 mg/mL,
1.002 ± 0.006 mg/mL, and 1.000 ±0.005 mg/mL, respectively. Fromthe concentration values, it was concluded that although the references
standard solutions contained different impurities, the in-house validated method provided a comparable
chromatographic separation of CBDfrom the impurities when comparedto the chromatographic assay method used to prepare the CoA.

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

Only two out of the three ∆9-THC
DEA-exempt ampouled formulations were within the concentration
range reported on the respective
CoA when compared to the linear regression of the ∆9-THC isolate. The
UV-PDA spectral purity and MS response for ∆9-THC in the formulationand the isolate were comparable. The
reference standard formulation thatlies outside the CoA concentration
range does not immediately imply
that the manufacturer provided an inaccurate reference standard concentration assessment. It is a reminderthat qualification of an incoming reference standard should not be madebased upon a single testing result. In
this study, results were generated for
only one reference standard vial. It is
recommended that replicate vials areanalyzed from the same lot, and that
conclusions are made based on anaverage concentration determinationand standard deviation value for theincoming lot.
Alternatively, an evaluation of acceptability can also be made bycomparing the average response
factor (RF) (equation 1) of the incoming reference standard to the RF observed in the historical data for previous reference standards of the same
analyte. This approach requires thatcannabis testing laboratories compile average RF and concentration
information over time for incoming
lots, and define acceptable incoming
RF tolerance limits. With this technique, it is important to use the same
chromatographic separation method, confirmed to be consistent androbust over time by fulfilling method
system suitability criteria (that is, recovery and resolution).
Equation 1 shows the average response factor (RF):Peak area (μV * s)RF =Concentration (

mg
)
mL

[1]

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Big Sur Scientific
Bringing Science to the Art of Cannabis

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26

Feature(a)(b)

3.5E+06

4.0E+06y = 3e6x + 5.44e5
R2 = 0.8763

3.0E+06y = 3e6x + 1.46e4
R2 = 0.9999

3.5E+06

3.0E+06

3.5E+06

2.5E+06
2.0E+06
2.0E+06
1.5E+06
1.5E+06
1.0E+06
1.0E+06
5.0E+05

5.0E+05

0.0E+00

0.0E+00
0

0.2

0.4

0.6

0.8

1

1.2

0

0.2

0.4

0.6

0.8

1

1.2

Figure 2: DEA-exempt CBD reference material standard curves generated using(a) air-displacement and (b) glass volumetric or positive-displacement pipettes. Replicate
curves were prepared by multiple analysts to confirm linear regression trends.

Preparation of ReferenceStandards for Sample Testing
In the testing laboratory, reference
standards and sample solutions often
require dilution of the initial stock solution to prepare a working standard.
When working with solvent-based solutions such as cannabinoid formulations, it is important to select a pipette that will maintain accuracy. In
this study, cannabinoid DEA-exempt
and isolate reference standards wereprepared via serial dilution using volumetric pipetting devices common
in testing laboratories. Calibration
curves for CBD and ∆9-THC were prepared using a glass volumetric pipette, an air interface pipette, anda positive-displacement syringe pipette using a 1.0-mg/mL cannabinoid reference standard formulation.
Practical precautions were used toreduce error, such as using calibrated pipettes, prewetting the pipette
tip with sample solution, working at
a constant temperature, pipetting ina fully upright position, and avoiding
transfer of the solution on the outsideof the pipette tip to the collection
vessel. The standard curves for linear
regression were prepared to show theaccuracy of each pipetting method.

Figure 2a exhibits the standard
curve generated for DEA-exempt
CBD reference standard using the
air interface pipette. Although several of the data points in the serial dilution sequence appear to follow a
linear trend, the curve was not linear
by statistical regression analysis (R2 =0.8763). There is no justification to exclude the data points that do not statistically conform to the linear regression line (y = mx + b). The results werereplicated by two analysts with two
different air-displacement pipettes toconfirm the nonlinear trend was consistent for this type of pipette.
In contrast, for calibration curves
prepared with a positive-displacement syringe pipette, or a glass volumetric pipette, the data points
were repeatedly statistically linear(R2 ≥ 0.999), as demonstrated for CBD
in Figure 2b.
Differences in linearity between
the pipetting methods can be understood by considering the mechanismof operation and how it is impacted
by the physical properties (that is,density and vapor pressure) of the solution. For example, air-displacement
pipettes rely upon the movement ofa piston and calibrated air-cushion to

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regulate the volume measurement.
Upward movement of the piston produces partial vacuum in the tip, whichcauses a metered amount of the sample to be aspirated into the tip. The
air-cushion acts like an elastic springfrom which the volume of liquid in
the tip is suspended (Figure 3a). The
volume of the air-cushion, which varies depending on the density, vapor pressure, viscosity, and temperature of the liquid being pipetted(4,5), is most often calibrated with distilled water as the test medium. Solvents with vapor pressure different
from that of water, such as those utilized for commonly used cannabinoid
solvents, push against the calibrated air-cushion forcing it to expand.
The aspirated solution is then displaced from the pipette tip via dripping. This phenomenon compromises the accuracy and precision of thedispensed volume (5). Additionally,
commonly used solvents for cannabinoids such as methanol, ethanol, or
hexane have a lower density than thatof water. Thus, the volume of liquid
pipetted with an air-displacement pipette is systematically high when using these solvents neat, or as a partof a mixture, if the air-cushion pipette
was calibrated with water.
The physical influences that impact an air-cushion pipette are notapplicable to positive-displacement
or glass pipettes. These pipettes repeatedly generated serial dilutions
that were statistically linear. Positivedisplacement pipettes operate using
an integrated piston, or internal syringe. The pipette tip is immersed in
the liquid and the piston rod moves
down to displace the volume of aircorresponding to the desired volume of the pipetted liquid. As thepiston is released, the liquid is drawn
into the tip. The piston comes into
direct contact with the liquid, leaving no air-space (Figure 3b). This pipetting method is suitable for both

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Featturesolvent-based cannabinoid reference
standards and highly viscous liquids,
such as extracted cannabis oils.
When using glass volumetric pipettes, although the pipetted solution comes in contact with the airspace, the meniscus is visually titrated
against a volumetric calibration mark.
Delivery time and waiting time determine pipetting accuracy. The delivery time is the period of time after
the suction is released for the meniscus to fall from the upper volumetricmark to the pipette tip. Waiting time
begins after the liquid reaches the
tip and comes to rest (6). Both must
be adequately used to ensure accurate pipetting, no matter the physicalproperties of the liquid.

Internal
piston(a)(b)

Plunger
SampleSampleDisposable
pistonAir-space

Figure 3: Comparison of pipetting mechanisms for (a) air-displacement and (b) positivedisplacement pipettes.

1.85

Storage and
In-Use Considerations

1.75

Instrumentation and consumables are
the largest expense when operating atesting laboratory. Consumables aredefined as items that are used for an intended purpose and must be replaced
because they wear out or are used up(7). They include both reference standards and sample testing vials (8). Cannabinoid reference standards are packaged in glass ampoules sealed underinert gas to promote stability by preventing evaporation and degradationfrom air and light during transport (9).
After the ampoule has been opened in
the laboratory, a key concern is the potential for degradation during general use. A decrease in purity because ofchemical degradation is always a concern, but for purposes of this manuscript, the solutions were stored before
use at the temperature recommended
in the package insert.
It is common practice to transfer
reference standard solutions fromthe shipping ampoules to liquid chromatography (LC) vials for use andstorage. LC vials are typically manufactured from polypropylene plastic or glass. Although polypropylene

1.55

VOL 1 • NO 4 • NOVEMBER/DECEMBER 201827

Self-sealing septum

Concentration

1.65

1.45
Punctured
septum1.35

Self-sealing after puncture

1.25
Degraded septum after
puncture

1.15
1.05
0.95
0

5

10

20

15

25

30

35

Time after injection (h)Figure 4: Plot of solution concentration for CBD reference standard stored in a vial witha degraded septum compared with a PTFE–silicon self-sealing septum.

vials may be more economical, surface-treated inert glass vials can becertified as chemically clean by the
manufacturer. This certification minimizes the potential for chromatographic anomalies caused by manufacturing process contamination, andis especially important for samples intended for low-level impurity analysis
by mass spectrometry.
The most common closures forthese LC vials are caps that snap orscrew onto the vial. Snap caps provide
an advantage because they are easy
and fast to assemble. Glass LC vials
may show imperfections because of

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the manufacturing process. For example, cracks in the cap may result after
stretching over an opening that is toolarge, or for a smaller opening, the cap
may not provide an adequate air seal.
Both result in the escape of the solvent
from the reference standard solution,
resulting in an increase in the cannabinoid concentration. Although it may
take a few extra seconds to secure acap with screw threads, the threads
provide adequate mechanical force tohold the septum in place and provide
a consistent air seal.
There is an overwhelming variety of cap septum offerings including|

CANNABIS SCIENCE AND TECHNOLOGY

28

Featurerubber, polyethylene, polypropylene,
silicone, and polytetrafluoroethylene(PTFE). The challenge is determining
which is appropriate for solvent-based
cannabinoid solutions. Rubber and silicone alone are not recommended because they may express extractables
and leachables when in contact withsolvents. Chemically resistant polyethylene and polypropylene septa are intended for single injection, aqueousbased sample mixtures. Although
polypropylene septa offer improved
solvent compatibility compared topolyethylene, the piercing force isslightly higher, resulting in an increasein the probability of coring. Pure PTFE
septa are not resealable and should
not be used with highly volatile solvents, short cycle times, or multiple
injection methods, all of which arecommon when testing cannabinoids.
Laminated hybrid PTFE–silicone septa
provide the ideal solution. A thin filmof PTFE laminated to the side of the
septum that faces the sample limits
exposure of the silicone elastomer tothe cannabinoid solvent, while the silicone on the outside surface provides
resealing capability (10). Additionally, these hybrid septa are offered in apreslit format to eliminate vacuum formation or coring as it is pierced by the
injection needle.
To demonstrate how quickly the reference standard solution can be affected by an inadequately sealed vial, a
DEA-exempt CBD reference standard
was removed from the sealed ampouleand aliquoted into two, certified, Acquity 12 x 32 mm sample manager LC
vials (Waters Corporation). Both vials
were sealed with screw-cap closures.
One screw cap contained an inexpensive solvent-incompatible septum
susceptible to coring (source withheld), and the other contained a preslit PFTE–silicone self-sealing septum(Waters). Replicate injections were performed from each vial over the courseof 1.5 days while the vials were stored

in the sample manager at 20 °C.
The DEA-exempt reference standard CBD concentration inside the vialthat used the self-sealing PTFE–silicone septum remained stable after
1.5 days of replicate injections (Figure 4). A hole was observed in the lessexpensive, solvent-incompatible septum after collecting data at two injection time points. The coring resulted in
evaporation of the reference standard
solvent from the cannabinoid over 1.5
days, resulting in concentration of thesolution. It is anticipated that a sample
manager without temperature control
capabilities would likely result in aneven greater increase in solvent evaporation through the open septum.
It is not suggested that reference
standard solutions are stored for long
periods in LC vials with septum. They
can be stored for longer periods in
an LC vial with a chemically compatible septumless storage cap to reduce
solvent loss (11). Even with this precaution, one must consider the number oftimes the vial is opened and closed tominimize solvent evaporation. As withincoming reference standards, the RF
value can be monitored to determine
if the standard is fit for use after storage based on its concentration.

Conclusions
Cannabis testing laboratories rely directly on solvent based DEA-exempt
cannabinoid reference standards toaccurately quantify cannabis samples.
After selecting a reputable supplier,laboratories should consider adopting a qualification process for the incoming reference standards to ensure
incoming formulations meet in-houseassay specifications. Because cannabinoid reference standard solutions are
solvent based, laboratories must be
diligent when handling these formulations (that is, pipetting, vial storage) topromote integrity of the concentrationfrom which potency determinations
are established.

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

References
1) United States Department of Justice,
Drug Enforcement Administration,
Diversion Control Division.
Controlled Substance Schedule:
Marijuana. https://www.deadiversion.
usdoj.gov/schedules/#define.
(accessed Oct 17, 2017).
2) United States Department of Justice,
Drug Enforcement Administration
21 CFR Part 1301 [Docket No.
DEA–447] “Applications to Become
Registered Under the Controlled
Substances Act To Manufacture
Marijuana To Supply Researchers
in the United States,” Federal
Register, 81(156), August 12, 2016.
3) C. Layton and A.J. Aubin,
J. Liq. Chromatogr. Relat.
Technol. 41, 114–121 (2018).
4) K. Ewald, “Influence of PhysicalParameters on the Dispensed
Volume of Air-Cushioned
Pipette,” Eppendorf User
Guide No. 21. June 2015.
5) K. Ewald, “Fundamentals of
Dispensing,” Eppendorf User
Guide No. 19. June 2015.
6) “Volumetric Measurement in the
Laboratory,” www.Brand.com.
(accessed January 16, 2018).
7) “Consumables,” www.Investopedia.
com. (accessed June 6, 2018).
8) J. Witonsky, “Laboratory Spending
Trends,” Lab Manager (2011).
9) M. Rettinger, “Potency Claims –Only as Accurate as Your Reference
Material,” Cerilliant Corporation,
Emerald Conference, 2016.
10) Chromatography Columns
and Consumables, “Septum
Selection Guide,” Thermo
Scientific, 2014–2015.
11) “Waters Quality Parts,
Chromatography Columns
and Supplies Catalog,” Waters
Corporation, 2015–2016.

Catharine E. Layton and Andrew
J. Aubin are with Waters Corporation in Milford, Massachusetts.
Direct correspondence to: Catharine_
Layton@waters.com

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

30

FeatureLeveraging Selectivity and Efficiency to
Take the Strain Out of LC–UV Method
Development for Cannabinoid Profiling
More than 100 cannabinoids have been isolated from cannabis in addition to the five most commonly
tested: ∆9-tetrahydrocannabinol (∆9-THC), ∆9-tetrahydrocannabinolic acid (THCA), cannabidiol(CBD), cannabidiolic acid (CBDA), and cannabinol (CBN). Although many methods have been
published that show the separation of these major cannabinoids, most do not take into accountthe possibility of interference from minor cannabinoids. This interference is most problematic inconcentrates where minor cannabinoids can be enriched to detectable levels. Additionally, someterpenes absorb ultraviolet (UV) light at the same wavelength as cannabinoids, which can result inan additional source of interference. In this study, the liquid chromatography (LC)–UV separationof 16 cannabinoids of interest was performed while the potential impact from minor cannabinoids
and terpenes on reported potency values was monitored. The method was applied to commerciallyavailable CBD oils that have recently become suspect because of inaccurate label claims.

J

ust as consumers rely on nutrition facts labels onfood for making informed choices about their diets,labels on cannabis products are intended to provide
critical information for accurate dosing. Consumer confidence in labeling claims can be shattered by reports of inaccuracies. A recent study published by the Journal of theAmerican Medical Association showed that of 84 cannabidiol (CBD) products purchased online, only 31% were accurately labeled (1). This labeling problem is alarming sincecannabinoids such as CBD and ∆9-tetrahydrocannabinol(∆9-THC) have been found to be very effective for the treatment of various medical disorders; however, accurate dosing is required for positive patient outcomes. As examples, CBD was determined to be an effective treatment
for those suffering from treatment-resistant epilepsy while∆9-THC has been found to be an effective treatment for
pain when coadministered with reduced doses of opioids(2,3). Whether labeling inaccuracies stem from inadequate
analytical methods, instability of formulations, or surreptitious laboratory practices, all result in the same potentially

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VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018TALI RUSS/SHUTTERSTOCK.COM

Justin Steimling

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32

Feature

1

3

4

2

9
8
56

14
7
10

15
11

12

13
16

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 8.50 9.00
Time (min)Figure 1: The separation of 16 cannabinoids by HPLC–UV. Column: 150 mm x 4.6 mm,
2.7-μm Raptor ARC-18; mobile-phase A: water, 0.1% formic acid (v/v), 5 mM ammonium
formate; mobile-phase B: acetonitrile, 0.1% formic acid (v/v); elution: isocratic at 75% B
over 9 min; flow rate = 1.5 mL/min; injection volume: 5 μL; oven temperature: 30 °C; detection: UV absorbance at 228 nm. Peaks: 1 = CBDVA, 2 = CBDV, 3 = CBDA, 4 = CBGA,
5 = CBG, 6 = CBD, 7 = THCV, 8 = THCVA, 9 = CBN, 10 = CBNA, 11 = ∆9-THC, 12 =∆8-THC, 13 = CBL, 14 = CBC, 15 = ∆9-THCA, 16 = CBCA.

negative impact to the health andsafety of consumers.
Although the state of analytical
testing in the cannabis industry has
improved since the inception of legalized medical cannabis, there arestill many opportunities to update existing methods in this dynamic market. Historically, interest in cannabinoids typically focused on THC, CBD,and their carboxylated forms, but theanalysis of more-abundant minor cannabinoids is starting to gather momentum. Testing laboratories mostfrequently use liquid chromatography(LC)-based techniques paired with ultraviolet (UV) detection for cannabinoid profiling because of its low initial cost, ease of use, and robustness.
Because UV detection is limited in its
spectral deconvolution abilities, chromatography plays a critical role in not
only cannabinoid identification, butalso accurate quantitation. The demands on the analytical column are
only made more difficult considering
the complexity of the matrix. Cannabis is a complex matrix that contains
more than 100 cannabinoids as well as
hundreds of additional components

including terpenes, fatty acids, sugars, flavonoids, and pigments (4). The
introduction of cannabis concentrates
into additional matrices to create cannabis-infused products further complicates analysis. If product labels areto accurately reflect cannabinoid content, the complete sample composition must be considered in developing a robust and accurate analyticalmethod. Herein, the process of developing a complete workflow solution for the analysis of cannabinoids
is discussed with emphasis on LC–UV
conditions, sample preparation strategies, method applications, and highthroughput enabling technologies.

Development of LC
Method Conditions
Method development began withthe goal of achieving baseline resolution for the following 16 cannabinoids
by LC–UV: ∆9-THC, ∆9-tetrahydrocannabinolic acid (THCA), CBD, cannabidiolic acid (CBDA), cannabinol(CBN), cannabidivarinic acid (CBDVA),
cannabidivarin (CBDV), cannabigerolic acid (CBGA), cannabigerol (CBG),
tetrahydrocannabivarin(THCV),CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

tetrahydrocannabivarinic acid (THCVA), cannabinolic acid (CBNA), ∆8 -tetrahydrocannabinol (∆8 -THC), cannabicyclol (CBL), cannabichromene (CBC),and cannabichromenic acid (CBCA).
A 150 mm x 4.6 mm C18-type column packed with 2.7-μm superficially porous particles (SPPs) was initially
scouted using popular mobile phases for the analysis of cannabinoids(water and acetonitrile modified with
0.1% formic acid) with UV detection
at 228 nm. C18-type columns are ideal for the separation of cannabinoids
because of their hydrophobic andshape-selective characteristics. The
combination of the appropriate stationary phase with SPPs increases the
speed and improves resolution compared to traditional fully porous particles (FPPs) of the same particle size.
The use of a 150 mm x 4.6 mm analytical column allows for the most efficient separations under the constraints of legacy instrumentation.
Using isocratic conditions it was
found that 14 of the 16 cannabinoids
could be baseline resolved; however,
CBNA was coeluted with ∆9-THC regardless of flow rate, column temperature, or mobile-phase composition.
In an attempt to separate CBNA
from ∆9-THC, the pH of the mobile phases was adjusted by using
0.1% acetic modified mobile phases
in place of formic acid. This strategy
was attempted in an effort to take advantage of the pKa of CBNA because
it would be less retained in its ionized form, but THC would not be impacted as a neutral compound. Ionized compounds are more polar andnot as strongly retained by reversedphase mechanisms. The use of acetic
acid maintained the same selectivity
and resolution of the original separation, but still resulted in the coelutionof CBNA and ∆9-THC. The pH of themobile-phase system was further increased by the use of water modified
with 5 mM ammonium formate and unmodified acetonitrile. This approach
VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Featture

33

Table I: Inter-run accuracy and precision (n = 6)

AnalyteCBD

QC LLOQQC Low

QC MidQC High

QC Dilution (20-fold)

5.00 μg/mL

30.0 μg/mL

150 μg/mL

400 μg/mL1000 μg/mL

Avg.
Conc.
(μg/
mL)

Avg.
Accuracy
(%)

%
RSD

Avg.
Conc.
(μg/
mL)

Avg.
Accuracy
(%)

%
RSD

Avg.
Conc.
(μg/
mL)

Avg.
Accuracy
(%)

%
RSD

Avg.
Conc.
(μg/
mL)

Avg.
Accuracy
(%)

%
RSD

Avg.
Conc.
(μg/
mL)

Avg.
Accuracy
(%)

%
RSD

4.96

99.2

3.14

30.8

103

1.84

156

104

0.455

396

99.0

0.455

1,036

104

0.341

resulted in a loss of retention for all
acidic cannabinoids because of theionization of carboxylic acid functional groups. To reach an intermediate pH, the aqueous mobile phase
was modified with both 0.1% formic
acid and 5 mM ammonium formate,
whereas the organic mobile phase wasmodified with only 0.1% formic acid.
These mobile phases combined witha 1.5 mL/min flow rate using 75% organic allowed for the partial resolutionof CBNA from ∆9-THC while still maintaining the separation of the remaining 14 cannabinoids. To this point, acolumn oven temperature of 40 °C
had been used for method development. To enhance the shape selective
characteristics of the stationary phase,the column oven temperature was reduced to 30 °C. This adjustment resulted in the baseline separation of all
16 cannabinoids with a complete cycle
time of 9 min (Figure 1).

Additional Sourcesof Interference
During LC method development, it
was determined that minor cannabinoids can affect the quantitation of
the major cannabinoids CBD and ∆9THC. Another class of compounds
found in cannabis, terpenes, can also
be present in high enough concentrations to interfere with sample analysis. A mix of 21 common terpenes
found in cannabis was prepared andPF7 Heavy Metal Analyzer
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VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

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M7 GCMS|CANNABIS SCIENCE AND TECHNOLOGY34

FeatureTable II: Determined concentrations of CBD in commercially available hemp-derived CBD oils
Product TypeCBD, Label
Claim (mg/mL)±10% Range(mg/mL)

CBD, Actual
Concentration (mg/mL)

Product 1

Vape oil

3.33

3.00–3.66

2.05

Product 2

Vape oil

6.67

6.00–7.34

5.59

Product 3

Vape oil500

450–550

0.242

Product 4

Sublingual oil

11.0 (hemp extract)

NA

6.24

Product 5

Sublingual oil

6.11

5.50–6.72

5.21

Product 6

Raw hemp oil

30.0

27.0–33.0

18.4

Product Nameextracted using 950 μL of methanol followed by vortexing for 30 s at
3000 rpm. After that, 750 μL of thesample was then mixed with 250 μL ofwater followed by vortexing for 10 s at
3000 rpm. Finally, 400 μL of the sample
was filtered using a Thomson Single
Step standard filter vial with a 0.2-μm
polyvinylidene fluoride (PVDF) membrane before LC–UV analysis.

1

3
4
9

2
8

14

56
7
10
11
12

15
13
16

0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 3.20 3.40 3.60 3.80 4.00
Time (min)Figure 2: The separation of 16 cannabinoids by UHPLC–UV. Column: 100 mm x 3.0 mm, 1.8-μm
Raptor ARC-18; mobile-phase A: water, 0.1% formic acid (v/v), 5 mM ammonium formate; mobilephase B: acetonitrile, 0.1% formic acid (v/v); elution: isocratic at 75% B over 4 min; flow rate =1.0 mL/min; injection volume: 1 μL; oven temperature: 30 °C; detection: UV absorbance at 228 nm.
Peaks: 1 = CBDVA, 2 = CBDV, 3 = CBDA, 4 = CBGA, 5 = CBG, 6 = CBD, 7 = THCV, 8 = THCVA,
9 = CBN, 10 = CBNA, 11 = ∆9-THC, 12 = ∆8-THC, 13 = CBL, 14 = CBC, 15 = THCA, 16 = CBCA.

injected using the same conditionsas previously developed for cannabinoids. Fortunately, the absorbance
profile for most terpenes differs fromcannabinoids such that they do not
result in over reporting for cannabinoids. The terpenes that absorb UVlight best at 228 nm, ocimene andits isomers, do not interfere with thequantitation of any monitored cannabinoid. Minor terpene interferences were found that could impact
the quantitation of CBGA and THCVA if present in substantial concentrations, but the quantitative analysisof these cannabinoids is not currently required in states such as California
and Colorado (5,6).

Sample Preparation
The utility of the chromatographic
method was evaluated by performing quantitative analysis of CBD incommercially available hemp-derived
CBD oils. Calibration standards andquality control (QC) samples wereprepared in 25:75 water–methanol
across a linear range of 5–500 μg/mL.
A QC dilution sample was preparedat 1000 μg/mL and diluted 20-foldto demonstrate the validity of diluting samples into the linear range.
Six hemp-derived CBD oils were obtained for analysis. These products
consisted of three vape oils, two
sublingual oils, and one raw hemp
oil. Next, 50 μL of CBD product was

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Results and Discussion
Using linear 1/x weighted regression, the method showed good linearity for CBD with an r 2 value of 0.999.
The method accuracy was demonstrated to be within 4% of the nominal
concentration for all QC levels. The
percent relative standard deviation(%RSD) was within 3.14% for all QC
levels indicating good method precision (Table I). According to California
regulations, a cannabis product must
not differ from the labeled concentration of CBD by ±10% (5). Applying
this labeling guideline to the samples
evaluated in this study results in thepossibility of all six products not being in compliance with these regulations (Table II). One product failure is
attributed strictly to labeling nomenclature as the CBD content is not directly stated. Vape oils did not contain a significant amount of CBDA toaccount for the discrepancy in the labeling. The large discrepancy in the
result for Product 3 is most likely because of photodegradation from improper packaging. In addition to
CBD, other cannabinoids were found
VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Featturein most samples. Additional cannabinoids that were found included: CBDVA, CBDV, CBDA, CBG, ∆9-THC,∆8 -THC, CBN, CBNA, and CBC. The
concentrations of these cannabinoids
were not quantitatively evaluated because of their relative low abundance,
but the concentration of ∆9-THC in all
samples appeared to be well below
0.3% w/w based upon the peak heightof a 50-μg/mL standard allowing theuse of THC-free labels.
To ensure that sample results were
not skewed because of poor extraction efficiencies, a recovery experiment was performed by spiking
each product type with an additional 2.00 mg/mL of CBD. Recovery results for vape oil, sublingual oil, andraw hemp oil were 102%, 98.5%, and105%, respectively.
With regard to sample preparation,
it should be emphasized that the addition of water following extraction
with methanol is critical to precipitate
lipids that are present in raw hemp oils
and common carrier oils for sublingual products (that is, coconut medium-chain triglycerides [MCT] oil, sunflower oil, sesame oil, and so forth).
Failure to perform this step will cause
sample precipitation to occur once introduced into the mobile phase during high performance liquid chromatography (HPLC) analysis. The inlet fritof the analytical column will quickly
clog resulting in elevated back pressures and decreased column lifetime.
It is important to not combine the addition of water into the extraction stepwith methanol because this has beenshown to result in reduced recoveries
for cannabinoids in cannabis oils (7).

Ultrahigh-Pressure Liquid
Chromatography Analysis
To improve laboratory throughput,the efficiency of sub-2 μm SPPs can beused to increase the speed of analysis while maintaining the same resolution. By pairing an appropriate system to a 100 mm x 3.0 mm analytical
VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

column packed with 1.8-μm SPPs of
the same stationary phase, the separation can be achieved in 4 min (Figure 2). This approach results in a cycle time that is more than twice as fastwith a 70% reduction in consumed
mobile phase per sample. Columns
must be effectively paired to an appropriate LC system that is not onlyrobust at high system back pressures,
but also optimized to reduce extra
column volumes. Any dispersion that
occurs in the valves, connecting tubing, and flow cell will reduce the efficiency and the resolution of separations. It is particularly important touse low-volume flow cells (approximately 1 μL) because of the relatively large volumes present in standard
flow cells (8).

Conclusions
Considering the structural similarities
of cannabinoids, it can be difficult todevelop a robust analytical methodthat is capable of producing accurate
results. Increasing interest in the analysis of minor cannabinoids can further
complicate the separation. Fortunately, demanding separations can still beachieved through deliberate method
development by leveraging selectivity
and efficiency. The power of selectivity is realized through changes to themobile phase that can alter the pH
enough for a critical separation to occur or a change in oven temperaturethat can change the characteristics
of a stationary phase. The increased
efficiencies of SPPs compared to fully porous particles of the same particle size enables faster separations.
Pairing sub-2-μm SPPs with appropriate instrumentation is critical for thoselaboratories interested in pushing thelimits of sample throughput. It wasdemonstrated that 16 cannabinoids
of interest can be separated in 9 min
on a traditional HPLC system. The developed method was compatible forthe identification of cannabinoids andquantitation of CBD in hemp-derived
www.CannabisScienceTech.com

35

CBD oils. As interest in expanded cannabinoid profiles continues to grow,selectivity and efficiency can continue
to be leveraged to remove the strain
of LC–UV method development.

References
1) M.O. Bonn-Miller, M.J.E. Loflin, B.F.
Thomas, J.P. Marcu, T. Hyke, andR. Vandrey, JAMA, J. Am. Med.
Assoc. 318, 1708–1709 (2017).
2) O. Devinsky, E. Marsh, D. Friedman,
E. Thiele, L. Laux, J. Sullivan, I.
Miller, R. Flamini, A. Wilfong, F.
Filloux, M. Wong, N. Tilton, P.
Bruno, J. Bluvstein, J. Hedlund, R.
Kamens, J. Maclean, S. Nangia,
N. Shah Singhal, C.A. Wilson, A.
Patel, and M. Roberta Cilio, Lancet
Neurol. 15, 270–278 (2016).
3) S. Nielsen, P. Sabioni, J.M. Trigo,
M.A. Ware, B.D. Betz-Stablein, B.
Murnion, N. Lintzeris, K. Eng Khor,
M. Farrell, A. Smith, and B. Le
Foll, Neuropyschopharmacology
42, 1752–1765 (2017).
4) M. ElSohly, W. Gul, in Handbook ofCannabis,1st Ed., R.J. Pertwee, Ed.
(Oxford University Press, Oxford,
United Kingdom, 2014), pp. 3–22.
5) California Code of Regulations,
Title 16, Division 42, “Chapter
6, Section 5724 – Cannabinoid
Testing,” (Adopted May 5, 2018;
Effective June 6, 2018), p. 105.
6) Code of Colorado Regulations,
1 CCR 212-1, “Section M 1503 –Medical Marijuana Testing Program– Potency Testing,” (Adopted
February 21, 2018; Effective
February 21, 2018), pp. 218–221.
7) E.M. Mudge, S.J. Murch, and
P.N. Brown, Anal. Bioanal. Chem.
409, 3153–3163 (2017).
8) J. De Vos, K. Broeckhoven,and S. Eeltink, Anal. Chem.
88, 262–278 (2016).

Justin Steimling
is an Applications Manager, LC Solutions at Restek Corporation in Bellefonte, Pennsylvania.
Direct correspondence to:Justin.Steimling@restek.com|

CANNABIS SCIENCE AND TECHNOLOGY36

Feature

Certified Reference Material
Manufacturing Challenges
Some analysts will look at a list of pesticides or solvents and visualize adding small amounts of purematerial of each analyte into a volumetric flask and then bringing the flask up to volume with theirsolvent of choice. In rare instances this technique will work, but not often. Prior to making a mixture,
factors such as solubility and reactivity must be considered. Are all of the analytes soluble in thesolvent that I want to use? Do I need to use an intermediate solvent? Will the analytes react witheach other or will they react with the solvents? Do I need to add a preservative? Which preservative
should I use and will any of the analytes react negatively to the preservative? The answers to thesequestions come from experience and a working knowledge of the chemistry of reference material(RM) production. Manufacturing the standard mixture is only the first step in creating a certified
reference material (CRM). The CRM must be characterized using a metrologically valid procedure.
A certificate of analysis is produced listing certified values for specified properties and all analytes,
including a calculation of total uncertainty, homogeneity, stability under specified conditions, andmetrological traceability. The certificate of analysis is delivered with the standard.
Don ShellyI

f you work in an analytical chemistry laboratory you
may have heard the terms certified reference material (CRM) and reference material (RM). An RM typicallycomes with a certificate of composition (COC) that states
the identity of the product, the purity of the product, andthe details of its characterization. In addition to the information found in the RM COC, the CRM certificate of analysis (COA) declares that the material characteristics were
determined by a metrologically valid procedure for the
specified properties and contains a statement of metrological traceability, homogeneity data, long term stability results, and all factors that determine the CRMs total
combined uncertainty, to name a few. This uncertainty includes the measured uncertainty inherently found in allmeasurement tools used in the manufacturing process
as well as the effects of storage, transportation conditions, and possible chemical interactions affecting longterm stability.

The Benefits of CRMs
CRMs, as opposed to RMs, give labs a competitive advantage and peace-of-mind. ISO 17025 recommends that accredited labs use CRMs whenever available. As a laboratory, you can trust that everything has been done to provide
you with a high quality standard that helps to ensure thatyour data can be generated correctly the first time, andevery time. After all, the quality of your data can directly affect consumer safety. Because the use of CRMs helps
to ensure data quality, your services are of greater value toyour clients and prospective clients.

CRM Challenges
All CRM manufacturers strive for the lowest possible combined uncertainty during the manufacturing process. There
are some variables that cannot be precisely controlled during the manufacturing process such as the limitations ofClass A glassware (typically, the uncertainty at a specifictemperature is written on the glassware) and syringes, precise room temperature, and the uncertainty inherent in all
analytical balances despite calibration with National Institute of Standards and Technology (NIST) certified weights.
The most challenging uncertainty to calculate is the uncertainty obtained from possible analyte to analyte and analyte
to solvent interactions.

What Skills Are Needed to Create CRMs?
The first skill required when making a stock standard froma neat material is knowing which solvent is miscible or soluble with the analyte and if the analyte and solvent will quickly interact under the given storage conditions. If your working standard will be in a solvent different from your stock
solvent, then the stock’s solvent is sometimes known as anintermediate. For example, if you want to spike used motor
oil into water, you know that oil and water aren’t miscible. If
you first dilute your oil with isopropanol at a reasonable concentration, the oil–isopropanol solution can be successfully
spiked into the water matrix and you will have the used motor oil in solution with your water. The isopropanol is your intermediate solvent.
You have created all of your individual stock standards andnow you want to combine portions of each stock to make

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Featture

your working standard mixture. Again,
you need to ask, are the solvents miscible and will my analytes stay in solution? Will that solution be homogenous? Will the analytes quickly interact
with each other or with the solvents?
To answer these questions you needexperience. If you have done this before you will know what is going to happen. If this is your first time making thismixture, you won’t know for sure until you have finished the mixture andsome time has passed. I will give youa hint: All organic chemicals interact
as do many metals. To minimize yourinteraction and increase the shelf life,
you need to know the correct storage
conditions (colder is not always better) and which preservative, and how
much of it, to add to your mixture. Storing a standard at too low of a temperature can negatively affect homogeneity and possibly cause some analytes
to precipitate out of solution. It’s usually a good idea to sonicate or shakemixtures at room temperature before
using, especially if they are cloudy or
if you see solids floating in the solvent.
Many of you are probably now asking yourselves, what is a preservative?
Analyte–solvent interaction can impact
the pH of your solution and redox potential over time. Acetonitrile can break
down into acetamide as the solvent
ages, which makes your solvent basic.
Urea based pesticides will degrade under these conditions. A small amountof dilute formic acid can be added toyour mixture to counter these reactions.
Over time, halogenated hydrocarbons
will interact with methanol to form acids. Low pH will degrade linear ketones
very quickly. A dilute ammonium hydroxide solution will slow these reactions. Now you know why you should
keep your acid sensitive and base sensitive analytes in separate mixtures.
These are just a couple of examples ofanalyte–solvent interactions. There are
hundreds of known interactions andmany interactions are dependent on

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

the number and concentration of youranalytes in a mixture. Many laboratories
request CRMs with all possible analytes
at a high concentration in one ampule
for cost savings. When your CRM expires in a couple of months, are you saving money? More organic compounds
at higher concentrations mean there
are greater chances for fast chemical interactions to occur. Use a stock productor, if a custom one is required, keep theconcentrations reasonable and allow
the manufacturer the option of separating analytes into multiple mixtures. The
analytes’ shelf life will be longer andyour headaches fewer.

How to Ensure Stability
Precision and accuracy are not the only
concerns you might have about yourstandards; stability is also a major factor.
The accidental use of a standard thathas degraded will result in costly reanalysis and increased turn-around time, severely hurting your bottom line and yourlaboratory’s credibility. CRM manufacturers follow a set of ISO 17034 protocols
to estimate a products shelf life.
There are three types of data thatcan be used to determine a products
shelf life: historical data, classical method data, and the accelerated methoddata. Historical data rely on the manufacturer’s knowledge and data of theexact reference material being madeto know how long that material can be
expected to remain accurate under
the assigned storage conditions. Using
the classical method, the manufacturer
makes the product and tests retained
samples of the standard over time until
the product fails. As you can imagine,
this method is very time consuming
and I doubt that you want to wait years
to find out when your standard will fail.
Since most laboratories prefer custom
standards, the only practical way to determine shelf life is by using the accelerated method.
The accelerated method makes theassumption that the product failure

www.CannabisScienceTech.com

37(rate of degradation) increases as environmental conditions become harsher
compared to the stated storage conditions. This ensures that the certified values for the analytes are within the stated uncertainties for the specified shelflife. The method is typically performedby heat stressing the standard. Several
ampules of the standard are made andone is placed in a storage unit at the correct temperature. The other ampules
are placed in heated environments atthree or more temperatures between
the stated storage temperature and
100 °C for a set time. The ampulized
standards are analyzed sequentially using a metrologically validated method.
If recovery of any of the analytes demonstrates a recovery of 95% or less, thestandard is considered failed. This datais entered into an Arrhenius plot to provide a conservative estimate of shelf life.
As the product ages, retained samples
can be pulled from storage and tested using the classical method to determine if the shelf life can be lengthened
or if it needs to be shortened.

Summary
As you can see, a great deal of effort isput into determining the values printed on your COAs. Even so, there canbe unknowable aspects in the scienceof chemistry and the unforeseen canoccur, but you can be assured that thebest available technology was used
to certify your reference materials. To
reduce the possibility of the unforeseen, I recommend resisting the urge
to amend your custom or catalog mixtures unless truly necessary. Also,
when in doubt, let the professionals do
it. You will save yourself time, money,
and headaches.

Don Shelly is the Food and Environmental Product Manager, North America for LGC Standards in Manchester,
New Hampshire. Direct correspondence to: don.shelly@lgcgroup.com|

CANNABIS SCIENCE AND TECHNOLOGYChoosing a Laboratory
Information Management System
A Q&A (LIMS) for the Cannabis Industry
LabVantage Cannabis boosts laboratory testingproductivity while reducing total cost and risk.

Marty Pittman
Senior Product Manager
LabVantage Cannabis

abVantage Cannabis is a purpose-built Laboratory Information Management System(LIMS) that offers unique benefits to the cannabis testing industry. Product features are
configured to meet cannabis testing requirements, taking into account the varied regulatory landscape. LabVantage Cannabis streamlines laboratory operations by offloading manual
data entry and providing an electronic repository that can be easily queried for fast accessto results. Cannabis Science and Technology (CST) recently sat down with Marty Pittman,senior product manager, to discuss how LabVantage Cannabis benefits testing laboratories
and options for its deployment.

L

CST: Why do cannabis testing laboratories need a Laboratory Information
Management System (LIMS)?
Pittman: Initially, most laboratories find that the amount of data associated with their customers’
testing is minimal enough to be managed in spreadsheets and other paper formats. However,as their customers’ businesses grow, the amount of data that testing laboratories have to workwith increases. A LIMS can resolve much of the extra workload, helping laboratories to focus
more on testing and less on managing data.

CST: What is unique about the LabVantage Cannabis product, which is LabVantage
Solutions’ LIMS for this industry?
Pittman: LabVantage Cannabis, which is derived from our core LabVantage product, is configured for the cannabis industry. For example, American Herbal Pharmacopoeia methods that are
specific to cannabis testing are included. This saves customers a lot of time in setting up andconfiguring the LIMS before they can make a product. LabVantage also provides a portal thatcannabis growers can use to request testing directly. This feature facilitates sample collection,
testing, and return of results. In addition, LabVantage provides an interface with government
systems, keeping regulatory monitoring of the cannabis product and testing in one place.

CST: How do speed and cost of implementation of LabVantage Cannabis comparewith that of a traditional LIMS deployment?
Pittman: When implementing a LIMS out of the box, a laboratory must make many determinations. These may include deciding upon what master data must be collected to comply withregulatory requirements, process flows in the laboratory, what data must be gathered fromwhich instruments, and the data approval process. LabVantage Solutions worked with its
customers in the cannabis industry to identify these items upfront. As a result, LabVantage

SPONSORED BY

CHOOSING A LABORATORY INFORMATION MANAGEMENT SYSTEM (LIMS) FOR THE CANNABIS INDUSTRY

Cannabis incorporates much of the information that would otherwise have to be discovered, documented, and configured
from scratch. This allows the LabVantage Cannabis customer
to jump right in and begin using the LIMS.

CST: What features make LabVantage Cannabis uniqueto cannabis testing?
Pittman: In the cannabis industry, there are some uniquerequirements when requesting samples. The request does
not come from an internal laboratory source; external growers
or other cannabis product manufacturers must be able torequest the test. LabVantage Cannabis provides a portal thatallows the grower to submit the request for testing, which
initiates the sample collection process. LabVantage also
includes a chain of custody that is in place when the sample
is received so that it is processed in a known workflow. Data
are peer reviewed to ensure that there are no transcription
errors. Finally, a Certificate of Analysis is generated.
During the process (from sample collection to completionof the Certificate of Analysis), data must be provided to state
governments at certain points to track the cannabis material
and testing results. As I mentioned, LabVantage provides theinterface to do that. Much of the functionality that is needed forAmerican Herbal Pharmacopoeia testing is provided upfront.
In some cases, this is extended to allow for automated instrument integration. This enables an instrument to produce an
output file, which can be parsed and imported into the LIMS.
This spares an analyst from having to manually key data fromthe instruments into the LIMS for tracking and generation of
the Certificate of Analysis.

CST: How does LabVantage Cannabis address thevaried regulatory landscape?
Pittman: The highly flexible configuration options of our core
LabVantage LIMS are retained in the LabVantage Cannabis
product. Customers can modify LabVantage Cannabis asneeded to meet their own requirements. For example, it could
be configured on the basis of where the customer is located,
what regulatory bodies they must comply with, or what laboratory methods they have in place.

CST: Please describe the two options offered for the
deployment of LabVantage Cannabis.
Pittman: LabVantage has a software as a service (SaaS)based option and a traditional enterprise option in which
the customer purchases a license. The latter is typicallyused for implementations in on-premise hardware or incustomer-owned cloud environments. The customer needs
an annual subscription for maintenance, but owns the product.
As such, they are responsible for providing all support andtesting of the operating system, application server, and database server, as well as for working with LabVantage to support
the application itself.
The SaaS model is a “pay-as-you-go” solution in which thecustomer pays an annual subscription fee per user. In this case,
LabVantage manages the operating system, application server,
and database server; the customer has to deal only with the
LIMS itself. This allows the customer to focus on its laboratory
processes (i.e., collecting and managing data) without having
to worry about the behind-the-scenes hardware and operating
systems needed to support the environment.
Some LabVantage customers have reported that thelower yearly cost of the SaaS model is an advantage. Other
customers prefer the enterprise model because they can purchase it upfront and then just pay for the annual subscription
for maintenance. Offering these two models gives customers
a lot of flexibility in terms of deciding their payment schedule.

CST: How does all of this benefit users?
Pittman: The biggest benefit is that users can focus more on
their specialty—namely, the testing of laboratory materials. By
having the LIMS in place, users worry less about transcription
errors in Excel spreadsheets and where papers are locatedin the laboratory. LabVantage gives laboratories the ability tostore all of their data in a central location where it can be easily
accessed when customers have questions about testing
results or the status of samples. LabVantage offloads manyof the day-to-day physical transactions of entering data or
moving papers from desk to desk. Users can concentrate on
the analysis of materials and tracking of results.

CST: Lastly, when a customer invests in LabVantage
Cannabis, how do they know if they are getting theirmoney’s worth?
Pittman: LabVantage Cannabis confers advantages in multiple
areas. Customers quickly find that they can process more
samples with the same number of resources. It allows chemists to spend more time on bench-top analysis and less ondata entry. In addition, electronic data can be mined, queried,
and analyzed. LabVantage Cannabis customers can drill
down to look for trends in their data. The ability to perform
more data analysis could also aid the cannabis grower, byidentifying plant strains that are “good” versus those that may
have undergone mutations.

40

Tutorial

Holding Data to a Higher
Standard, Part II: When Every
Peak Counts—A Practical Guide to
Reducing Contamination and Eliminating
Error in the Analytical Laboratory

Patricia Atkins

C

hemical reference standards have been an important component in accurate analysis for decades. Over the years, the challenges facing chemical laboratories have changed. As a manufacturer ofcertified reference materials (CRMs), many questions
have arisen during our daily interaction with customers

on how to best use CRMs. Sometimes a customer is noteven aware that the issue they are questioning is really anproblem of contamination or error. A common scenario
is that a scientist will express a concern that their standard is too high in particular elements. Usually during theconversation, our scientists discover that the customer

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

BIDAALA_STUDIO/SHUTTERSTOCK.COM

Operator, environmental, and method errors often include sources of contamination. In an increasing,more exacting analytical landscape in pursuit of parts-per-billion (ppb)-level analytes, it is very important
not only to understand the sources of error and contamination but how to reduce them. During thedawn of analytical instruments, the laboratories tested for a select number of compounds or elements
at parts-per-thousand levels. Modern instrumentation now has increased the number of compounds
and elements to be quantitated and lowered the analytical threshold to sub-part-per-billion levels
where 1 ppb is equivalent to 1 s in 32 years! In this type of testing environment even low parts-perbillion levels of contamination can cause large errors in quantitation. In this guide, we look at all of themost common sources of contamination and error in an analytical process from the water used in thelaboratory to the inherent mistakes and error caused by laboratory equipment and operators.

Tutorialis inadvertently allowing contamination into their analysis.
Contamination and error can occur
at almost any point of the process andthen can be magnified as the method
and analysis runs its course. Modern
instrumentation has raised the bar orin this case lowered the limits of detection to the parts-per-billion (ppb)or even parts-per-trillion (ppt) levels. The concept of such small measurements would have been almost inconceivable during the emergence ofmodern laboratory analysis.
To put this into a different context, 1 ppb expressed as a unit of time
would be 1 s in 32 years and 1 ppt
would be 1 s in 320 centuries! In thepast, issues of laboratory contamination were problematic but now contaminants, even in trace amounts,
can severely alter results. It is hard
to imagine that such small amountsof contamination can dramaticallychange laboratory values.
Most questions about contamination come in the form of an inquiry
about a particularly high result forsome common contaminant. In mostcases, the root of that contamination
can be traced to a common source.
The most common sources of standard and sample contamination arefound in the laboratory: reagents,
labware, laboratory environment,
storage, and personnel.

Water Quality
Water is one of the most basic yet
most essential laboratory components. Most scientists are aware thatthe common perception that all water
is the same is untrue. There are many
types, grades, and intended uses forwater. Water is most often used in two
ways in the laboratory: as a cleaning

41

solution and as a transfer solution forvolumetric or gravimetric calibrations
or dilutions. In both of these uses, thewater must be clean to reduce contamination and introduce error into
the process. Poor quality water cancause a host of problems from creating deposits in labware or inadvertently increasing a target element or
analyte concentration in solution.
The confusion starts when laboratories are unsure about which type ofwater they get from their water filtration system. ASTM has guidelines thatdesignate different grades of water.
Table I shows parameters for the four
ASTM types of water (1).
The actual type of water produced
by a commercial laboratory water filtration system can vary in pH, solutes, and soluble silica. Critical analytical processes should always requirea minimum quality of ASTM Type I

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CANNABIS SCIENCE AND TECHNOLOGYTutorial

42

Table I: ASTM designations for reagent laboratory water (1)
ASTM Type
Requirement
I

II

III

IV

Use

Critical laboratory
applications andprocesses

General lab gradeused for pH, buffers,
feeding other water
polishing systems

Cleaning glassware,feeding water polishingsystems, water baths

Not good for lab use

Specific Resistance(megohm/m) (max)

18

1

4

0.2

pH

N/A

N/A

N/A

5.0–8.0

Sodium (max)

1 μg/L

5 μg/L

10 μg/L

50 μg/L

Total Silica (max)

3 μg/L

3 μg/L500 μg/L

highTotal Organic
Carbon (max)

50 μg/L

50 μg/L

200 μg/L

N/A

Table II: Elemental leaching from laboratory tubing (μg/L) (2)Tubing TypeSilicon

Neoprene

Silicon

Neoprene

Leaching Solution

DI H2ODI H2O

5% HNO3

5% HNO3

Fe

0

0

27

5

K

2

2

2

2

Mg

7

0.5

8

2

Na

0

0.8

4

4

Ni

0.2

0.2

4

0.1

Pb

0.1

0.1

3

2

Si

0

0

500

0

Sn

0.01

0.01

1

1.9

Zn

1

55

4

50

91.0
100
80
60

28.7
40

9.1
20

1.2

4.5

3.2

0
HPLC

LC–MS

DI source DI source DI bottle Municipal
flushedstationarytap

Figure 1: Phthalate concentrations in laboratory water sources (pbb) (3).

water. All trace analysis standards, dilutions, dissolutions, extractions, anddigestions should be conducted withthe highest purity of water. Analysts
who use CRMs and perform quantitative analysis need to use quality water
so as not to contaminate their CRMs,

standards, and samples with poor
quality water.
High-purity water is often achievedin several stages in multiple processes
that remove physically and chemicallypotential contaminating substances.
Municipal water supplies often test

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

their own water sources on an annual basis, but that does not mean it isapplicable for use in laboratory applications. Municipal water can becomecontaminated from its distribution
point, especially when left static sitting in pipes, tubing, and hoses. Water left stationary in a laboratory water
system can be exposed to leaching ofelements and compounds from thepiping and hoses. In one experimentconducted at SPEX CertiPrep, leaching solutions of either ASTM Grade I
water or 5% nitric acid in ASTM GradeI water were run through lengths of silicon and neoprene laboratory tubing.
The solutions were collected and tested by inductively coupled plasma–mass spectrometry (ICP-MS). Many
common elements were found to haveleached into the solutions from exposure to the laboratory tubing adding
potential contamination to critical analytical processes, which can be seenin Table II. If the tubing was used totransfer acidified solutions between
vessels the acid further increased thecontamination, elements such as leadincreased from 0.1 μg/L in the ASTM
I deionized (DI) water to 3 μg/L in thesilicon tubing with 5% nitric acid and2 μg/L in the neoprene tubing with 5%
nitric acid.
Another potential source of contamination of laboratory water isphthalates. Phthalates are ubiquitous in the environment and in the
VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Tutorial

43

Table III: Grades of laboratory solvents and their uses
Grade
ACS

Application or Use

Analytical

General procedures

Meets or exceeds ACS specifications

Anhydrous

Water-sensitive reactions and synthesis

Low water levels (10–30 ppm)

Biotechnical

Biotechnical applications

Low water, low residue, low UVEnvironmental

Environmental analysis,
HPLC, trace organic

Trace organics

Food/FCC grade

Food and drug applications

Meets specifications of Food
Chemicals Codex (FCC)GC

GC applications

ppb levels of contamination

HPLC

HPLC applications

Sub-micrometer filtration, somelow UV absorbance

LC–MSPesticide residue
Reagent

LC–MS applications

Low ionic impurities, <0.1 ppm

Pesticide, environmental analyses, trace
analyses, and GC with various detectors

Meets or exceeds ACS
pesticide specifications

General laboratory use>95% purity

SpectrophotometricTechnical
USP

laboratory. Plastics are found everywhere from bottles, tubing, caps, andcontainers. In a laboratory water study
performed at SPEX CertiPrep, we examined bisphenol A and phthalate
content present in a variety of laboratory water sources including bottled
high performance liquid chromatography (HPLC)-grade, liquid chromatography–mass spectrometry (LC–MS)-grade water, municipal tap water,
and water obtained from our in-house
DI (ASTM I) water source (3). The inhouse DI water was tested from a carboy filled within the laboratory, anddirectly from the faucet outlet. The
faucet samples were collected after
sitting overnight and a second sample was collected after the system had
been flushed with multiple gallons offresh water. Phthalates were found in
all the water sources with the highest total phthalates found in the HPLC
bottled water with about 91 ppb ofphthalates as seen in Figure 1.
To reduce contamination from laboratory water sources, the first line of
attack is to choose the correct water source for the given application.
It is also important to realize that water can change quality over time depending on the storage conditions.
VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

UV applications

UV, vis, IR

General laboratory use

Noncritical tasks

Food and drug applications

Meets or exceeds USP specifications

Bottled-water sources can leach organic and inorganic contaminantsfrom the bottle, cap, and liners. Bottled water can also have an expiration date and a shelf life that should
be checked before use. Water thathas been decanted into other vessels can be exposed to many typesof contaminants including dust, microbial growth, and oxidation effects.
Water left in liquid systems such as
HPLC, LC–MS, or ion chromatography (IC) systems should be changed
frequently to prevent contaminationand microbial growth.

by individual manufacturers basedon intended use. Some are generallaboratory grades with intended use
for noncritical applications while other grades usually high in purity andlow in contaminants are designated for more-critical analyses. Table
III shows some general descriptionsof types and grades of solvents andtheir intended uses.
Many analytical laboratories use avariety of chromatography and spectrometry instruments such as gas
chromatography (GC), GC–MS, HPLC,
and LC–MS in their analyses. Solvents
play a large role in these analyticaltechniques as either mobile phases
or matrices for analysis. During sample preparation, many laboratories
expose samples to a variety of solvents ahead of introduction to an analytical instrument. In some cases, thekind of solvent is chosen to best fit thetechnique. LC, GC, and MS systems
each have different modes of analysis
that benefit from specific chemical or
physical properties found in solvents.
For example, in GC and GC–MS,
the most widely used solvents have
low boiling points, are eluted quickly, and don’t interfere with the target
analytes. Solvents with boiling points

Reagents
An analytical laboratory often uses
a large amount of various reagents,
solvents, and acids of varying quality and contamination levels. Thesechemical components can be a large
economic investment for a laboratory, but also a large source of potential contamination. Just as in the caseof water, there are different types orgrades of chemicals, reagents, acids,
and solvents. Some designations areset forth by standards set by the U.S.
Pharmacopeia (USP) or the American
Chemical Society (ACS). Other types
or grades of material are designated
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Table IV: Properties of common chromatography and spectroscopy solvents
Solvent

MW

UV Cutoff

BP (°C)Polarity Index

Water
Methanol

18

NA

100

10.2

32

205

65

5.1

Acetonitrile

41.1

190

82

5.8

Acetone

58.1

330

56

5.1

2-Propanol

60.1

205

82

3.9

Tetrahydrofuran

72.1

210

66

4

Ethyl ether

74.1

218

35

2.8

DMSO

78.1

262

189

7.2

Cyclohexane

84.2

202

81

0.2

Methylene chloride

84.9

233

40

3.1

Hexane

86.2

195

69

0.1

Ethyl acetate

88.1

255

77

4.4

Toluene

92.1

285

111

2.4

Isooctane

114

205

99

0.1

within the analytical range of the target analytes have the potential to becoeluted with the targets and hinder
quantitation. (See Table IV.)
LC and MS techniques depend on
the type of analysis being performed.
Normal-phase LC uses polar columns
and nonpolar solvents such as hexane
and cyclohexane. Reversed-phase LC
uses nonpolar columns such as octadecyl (C18) columns with polar solvents including methanol, water,
and acetonitrile. If ultraviolet–visible
light diode-array detection (UV-vis
DAD) or equivalent is used then the
wavelength of the solvent also becomes important. The wavelength ofthe mobile phase and solvents usedshould be outside of the wavelengthsof the target analytes in the analysis.
The most common range for a typical reverse phase is above 190 nm
UV cutoff for acetonitrile and below
300 nm, which is the UV cutoff for acetone, both popular solvents for LC
applications seen in Table IV.
Solvents are both a material thatcan become contaminated anda source of contamination. Solvents can be contaminated by particles such as dust, rust, and mold.

The solvents can also be contaminated by gases, oxidation, or compounds like the phthalates found inseals and bottle closures. Some solvents have added preservatives that
could add contaminants to analysis
or leach additional elements fromthe storage containers.
There are many persistent solvents that can be found in the laboratory which can cross-contaminate
samples by their presence. Somepersistent solvents include dichloromethane which can cause chlorine contamination as well as dimethyl sulfoxide (DMSO) and carbon
disulfide, which can add sulfur residues. There are solvents that reactwith air to form peroxides, which cancause contamination and safety issues in the laboratory.
Acids are another laboratory reagent that can become both a potential danger and a potential contaminant. Acids by their nature areoxidizers and many of the strongest
acids are used in the processing ofsamples for inorganic analysis. Common acids in digestion and dissolution include perchloric acid, hydrofluoric acid, sulfuric acid, hydrochloric

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acid, and nitric acid. Many of these acids are commercially available in several grades from general laboratory
or reagent grade to high-purity trace
metal–grade acids. Acid grades often
reflect the number of sub-boiling distillations the acid undergoes for purification before bottling. The more anacid is distilled, the higher the purity. These high-purity acids have thelowest amount of elemental contamination but can become very costly at
up to 10 times the cost of the reagent
grade of acids.
Often the question is asked if highpurity acids are necessary in sample
preparation if the laboratory is using
a high-quality ICP-MS-grade CRM.
Clean acids used in sample preparation, digestion, and preservation canbe very costly. But, the difference between the amounts of contamination
in a low-purity acid and a high-purity acid can be dramatic. High-quality standards for use in parts-per-billion and parts-per-trillion analyses
use the highest purity acids available
to reduce all possible contaminationfrom the acid source. An example ofpotential contamination is an aliquotof 5 mL of acid containing 100 ppb
of Ni as contaminant, used for diluting a sample to 100 mL, can introduce
5 ppb of Ni into the sample.
To reduce contamination it is recommended that high-purity acids beused to dilute and prepare standards
and samples when possible. In addition to using pure acid, it is importantthat the chemist check the acid’s certificate of analysis to identify the elemental contamination levels present
in the acid. Some laboratories prefer to use blank subtractions to negate the background contamination,
but blank subtraction for acids canonly work in a range well over the instrumental level of detection. If blank
subtraction causes an analytical result
to fall below the instrument’s level ofdetection, it should not be used.

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Table V: Dispensing volume error associated with various size syringes (4)Table VI: Compound carryover found insyringe washes (ppm of carryover) (4)VolumeDispensed (μL)

% of Syringe
Volume% Error

10

2

20%

23.15%

10

5

50%

8.16%

Syringe Size

10

10

25

100%

2

25

8%

5

20%

Syringe Wash
Number1000 μL

10 μL

1

24.4

360.51

2.72%

2

0.69

46.96

8.82%

3

0.06

8.12

5.47%

4

0.03

4.1

0.04

2.02

25

10

40%

2.37%

5

25

20

80%

1.05%

7

0.01

1.37

25

25

100%

1.25%

10

0.03

1.37

6.09%

15

0.02

1.13

20

0.01

0.43

100

10

10%

100

25

25%

1.67%

100

50

50%

0.64%

100

100

100%

0.61%
1.05%

1000

250

25%

1000

500

50%

1.14%

1000

1000

100%

0.47%

Volumetrics and Labware
Volumetric measurement is a common

45

repeated daily activity in most analytical laboratories. Many processes in thelaboratory from sample preparation to
standards calculation depend on accurate and contamination-free volumetric measurements. Unfortunately,laboratory volumetric labware, syringes, and pipettes are among the mostcommon sources of contamination,
carryover, and error in the laboratory.

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CANNABIS SCIENCE AND TECHNOLOGY

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Tutorial

Table VII: Major elemental impurities found in laboratory container materials (2)Number of Elements

Total ppm

Polystyrene-PS

Material

84Major Impurities
Na, Ti, Al

Tetrafluoroethylene (TFE)

24

19

Ca, Pb, Fe, Cu

Low density PE-LDPE

18

23

Ca, Cl, K, Ti, Zn

Polycarbonate-PC

1085

Cl, Br, Al

Polymethyl pentene-PMP

14

178

Ca, Mg, Zn

Fluorinated ethylene
propylene (FEP)

25

241

K, Ca, Mg

Borosilicate glass

14

497

Si, B, Na

Polypropylene-PP

21

519

Cl, Mg, Ca

High density PE-HDPE

22

654

Ca, Zn, Si

Table VIII: Elemental impurities found in nitric acid distilled in clean laboratories versus
regular laboratories (2)Element

Regular Laboratory

Clean Laboratory

60

15

As

0.17

<0.02

Ca

150

100

Cd

0.3

0.003

Cr

2.5

0.4

Cu

1.7

0.23

Fe

50

9

Al

Mg

10

4

Mn

1.1

0.1
0.03

Mo

0.8

Pb

0.5

0.4

Sb

0.04

0.013

Zn

5.5

0.7

The root of these errors is based on
the four “I” errors of volumetrics:• Improper use• Incorrect choice• Inadequate cleaning• Infrequent calibration.
These four I’s can lead to error andcontamination, which negate all intent
of careful measurement processes.
The first two I’s stand for improper use, meaning that the volumetric is not used correctly or the incorrect choice is made. Many errors can
be avoided by understanding themarkings displayed on the volumetrics and choosing the proper tool
for the job. There is a lot of information displayed on volumetric labware.
Most labware, especially glassware,is designated as either Class A or
Class B labware. Class A glassware
is a higher quality analytical classof glassware whereas Class B glassware is a lower quality glassware witha larger uncertainty and tolerance.
If a critical measurement process isneeded, then only Class A glassware
should be used for measurement.
Other information that can befound on labware is the name of the
manufacturer, country of origin, tolerance or uncertainty of the measurement of the labware, and a seriesof descriptors that indicate how theglassware should be used. Labware
can be marked with letters that designate the purpose of the container.
If a volumetric is designed to contain

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liquid it will be marked by either theletters TC or IN. Labware that is designated to deliver liquid will be marked
by either the letters TD or EX. Sometimes there are additional designations such as wait time or delivery time
inscribed on the labware. The delivery time refers to a period of time required for the meniscus to flow fromthe upper volume mark to reach thelower volume mark. The wait time refers to the time needed for the meniscus to come to rest after the residualliquid has finished flowing down fromthe wall of the pipette or vessel.
A second type of improper use
and incorrect choice can be seenin the selection of pipettes and syringes for analytical measurements.
Many syringe manufacturers recommend a minimum dispensing volume of approximately 10% of the total volume of the syringe or pipette.
A study by SPEX CertiPrep showedthat dispensing such a small percentage of the syringe’s total volume created a large amount of error. In this study, four syringes, 10 μL,
25 μL, 100 μL, and 1000 μL were used
to dispense between 8–100% of thesyringe’s total volume of water. Eachvolume was weighed and replicated
10 times by several analysts and theresults were averaged together tocalculate average error.
The largest rates of error were seenin the smaller syringes of 10 and 25 μL.
Dispensing 20% of the 10 μL syringe
created 23% error. Error only dropped
down to below 5% as the volume dispensed approached 100%. In the larger syringes, measurements over 25%
were able to see error in and around
1%. The larger syringes were able toget closer to the 10% manufacturer’s
dispensing minimum without a large
amount of error, but the error did dropas the dispensed volume approached100%, which is seen in Table V.
The third “I” of volumetric error
is inadequate cleaning. Many volumetrics can be subject to memory
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effects and carryover. In critical laboratory experiments, labware sometimes needs to be separated by purpose and use. Labware subject tohigh levels of organic compounds or
persistent inorganic compounds candevelop chemical interactions andmemory effects. It is also sometimes
difficult to eliminate carryover fromlabware and syringes even when using a manufacturer’s stated instructions. For example, many syringes
are cleaned by several repeated solvent rinses before use. A study of syringe carryover by SPEX CertiPrep
showed that some syringes are subject to high levels of chemical carryover despite repeated rinses.
In this study, several syringes ranging in volume from 10 μL to 1000 μL
were used to dispense a 2000 μg/mLinternal standard mix of deuterated
compounds. The subsequent washes
were collected and tested by GC–MS
to determine the amount of carryoverin each wash (see Table VI).
The larger syringes needed lessrinses to reduce carryover than thesmaller 10-μL syringes. The smaller syringes had more than 1 ppm carryover through over 15 rinses. The typical number of rinses usually employed
to rinse syringes is between three andfive, which in the case of the smaller syringe would not be adequate to clear
all the carryover from the syringe.
The final source of error is infrequent calibration. Many laboratories have schedules of maintenancefor equipment such as balances and automatic pipettes, but often overlook calibration of reusable burettes, pipettes, syringes, andlabware. Under most normal use, labware often does not need frequentcalibration but there are some instances where a schedule of recalibration should be used. Any glassware or labware in continuous use
for years should be checked for calibration. Glass manufactures suggestthat any glassware used or cleaned
VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Air and skin

Glass,
wool, leadHair, Al,paper

Cotton,steel,
wood

Rubber, Ni,
Cu, S,
polyesterPS, tape,
PE, PP

47

PVC,
silicon,PTFE

Figure 2: Triboelectric charge potential of common materials and particles in the laboratory.

at high temperatures, used for corrosive chemicals, or autoclaved should
be recalibrated more frequently.
It is also suggested that under normal conditions that soda-lime glass
be checked or recalibrated every five
years and borosilicate glass after it
has been in use for 10 years. The error
associated with the use of volumetrics can be greatly reduced by choosing the correct volumetric for the task,using the tool properly, and by making sure the volumetrics are properly cleaned and calibrated before use.
Inorganic analysts know that glassware is a source of contamination.
Even clean glassware can contaminate
samples with elements such as boron,
silicon, and sodium. If glassware, suchas pipettes and beakers, is reused, thepotential for contamination escalates.
A study was made of residual contamination at SPEX CertiPrep of our pipettes after they were manually andautomatically cleaned using a pipettewasher (2).
An aliquot of 5% nitric acid was
drawn through a 5-mL pipette after
the pipette was manually cleaned according to standard procedures. The
aliquots were analyzed by ICP-MS.
The results showed that significant residual contamination still persisted in
the pipettes despite a thorough manual cleaning procedure.
The experiment was repeated using a pipette washer especially madefor use in parts-per-trillion analysis. The pipette washer repeatedly
forced deionized water through thepipettes for a set time period. The
pipettes were cleaned in the pipette
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washer, and then the same aliquot of
5% nitric acid was drawn through the
5-mL pipettes. The aliquot was analyzed by ICP-MS. The automatedwasher reduced the contamination
significantly over manual cleaning of
the pipettes. The reduction of contamination by moving from manual
cleaning to an automated cleaning
process was clear. High levels of contamination of sodium and calcium (almost 20 ppb) dropped to <0.01 ppb.
Other common contaminants including lead and iron dropped from 5.4
and 1.6 ppb, respectively, to lessthan 0.01 ppb.
The reduction of contamination inlabware can depend on the materialof the labware and its use. Different
materials contain many types of elemental and organic potential contamination as seen in Table VII (5). Trace inorganic analyses are best performedin polymer or high purity quartz vessels, such as fluorinated ethylene propylene (FEP), and minimize contact
with borosilicate glass. Metals suchas Pb and Cr are highly absorbed byglass but not by plastics. On the other hand, samples containing low levelsof Hg (parts-per-billion levels) must be
stored in glass or fluoropolymer because Hg vapors diffuse through polyethylene bottles.

Laboratory
Environment and Personnel
All laboratories believe they observea level of laboratory cleanliness. Most
chemists recognize that there are inherent levels of contamination present in all laboratories. A common|

CANNABIS SCIENCE AND TECHNOLOGY

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Cosmetics andperfumesHairproducts

MedicatedlotionSoaps andcleaners

Phthalates,
colorants,
preservatives,
metals

Metals,dyes,
solvents,
fragrances,
VOA, SVOA

ZnO,
pharmaceuticals,
waxes,
solvents

Fragrances,
antibacterials,
alcohols

Jewelry,
all types

Cigarette
smoke

Lab
coats

Dust and
dirt

Rxns, plastics,
phthalates, paints,
dyes

VOA, SVOA,
metalsEverything in
the lab!

Pb, phthalates,
pesticides, VOA,SVOA, heavy
metalsFigure 3: Common sources of contamination found in the laboratory.

belief is that the small amounts of environmental and laboratory contamination cannot truly change the analytical results. To test the backgroundlevel of contamination in a typical laboratory, samples of nitric acid weredistilled in both a regular laboratory
and in a clean-room laboratory withspecial air handling systems (HEPA
filters). The nitric acid distilled in theregular laboratory had high amountsof aluminum, calcium, iron, sodium,and magnesium contamination. Table VIII shows that the acid distilled in
the clean room had significantly lower amounts of most contaminants (2).
Laboratory air also can contribute to contamination of samples andstandards. Common sources of air
and particulate matter contamination are from surfaces and building
materials such as ceiling tiles, paints,
cements, and dry wall. Surface contaminants can be found in dust andrust on shelves, equipment, and furniture. Dust contains many different
Earth elements such as sodium, calcium, magnesium, manganese, silicon, aluminum, and titanium. Dust
can also contain elements of humanactivities (Ni, Pb, Zn, Cu, As) and organic compounds like pesticides, persistent organic pollutants (POP), andphthalates. The dust and rust particles
can contaminate open containers in
the laboratory or enter containers bycharge transfer from friction by the triboelectric effect. The triboelectric effect or triboelectric charging is whenmaterials become charged after coming into contact with a second material creating friction. The most common
example of this effect is seen whenhair sticks to a plastic comb after astatic charge is created.
The polarity and the strength of theelectrical charge is dependent upon
the type of material and other physical characteristics. Many materials in
the laboratory have strong positiveor negative triboelectric charges asshown in Figure 2. In the laboratory,materials like dust, air, skin, and lead
have extreme positive charges andcan be attracted to the strongly negative charge of PTFE or other plastic
bottles when the bottle is opened andfriction is created, inducing a charge.
Laboratory personnel can add theirown contamination from laboratory coats, makeup, perfume, and jewelry. Aluminum contamination cancome from laboratory glassware, cosmetics, and jewelry. Many other common elements can be brought in as
contamination from lotions, dyes, and

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cosmetics. Even sweat and hair cancause elevated levels of sodium, calcium, potassium, lead, magnesium, andmany ions. If a laboratory is seeing anusually high level of cadmium in thesamples it could be from cigarettes,
pigments, or batteries. If the levels oflead are out of range, contamination
can be from paint, cosmetics, and hairdyes. Figure 3 shows potential sources of common elemental contamination from outside products.
Laboratory environment and personnel contamination can be reduced by limiting use of personalcare products, jewelry, and cosmetics that could contain contaminationand interfere with critical analyses.
Laboratory coats can collect all typesof contamination and should only beworn in the laboratory to avoid crosscontamination from other laboratories and the outside world. The laboratory surfaces should be kept clean.
Deionized water can be used to wipe
down work surfaces. Laboratory humidity can be kept above 50% to reduce static charge. An ethanol- or
methanol-soaked laboratory wipe
can be used to reduce static electricity as it evaporates.
Even with clean laboratory practices in place, erroneous results can often find their way into sample analysis. To eliminate some of these
spurious results, replication of blanks
and sample dilutions can be used.
The blank results should be averaged
and the sample run values can either
be minimally selected or averaged.
The difference between the two values can then be plotted against acurve established against two more
standards. A minimum of two standard points can be used if the chanceof contamination is minimal, such as
in the case of rare or uncommon elements. Additional standard points
should be considered if the potential
for contamination is high with common elements such as aluminum,
sodium, and magnesium. Multiple
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aliquots of blanks and dilutions canalso be used to further minimize analytical uncertainty.

General Principles and Practices
Laboratories should follow a general regime of three runs each of wash–rinse runs, blank runs, and sample
runs, as well as single runs of sample
plus spike, and standard or spike runs
without sample to use as a control solution to evaluate recovery.
Analysts must realize that the cleanliness and accuracy of their procedures, equipment, and dilutions affect the quality of the standards andsamples. Many laboratories will dilute CRMs to use across an array ofprocedures and techniques. This inhouse dilution of CRMs can be a savings to the laboratory but in the final
analysis can be a source of error andcontamination.

CRM manufacturers design standards for particular instruments to obtain the highest level of accuracy andperformance for that technique. They
also use calibrated balances, glassware, and instruments to ensure themost accurate standards are delivered
to customers. Certifications such as
ISO 9000, ISO 17025, and 17034 assure
customers that procedures are being followed to ensure quality and accuracy in those standards. After those
CRMs are in chemists’ hands, it is then
their responsibility to use all possible
practices to keep their analysis process
free from contamination and error.

492) SPEX CertiPrep Webinar, “Clean
Laboratory Techniques,” https://www.spexcertiprep.com/webinar/clean-laboratory-techniques.
3) SPEX CertiPrep Application Note,“Analysis of Laboratory Water
Sources for BPA and Phthalates,”
https://www.spexcertiprep.
com/knowledge-base/files/
AppNote_BPALabWater.pdf.
4) SPEX CertiPrep Application Note,“Understanding Measurement:
A Guide to Error, Contamination
and Carryover in VolumetricLabware, Syringes and Pipettes,”
available via the SPEX CertiPrep
website as a downloadable PDF.
5) J.R. Moody and R. Lindstrom,
Anal. Chem. 49, 2264 (1977).

References
Patricia Atkins
is a Senior Applications Scientist with
SPEX CertiPrep in Metuchen, New
Jersey. Direct correspondence to:patkins@spex.com

1) ASTM D1193-06(2018), Standard
Specification for Reagent Water,(ASTM International, WestConshohocken, Pennsylvania,2018) www.astm.org

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Tutorial

Rapid Screening of Cannabinoids in
Edibles Using Thermal Desorption-GC–MS
Most of the traditional methodologies for the determination of cannabinoids are based on solvent
extraction, filtration, and concentration. These techniques are cumbersome, time-consuming, andsuffer from analyst-to-analyst variability while producing data of limited value. Many laboratories
routinely “screen” each sample to quickly determine the potential for matrix interference andinstrument contamination while providing an estimate of the target compound’s concentration.
A good “screening” method is simple (that is, minimal or no sample preparation), fast (analysis
in less than 5 min), and semiquantitative. This article describes how thermal desorption (TD)-gas
chromatography–mass spectrometry (GC–MS) analysis eliminates conventional sample preparation
regimes and can be used as a good rapid screening technique.

M

ost of the traditional methodologies for the determination of cannabinoids are based on solvent extraction, filtration, and concentration.
These techniques are cumbersome, time-consuming,and suffer from analyst-to-analyst variability while producing data of limited value.
As the demand for the analysis of cannabinoids increases, it is imperative that the day-to-day analytical protocols
be reproducible, accurate, and efficient. Many laboratories routinely “screen” each sample to quickly determine the potential for matrix interference and instrument
contamination while providing an estimate of the target

compound’s concentration. A good “screening” method
is simple (that is, minimal or no sample preparation), fast
(analysis in less than 5 min), and semiquantitative.
One of the most widely used analytical techniques for“screening” is thermal desorption-gas chromatography–
mass spectrometry (TD-GC–MS) (1,2). This techniquedoes not require any solvent extraction or sample pretreatment. Milligram quantities are put in an inert sample cup which is then “ready to analyze.” The multimodepyrolyzer with a vertical micro-furnace design allows programmable and multiple thermal desorption analysis ona single sample. This process, which refers to evolved gas

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FUDIO/STOCK.ADOBE.COM

Rojin Belganeh and William Pipkin

Tutorial

analysis (EGA), starts with the acquisition of a thermal profile (that is, detector response as a function of sample temperature) of each sample
type. To perform EGA, a short, deactivated tube (2.5 m, 0.15 mm i.d.)
is used to connect the injection port
to the MS detector. The sample isdropped into the furnace at a relatively low temperature (40–100 °C).
The furnace is then programmed toa much higher temperature (600–
800 °C). Compounds “evolve” fromthe sample as the temperature increases. A plot of detector response versus furnace temperature
is obtained. Extracted ion chromatograms (EIC) are used to identify
the thermal zone over which specific compounds of interest evolve fromthe sample. Now, these optimum TD
temperatures can be used in subsequent TD-GC–MS experiments to introduce the key components of interest while minimizing introduction of
the matrix. Only this portion of thesample is actually transferred (that is,
injected on) to the analytical column.
Injecting only a small portion of thesample provides immediate benefits
to the laboratory, such as:• The high boiling fraction of thesample remains in the sample
cup. This eliminates the needfor a high-temperature bakeout. Thus, column lifetime
increases, there is little to nosystem contamination, and runto-run cycle time decreases.
• More sample can be put in thesample cup, which has the effectof lowering detection limits—without affecting instrument
performance or cycle time.
With respect to the analysis of cannabinoids, it is important to keep inmind that TD-GC–MS is based on thevolatilization of target compounds
from the matrix. Those compounds
that are thermally labile or easily converted to an alternative compound need to be identified. In these

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

51

185 °C4,000,000

H

3,000,000

OH

TIC

H
O

2,000,000
1,000,000

300

200

600

500

400

700

Thermal desorption range (100–300 °C)
m/z = 299

EIC

m/z = 314
m/z = 231

300,000

m/z = 271

200,000

100,000

300

200

600

500

400

700

Figure 1: EGA thermogram of THC standard and extracted ion chromatograms (EICs).

Run #18,000,000

THC

0.26 mg5,000,000

Area: 6083448

4.00

6.00

8.00

10.00

12.00

14.00

16.00

18.00

20.00

22.00

Run #28,000,000

0.26 mg
Area: 6664705

5,000,000

4.00

6.00

8.00

10.00

12.00

14.00

16.00

18.00

20.00

22.00

Run #38,000,000

0.25 mg5,000,000

Area: 6352708

4.00

6.00

8.00

10.00

12.00

14.00

16.00

18.00

20.00

22.00

RSD 4.6%

Figure 2: TD-GC–MS chromatograms of the brownie bite in triplicate.

instances, it is the reformed compounds that are identified and monitored. Decarboxylation is forced
to completion which could give the“screening determinations” higher
values: the concentration range increases and dilution factors are moreaccurately determined.

Experimental
Three edible samples were analyzed

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using the TD-GC–MS method forquantification of cannabinoids. The
experiments were performed bya Frontier Multi-Mode Pyrolyzer(EGA/PY 3030D) directly interfaced
to a benchtop GC–MS system. To
automate the sequence and reduce
the workload by increasing reliability of analysis, the Auto-Shot Sampler(AS-1020E) was combined with themultimode pyrolyzer. The vent-free|

CANNABIS SCIENCE AND TECHNOLOGY

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Tutorial

1e+07

5,000,000

4.00

6.00

8.00

10.00

12.00

14.00

16.00

20.00

18.00

Add 300 ng THC

16,000,000

Add 100 ng

12,000,000

22.00

y = 24,024.4071x + 6,222,377.7143
R2 = 0.9978

CBN

Add 0 ng

8,000,000

-259

CBD

4,000,000
0-300*STD solution is the mixture of CBD, THC and CBN

-200

-100

100

0

200

300

Brownie Standard addition calibration curve

X intercept : -259.0 (ng)label THC
10 mg/10 g= 1 mg/g

Sample weight 0.26 mg

THC concentration 996.2 ng/mg = 0.996 mg/g

Figure 3: Edible (brownie) sample standard addition calibration curve.

Run #1THC

0.099 mg3,000,000

Area: 4460437
2,000,000

1,000,000

4.00

6.00

8.00

10.00

12.00

14.00

16.00

18.00

20.00

22.00

Run #2
0.097 mg3,000,000

Area: 4884453

2,000,000

1,000,000

4.00

6.00

8.00

10.00

12.00

14.00

16.00

18.00

20.00

22.00

Run #30.105 mg3,000,000

Area: 4638695

2,000,000

1,000,000

4.00

6.00

8.00

10.00

12.00

14.00

16.00

18.00

20.00

22.00

RSD 4.6%

Figure 4: TD-GC–MS chromatograms of the chocolate pieces in triplicate.

GC–MS adaptor that allows switching of a GC separation column without breaking vacuum on the MS detector was also used. The adaptor
was utilized for switching the EGA
tube to the separation column andvice versa without venting the MS
detector, which saves time and increases productivity.
Sample 1Acommercial

packageofcannabis-infused chocolate brownie containing 10 brownie bites withthe total of 100 mg tetrahydrocannabinol (THC) was used. According to the product label, eachbrownie bite contains 10 mg of
THC. In this experiment, one of
the brownie bites from the package was placed on an analytical balance, and the weight was recorded
as 10.17 g. So, based on the label,
there is 10 mg/10 g = 1 mg/g of THC

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

present in that brownie bite. The
same brownie bite with the recorded weight was used to perform the
TD-GC–MS analysis to confirm thetheoretical THC value according to
the label.
To calculate and confirm theamount of THC, EGA was first performed on a THC standard (Absolute Standard). The pyrolyzer furnace was programmed from 100 °C
to 800 °C (20 °C/min), and the EGA
thermogram as shown in Figure 1
was obtained.
From the EGA thermogram, theoptimal thermal desorption zoneof THC was identified as 100 °C to
300 °C. In fact, using the MS interpretation library, the peak with the
apex of 185 °C (100 °C to 300 °C
temperature zone) was identified as
THC. TD-GC–MS analysis was thenperformed on the brownie bite intriplicate as shown in Figure 2. To
perform TD-GC–MS analysis, thepyrolyzer furnace was programmed
from 100 °C to 300 °C (100 °C/min)after the EGA tube was replaced bya separation column (easily facilitated by using the vent-free GC–
MS adaptor). The amount of sample
used to obtain the TD chromatograms was 0.25–0.26 mg.
The peak shown in Figure 2 (noted with a *) between the retention
time of 12 to 14 min was identified
as THC using the MS interpretation
library. The percent relative standard deviation (RSD%) of 4.6% was
calculated based on the area countsof the THC peak. The most intense
peak around 6 min was identified as
5-hydroxymethylfurfural (dehydration of sugar).
To confirm the THC concentration in the brownie bite, a standard addition calibration curve wascreated. The standard solution wasa mixture of cannabidiol (CBD),
THC, and cannabinol (CBN). Figure
3 shows the calibration curve and

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Tutorial

calculated amount of THC in thebrownie bite.
Using the calibration curve, theTHC concentration is calculated as
0.996 mg/g while the product label
indicates 1 mg/g of THC.
Sample 2
A commercial cannabis-infuseddark chocolate bar with the total of 100 mg THC and net weightof 50 g (1.7 oz) was used for sample 2. According to the product label, there are 20 pieces of chocolates and each piece of chocolate
contains 5 mg of THC, so there is
100 mg/50 g = 2 mg/g of THC present in each piece. To demonstrate
the accuracy and precision of themethodology, the analysis was performed in triplicate. The weightsof each piece were recorded using
an analytical balance as 0.099 mg,
0.097 mg, and 0.105 mg.
The same methodology was used
for analyzing sample 2. First, the
EGA was performed as the fast rapid screening technique. Then the
optimal thermal desorption zoneof THC was identified. The pyrolyzer furnace was programmed from
100 °C to 300 °C (100 °C/min) to obtain the thermal desorption chromatograms for all three pieces of
the chocolate. Figure 4 shows the
TD chromatograms in triplicate.
The peak shown in Figure 4 (noted with a *) between the retention
time of 12 to 14 min was identified
as THC using the MS interpretation
library. The RSD% of 4.6% was calculated based on the area counts of53

the THC peak.
To confirm the THC concentrationin the chocolate pieces, a standard
addition calibration curve was created. The standard solution wasa mixture of CBD, THC, and CBN.
Figure 5 shows the calibration curveand calculated amount of THC in
the pieces.
Based on the calibration curve,
the THC concentration is calculated
as 2.1 mg/g while the product label
indicates 2 mg/g of THC.
Sample 3Acommercial
cannabis-infusedgummy package with the net weightof 45 g (1.59 oz) was used for sample
3. The package contains 10 gummies
with THC and CBD (2-[(1R,6R)-6-isopropenyl-3 -methylc yclohex-2-en-

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54

Tutorial

THC

9,000,000
8,000,000
7,000,000
6,000,000
5,000,000
4,000,000
3,000,000
2,000,000
1,000,000
4.00

6.00

Add 300 ng

10.00

8.00

12.00

16.00

14.00

18.00

22.00

20.00

14,000,000

THC

y = 21,529.07x + 5,335,526.00
R2 = 0.994

12,000,000

Add 100 ng

10,000,000
8,000,000

Add 0 ng

6,000,000-216.84,000,000
2,000,000
0
-300

-100

-200

*STD solution is the mixture of CBD, THC and CBN

0

200

100

300

Brownie Standard addition calibration curve (TD300)

label THC

X intercept : -216.8 (ng)

100 mg/50 g= 2 mg/g

Sample weight 0.105 mg

2065 ng/mg = 2.1 mg/g

THC concentration

Figure 5: Edible (chocolate pieces) sample standard addition calibration curve.

CBD

1e+07

THC

Area (m/z = 231):9530122

Area (m/z = 299):2823342

8.00

14.00

Run #10.25 mg

6,000,000
2,000,000
4.00

6.00

10.00

12.00

CBD

16.00

20.00

18.00

22.00

Run #2THC

0.26 mg

1e+07
6,000,000

90781632708138

12.00

14.00

2,000,000
4.00

6.00

8.00

10.00

CBD

16.00

20.00

18.00

22.00

Run #3THC

0.26 mg
1e+07
6,000,000

94021972721218

12.00

14.00

2,000,000
4.00

6.00

8.00

10.00

16.00

20.00

18.00

22.00

RSD CBD 2.5%
RSD THC 2.3%

Figure 6: TD-GC–MS chromatograms of the gummy in triplicate.

Table I: Summary of the theoretical and calculated cannabinoids in the edibles
Brownie

Chocolate Bar

Gummy

Target compound

THC

THC

CBD

THC

Product label

1 mg/g2 mg/g

10 mg

5 mg

Calculated result

0.996 mg/g

2.1 mg/g

8.5 mg

6.1 mgRepeatability(N = 3) RSD (%)

4.6

4.6

2.5

2.3

Calibration
curve (R 2)

0.998

0.994

0.999

0.998

1-yl]-5-pentylbenzene-1,3-diol). According to the product label, eachgummy has 10 mg CBD and 5 mg
THC. The label also indicates that

tetrahydrocannabinolic acid (THCA),
cannabidiolic acid (CBDA), and CBN(other required cannabinoids) are
0.0 mg/package.

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

To perform the TD-GC–MS analysis, one of the gummies was weighedon an analytical balance The weight
was recorded as 0.109 mg. The sample was then placed in MeOH andsonicated for 1 h. Next, 1 μL of
MeOH solution was spiked into thesample cup.
It is important to mention thatthe gummy sample could be analyzed as is without dissolving in any
solvent. The experiment on sample
3 was performed based on external standard calibration to demonstrate the reliability and flexibilityof this technique.
Figure 6 shows the TD-GC–MS
chromatograms of the gummy samples in triplicate. The EGA thermogram of the gummy confirmed thethermal zone of 100 °C to 300 °C for
both THC and CBD. Note the detection peaks of both CBD and THC
in the chromatograms. The RSD%of 2.5% for CBD and 2.3% for THC
are calculated based on the area
counts of the THC peak.
To confirm the THC and CBD concentrations in the gummy sample,
an external standard calibration
curve was created. Figure 7 shows
the calibration curves and the calculated concentrations, which are
in excellent agreement with the
package label. CBD concentration is calculated as 8.5 mg/gummy compared to the label value of
10 mg/gummy. The calculated THC
is 6.1 mg/gummy while the label indicates the value of 5 mg/gummy.

Conclusion
Table I shows the calculated and label values of the cannabinoid concentrations in all three commercial
edible samples. Using TD-GC–MS
the cannabinoids were thermally extracted from the mixture and the calculated concentrations were in excellent agreement with the packagelabels. Standard addition calibration

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Tutorial

curves were used for the brownie
bite and chocolate piece while an external standard calibration curve wascreated to calculate THC and CBD in
the gummy sample.
In conclusion, thermal desorption analysis eliminates conventional sample preparation regimes; thesample is heated to the point thatthe cannabinoids desorb from theedible matrix (thermal extraction).
It is fast, uses minimal or no solvent,and eliminates the need for expensive glassware. TD-GC–MS is a “volatiles only” analysis; high boilingsample constituents remain in thesample cup which eliminates system contamination, increases system stability, and reduces run-to-run
analysis time.
A multimode pyrolyzer provides
users with a clear picture of thesample’s composition by identifying the thermal zones and the compounds in each zone. Using the
EGA thermogram, one can simply
determine the suitable temperature
program and program the pyrolyzer’s furnace appropriately.
Using pyrolysis GC–MS, solid samples can be analyzed. There is no
solvent required when using pyrolysis-thermal desorption GC–MS as
opposed to traditional GC–MS techniques. In other words, the solid andliquid samples can be injected (using an inert sample cup) into the pyrolyzer without any solvent and sample pretreatment. This advantage, as
well as rapid screening capability, is
one of the primary reasons many laboratories integrate multimode pyrolyzers into both their day-to-day
quality control and analytical research protocols.
Pyrolysis GC–MS techniques alsoenable material characterization ofvirtually any organic material by providing detailed information about
the composition of the samples. This
technique is used for identification of

VOL 1 • NO 4 • NOVEMBER/DECEMBER 201855

THC 50 mg/package CBD 100 mg/(CBN)

1.5e+071e+071000 ng

THC

CBD

THC 50 mg/package CBD 100 mg/package(THC 50 mg/gummy, CBD 10 mg/gummy)
300 ng5,000,000

100 ng
11.00

11.50

12.00

12.50

13.00

13.50

14.50

14.00

CBD

15.00

THC
20,000,00

40,000,00
y = 38389x - 2E+06
R2 = 0.99869

30,000,00

y = 17202x - 680172
R2 = 0.99825

15,000,00

20,000,00

10,000,00

10,000,00

5,000,00

0
0

200

400

600

800

1000

0

1200

0

200

400

600

800

1000

1200

CBN
100,000,000

CBD

THC

Label

10 mg/gummy

5 mg/gummy

Calculated(ESTD)

8.5 mg/gummy

6.1 mg/gummyy = 86574x - 3E+06
R2 = 0.99907

80,000,000
60,000,000
40,000,000
20,000,000
0
0

200

400

600

800

1000

1200

Figure 7: Edible (gummy) sample external standard addition calibration curve.

complex polymers, copolymers, volatiles, and additives as well as failure,
contamination, deformulation, anddegradation analyses. As opposed
to GC–MS alone, pyrolysis GC–MS
allows multiple and customized analysis on the same sample while the MS
libraries offer a broad range of references: from low boiling point compounds to pyrolyzates and heavier
polymeric fragmentations. In termsof the ability to run samples at higher temperature, pyrolysis GC–MS
can provide the user with an expanded temperature range from ambient+10 to 1050 °C (± 0.1 °C precision) as
well as a high interface temperature(maximum 450 °C).

References
1) ASTM International, ASTM D782316: Determination of Low Level,
Regulated Phthalates in Poly (Vinyl
Chloride) Plastics by Thermal
Desorption—Gas Chromatography/
Mass Spectrometry, https://www.
astm.org/Standards/D7823.htm.
2) International ElectrotechnicalCommission, IEC 62321-8:
Determination of certain substancesin electrotechnical products – Part
8: Phthalates in polymers by gas
chromatography-mass spectrometry(GC-MS), gas chromatography-mass
spectrometry using a pyrolyzer/
thermal desorption accessory (PY/
TD-GC-MS), https://webstore.
iec.ch/publication/32719.

Acknowledgement
The authors thank Robert Freeman, Itsuko Iwai (Research & Development, Frontier Laboratories), andTerry Ramus (application scientist,
Diablo Analytical) for contributing to
the article and providing the analytical work, without which this article
would not have been possible.

www.CannabisScienceTech.com

Rojin Belganeh is the technicaland marketing director for Frontier
Laboratories Ltd. North America in
Antioch, California. William Pipkin
is the president of ATRq in Orem,
Utah. Direc t correspondence to:rojin@frontier-lab.com and william.
pipkin@gmail.com|

CANNABIS SCIENCE AND TECHNOLOGY

56

Tutorial

Major Engine of Growth in the Cannabis
Industry: State of the Art Formulation
Technology for Product Innovationand Expanded Applications
Formulation technologies provide a powerful tool in product innovation and new applications
especially for purified and highly concentrated extracts including cannabidiol (CBD) andtetrahydrocannabinol (THC). Fortunately, the cannabis industry can choose from formulation
technologies and ingredients that have a record of use in pharmaceuticals, food and beverages,
dietary supplements, personal care, and veterinary and pet food products. This article aims to assist
in making choices that support safety, efficacy, stability, and consumer acceptance.

New, innovative products and applications havebeen a major driver of growth of the cannabis industry. The range and number of new products
is breathtaking and spans pharmaceuticals, food and dietary supplements, topical and personal care, and veterinary and pet food. It includes product formats ranging
from prescription pharmaceutical formulations to capsules,
chewable tablets, nutrition bars, gummies, drops, bottled
water, beverages and sports drinks, creams, lotions, sprays,
inhalation and vapor products, and pet snacks and treats.
In a significant milestone, in June 2018 the U.S. Food andDrug Administration (FDA) approved the drug Epidiolex(GW Pharmaceuticals), which is an oral solution of cannabidiol (CBD) for the treatment of seizures associated with
two rare and severe forms of epilepsy. Epidiolex is the first
FDA-approved drug that contains a purified drug substance derived from cannabis—in a strong pipeline of development and clinical testing.
Purified and concentrated cannabis extracts are powerful tools in product innovation. For medical applications,they allow the identification of the active ingredients, clinical testing for FDA approval and claims, and productsthat have defined potency and can be tested with established scientific methods for meeting specifications withCANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

WITTHAYA/STOCK.ADOBE.COM

Andreas M. Papas

Tutorialconsistency and stability. The same
reasons increasingly apply to dietary
supplements, beverages and sports
drinks, and other applications. The
use of purified and concentrated extracts also allows for the use of smaller amounts, which has significant benefits for taste, odor, color, or capsuleand tablet size for oral supplements.
The use of purified and concentrate
extracts also facilitates accurate testing using smaller sample size.

Why Formulation:
The Top Reasons
Formulation is key to new innovative
products and applications for the following reasons:• Solubility in water• Increased absorption
and bioavailability• Improved stability• Taste, odor and othercharacteristics• Regulatory
Let’s take a closer look at each reason
below.
Solubility in Water
Upon extraction and purification, important cannabinoids such as CBD andtetrahydrocannabinol (THC) come out
as oils that are practically insoluble inwater. For many products and applications such as beverages, medical formulations, sprays, topical formulations,and others, solubility in water is a must.
Increased Absorption
and Bioavailability
Absorption of oils requires optimalfunction of the liver, pancreas, and thecomplete digestive tract. Absorption
is also affected by the diet, age, and57

health conditions of the user. Clinically proven formulation technologies increase absorption and bioavailability
especially in the large population segments with suboptimal absorption (1,2).
Improved Stability
The stability and shelf-life of cannabinoids is affected by exposure
to sunlight, air, heat, and other factors. When cannabinoids are added to water, foods, creams, and other products, their stability can beaffected by exposure to oxidizing
agents, acidic or alkali conditions,and reactive compounds. Customized formulations provide powerfultools for optimizing stability.
Taste, Odor, andOther Characteristics
Taste is of paramount importanceIntegrated Solutions for Potency and Safety with the expression Compact Mass Spectrometer and Solation ICP-MS

Potent Solutions For Your Budding Lab

Advion.com/Cannabis • info@advion.com
For research use only under applicable state and country laws.

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

www.CannabisScienceTech.com|

CANNABIS SCIENCE AND TECHNOLOGY

58

Tutorial

Intestine
MicellesLipidsBlood

Pancreatic
enzymes

Bile

Pancreas

Liver

Figure 1: Absorption of lipids in humans. Bile and pancreatic enzymes are essential forthe formation of micelles and absorption of lipids. Suboptimal function and diseases ofthe liver, pancreas, and the digestive tract cause malabsorption.

Lipophilic interior
Hydrophilic exterior

Figure 2: Micelle-like particles enable solubility and enhance absorption. Micelles arecomposed of hydrophobic (lipid) interior and hydrophilic exterior. In the human body,formation of micelles is essential for emulsification and absorption of lipids.

in food, beverages, and other oral
products. Odor is also important.
Terpenes, which are abundant in cannabis plants, can have strong aromas that may be carried over into
extracts, concentrates, and even purified cannabinoids. Formulation provides the opportunity for addressing the taste, odor, texture, and othercharacteristics for the specific products and applications.
Regulatory
For medical applications, formulationis required for accurate dosing of thedesired product. With the expanding approval of cannabis products in
the United States, Canada, and other countries, there is increasing focus
on quality, testing and product specifications, potency, stability, and otherproduct characteristics.

Choosing Formulation
Agents: Top Criteria
The top criteria to consider whenchoosing the right formation agentsinclude safety, efficacy, positive or
neutral effect on important properties, and support of label and customer preferences. Let’s explore eachof those criteria in more detail.
SafetyThe FDA’s GRAS (generally recognized as safe) designation is a top selection criterion. A long record of safeuse on a daily basis, with significant
safety margins across wide dose ranges supported by clinical evidence,
provides additional confidence.
EfficacyThis criterion requires major homework, especially for the critical

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

parameters of water solubility, stability,
and increased absorption and bioavailability. While efficacy claims are abundant, few are supported by evidence.
The gold standard is research and clinical evidence from leading universities
and researchers, preferably supported by the National Institutes of Health(NIH) or similar quality funding organizations, and the results published in refereed scientific and medical journals.
Positive or Neutral Effecton Important Properties
This includes taste, odor, and color.
For oral products, especially foods
and beverages, taste and odor are ofparamount importance.
Support of Labeland Customer Preferences
Although there is no official definitionof clean label, consumers increasingly show preference for minimally processed products with safe ingredients, preferably derived from natural
sources. Additional consumer preferences include no sugar or salt added,
free of gluten, dairy, and animal products, nuts and other sources of allergens, and nongenetically modified
organisms (non-GMO).

Key Commercial
Formulation Applications
The major cannabinoids, CBD and
THC, are key components of innovative products. Increasingly, these cannabinoids are used in concentrated or
purified form, especially for medical,
dietary supplement and food and beverage applications, sprays, and topical
products. Key objectives of formulation
were discussed above and include:
1. Solubility in water especiallyfor the emerging market
segments of infused water,
beverages, sports drinks, andother water-based products.
2. Increased absorption andbioavailability, which is key
VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

Tutorial

for medical applications withoral dosing especially because
disease conditions often cause
poor absorption. Enhanced
absorption is important for
efficacy of dietary supplement
applications in wellness andhealth with strong and growing
consumer awareness3. Stability: Formulations ofcannabinoids in water based
products, especially whencombined with other ingredientsin the final product suchas vitamins, minerals, andnutraceutical, increase thechallenges to their stability (3).
A good number of solubilizing agentsare available and include:• Water-soluble organic solvents
such as ethanol, polyethylene
glycols, glycerin, N-methyl-2pyrrolidone, dimethylacetamide,
and dimethylsulfoxide (DMSO).
• Non-ionic surfactants such asvitamin E TPGS (d-α-tocopheryl
polyethylene glycol 1000
succinate), polyethoxylated
castor oil (Cremophors),
polysorbates (Tweens), sorbitanmonooleate, poloxamers,
macrogolglycerides linoleates, andmono- and di-fatty acid esters.
• Phospholipids suchas hydrogenated soy
phosphatidylcholine,
distearoylphosphatidylglycerol,l-α-dimyristoylphosphatidylcholine,
l-α-dimyristoylphosp
hatidylglycerol.
• Organic liquids and semi-solids
such as medium-chain mono- anddiglycerides, and cyclodextrins.

Producing the
Optimal Formulation
The choice of the right ingredientsdepends on many factors such as theproperties of the active ingredient or
the final form of the product. For example, cyclodextrins and solid monoglycerides have a key role in formulating tablets and other solid forms whileothers such as ethanol, polyethylene
VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

glycols, and glycerin support the formulation of liquids.
The increasing consumer awareness and strong preference for simple
formulations using ingredients withproven records of safety and efficacy,
and the major role of taste and odor,
especially for oral products, have limited the practical choices dramatically. For example, polysorbates (such as
Tween-80) which are common, strong
solubilizers in the pharmaceutical,
food and beverage, and cosmetic industries, can impact the taste. More
importantly, an increasing consumer
segment prefer products that do notcontain polysorbates (4).
Vitamin E TPGS, a derivative of naturally sourced alpha-tocopherol is
becoming the formulation ingredientof choice for cannabis products, especially purified or concentrated CBD
and THC and other extracts. The reasons include:• A proven record of safety (1,5)
based on decades of commercial
use in pharmaceuticals anddietary supplements, including
vitamin formulations for children.

59of allergens, sugar, salt, gluten,
dairy, and animal products.

References
1)

S.H. Wu and W.K. Hopkins, Pharm.
Technol. 23, 52–68 (1999).

2)

C. Högenauer and H.F. Hammer,
in Sleisenger and Fordtran’s
Gastrointestinal and Liver Disease,10th Ed., M. Feldman, L.S.
Friedman, and L.J. Brandt, Eds.
(Elsevier Saunders, Philadelphia,
Pennsylvania, 2016). Ch. 104.

3)

L.K.Sørensen and J.B. Hasselstrøm,
Drug Test Anal. 10, 301–309 (2018).

4)

http://www.ewg.org/skindeep/
ingredient.php?ingred06=705142&
refurl=%2Fproduct.php%3Fprod_
id%3D62813%26#.W6T0dvZRfyQ.

5)

European Food Safety Authority(EFSA), “D-alpha-tocopheryl
polyethylene glycol 1000 succinate(TPGS) in use for food for particularnutritional purpose,” The EFSA
Journal 490, 1–20 (2007).

6)

K.A. Papas, M.K. Sontag, C.
Pardee, R.J. Sokol, S.D. Sagel,
F.J. Accurso, and J.S. Wagener,
J. Cyst. Fibros. 7, 60–67 (2008).

7)

P.P. Constantinides, J. Han,
and S.S. Davis, Pharm.
Res. 23, 243–55 (2006).

• Efficacy based on conclusive
clinical evidence (6), not only
as a solubilizer for watersoluble formulations, but also
in its ability to form micellelike particles that enhanceabsorption and bioavailability.
Its efficacy is illustrated by its
use in clinically-tested (7), FDAapproved products formulated
for enhanced absorption.

Andreas M. Papas, PhD, is CEO andmember of the Board of Directors of
Antares Health Products, Inc., and an
Adjunct Professor of Health Sciencesof East Tennessee State University. A
Fulbright Scholar, Dr. Papas is a graduate of the University of Illinois andauthor of The Vitamin E Factor paperback and editor of the scientific book
Antioxidant Status, Diet, Nutrition and
Health. Dr Papas also founded YASOO
Health Inc., and led the company as
President and Chair of the Board of
Directors. He developed productconcepts and managed successfulcommercialization including formulation, clinical evaluation supported by
the National Institutes of Health andthe Cystic Fibrosis Foundation, stability and safety testing, as well as pilot
and commercial production and marketing. These disease specific nutritional products are considered thestandard of nutritional care in cystic
fibrosis, liver disease, and bariatricpatients. Direct correspondence to:apapas@tpgs.com• Neutral taste and odor and lightyellow color are particularly
important for oral and personalcare product formulations.
• Support of product stability.
Vitamin E TPGS contains somefree tocopherols that have strong
antioxidant activity and support
product stability especially foroil-based products. In addition
to reducing potency, productsof oxidation affect taste,odor, and can be harmful.
• Support of label claim of free
www.CannabisScienceTech.com|

CANNABIS SCIENCE AND TECHNOLOGY

60

Cannabis Crosssroads

Professor Jack Henion Shares Insights on
Cannabis Research, Academia, and the
Expanding Role of Mass Spectrometry
Cannabis analytical testing is rapidly expanding beyond cannabis quality control testing to academic,
pharmaceutical, and clinical markets. Mass spectrometry is also playing a critical role in this evolution. In thismonth’s “Cannabis Crossroads,” Professor Jack Henion shares his insights on cannabis research, academia,
and mass spectrometry, including challenges and opportunities in moving cannabis science forward.
Joshua Crossneyhigh-quality analytical techniques andtechnology. I remain excited about
working within and contributing to thisfast-paced, evolving industry.
Every scientist that I meet withstruggles in some way with analyzing
cannabis. What hurdles did you firstexperience in working with cannabis
and how did you overcome them?
Henion: Our experience with marijuanaplant materials to-date is somewhat limited because we do not yet have a Schedule I controlled substances license fromNew York State. We have applied for thislicense, but do not yet have it. As a result,
I have focused on the analysis of hemp
plant materials and products which ofcourse must contain less than 0.3% tetrahydrocannabinol (THC). I would not
say that the analysis of these plant materials is particularly difficult. In contrast
to my experience with parts-per-billion(ppb) and sub-ppb bioanalysis of drugs
and their metabolites in biological fluids, quantifying the important cannabinoids in hemp and marijuana is relatively
easy because the levels are much higher (percent levels) and the matrix is muchless complex than blood or urine. In contrast, the accurate and precise quantitative determination of as many as 100
pesticides at low ppb levels in marijuana plant materials is of course more challenging. Plant sample preparation whenhandling large sample numbers needs

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

some advancement, but the technologies and methods available when properly applied are not that difficult. Of
course, there are additional quantitative measurements needed such as for
terpenes, flavonoids, mycotoxins, andheavy metals, which in some cases require different sample preparation techniques and instrumentation. Thus, a “total analysis” of a cannabis plant sample
is not just one sample preparation technique followed by an injection into one
analytical system. It is a series of related,but different procedures.
You have started lecturing on
cannabis and hemp at Cornell
University. What were some of yourtakeaway messages and how were
those lectures received?
Henion: I recently gave a lecture to theCornell BioEngineering MS graduate
students where I focused on the importance and benefits of collaboration andinnovation in science and business development. I described the rapidly developing cannabis industry as a new frontier with many technology development
opportunities for these students in theirbioengineering careers. I received many
inbound inquiries after this lecture, whichsuggests I struck a chord of interest andexcitement with these students by sharing with them some industry intellect regarding opportunities in the cannabis
and hemp industries.

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OLEH MARKOV/SHUTTERSTOCK.COM

It seems most analytical scientists
have an “ah ha!” moment when theyrealize the incredible opportunities
in cannabis science. When did you
start to see these opportunities,
and how did you first get involved incannabis science?
Professor Jack Henion: I actually had
two “ah ha” moments. The first was asan analytical chemist I was intrigued tosee how analytical methodologies andtechnologies used for cannabis were
not as technologically current as thosein the good laboratory practice-regulated pharmaceutical bioanalyticalworld with which I was familiar. This coupled with the chemical complexity anddiversity of the many cannabis cultivars
and the importance of accurate and reliable analyses suggested that perhaps
I could contribute to improving the analytical sciences used in this growing industry. However, the real excitement,or second “ah ha” moment for me, occurred when I attended the first Cannabis Science Conference in 2016 where
I witnessed compelling testimonialsof the very positive medicinal marijuana benefits afforded to certain disease
sufferers. A common successful business model is to “find a need and fill it.”
I was convinced this was an exciting new
field where I could perhaps contributeto “filling a need” by providing positive
contributions to supporting the scientific integrity of this new industry throughCannaabis Crossroa
ads

As a pioneer and leader in mass
spectrometry, can you please commenton its role in cannabis science?
Henion: I believe mass spectrometry isan essential component for the credible growth and acceptance of the cannabis industry. I, of course, can be accused of being “overly prejudiced” in myinterest and support of MS as a detector
and, in particular, LC–MS techniques. In
my early days of racehorse drug testing
where our analytical results would have tostand up to legal scrutiny in court, my students used to call the mass spectrometer the “truth machine.” Currently, there
is no other detector for the determination of organic compounds that provides
the sensitivity, selectivity, and speed forthe money than MS. When MS is coupled to gas chromatography (GC) andfor even wider applications, LC (or bestwith ultrahigh-pressure liquid chromatography [UHPLC]), one has unequaled
analytical capabilities. I worry a bit about
the current unchallenged interest in LC–
photodiode-array detector (PAD) for

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018cannabis potency determinations because we know there are chemical entities in the sample matrix that can coelute or interfere with photodiode-array
detection. If LC–MS techniques could becompetitively priced and coupled withease-of-use, I would prefer to use thosetechniques for potency determinations
rather than LC–PAD. But that should beleft up to the individual laboratory and its
leadership.
Please comment on what is next foryou in cannabis science. What businessand research projects are you working
on that you can share with us?
Henion: As you may perceive from mycomments above, I am very excited toparticipate in and hopefully contribute to maintaining a high degree of scientific excellence used in the analysis of
any cannabis-related samples. This pertains to plant materials for potency andpesticides as well as the rapidly increasing diverse array of commercial products. I have heard reference to the “wild,
wild west” nature of some current procedures and policies in the medical marijuana world. The days of “snake oil”
sales pitches and unsubstantiated product promises should not return because
it will diminish the credibility and potential of this exciting field. I have proposedthat Advion, Inc., establish a “Cannabis
CRO” and plans for that are underway.
It is my goal to establish and maintain astate-of-the-art laboratory that maintains
the highest level of scientific analyticalservices. In the meantime, we are carrying out applied research in sample preparation and LC–MS analysis techniques
for hemp-based plants and products
to improve upon analytical procedures
currently used. To have a ready sourceof fresh hemp plant materials, this pastsummer I qualified as an approved “Cornell Affiliate” hemp grower under a permit issued by the New York State Agriculture and Markets and collaborated with
Cornell University to grow a small hemp

www.CannabisScienceTech.com

plot on my personal farm near Ithaca, NY.
So, now I know a little bit about growing
and analyzing hemp.
Are there any additional comments
you would like to make regarding thefuture of cannabis science?
Henion: I believe medicinal marijuana
and its promising industry will be part of
the future. However, we have a very steep
learning curve ahead of us. Academic research is thwarted because of misguided opinions and funding is limited forsimilar reasons. The good news is, I believe, this will change with time and thatin fact there are many exciting opportunities ahead. My plea is for the maintenance of scientific and business integrity
such that the benefits and opportunities
remain available for all. As Nike says, let’s“just do it.”
Reference1) http://www.cvent.com/events/2018fall-new-york-state-veterinaryconference/agenda-7c9177edd8
2241ccb90849e19093c5a3.aspx.

About the Interviewee
Dr. Jack Henion is aninternationally recognized
leader in the field of MS and
LC–MS. He is credited with
13 patents and has published more than 200 peerreviewed papers in scientific journals. In
addition to vast industrial experience,
Dr. Henion managed a major researchlaboratory at Cornell University, where
he served as a professor of toxicology formore than 24 years and is now Emeritus
Professor of Analytical Toxicology.

About the Columnist
Joshua Crossney is thecolumnist and editor of“Cannabis Crossroads”
and a contributing editor
to Cannabis Science andTechnology magazine.
Crossney is also the president andCEO of CSC Events. Direct correspondence to: josh@jcanna.com|

CANNABIS SCIENCE AND TECHNOLOGY

OLEH MARKOV/SHUTTERSTOCK.COM

Additionally, I recently presented two
lectures at the annual Cornell Veterinary
Conference at the Cornell University College of Veterinary Medicine, Ithaca, NY(1). There is growing interest and acceptance, especially among companion animal veterinarians for the use of cannabidiol (CBD) oils and related products
to manage pain and other ailments fortheir “patients.” These lectures included
a “tutorial” on liquid chromatography–
mass spectrometry (LC–MS) and related
techniques showing methods used forthe analysis of hemp and marijuana plantmaterials as well as a second lecture on
the comparison of analytical results fromcommercial veterinary oils, tinctures, andso forth versus what is listed on the labels.
My message was caveat emptor since often the product label does not accuratelyreflect what is in the bottle. The veterinarians in the audience appeared to be very
interested in these topics.

61

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Applicationn Note

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Marty Pittman, Senior Product Manager, LabVantage Solutions Inc.

LabVantage Cannabis is a purpose-built informatics platform, offering cannabis testing labs
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Tracking Capabilities
Both growers and lab administrators as well as lab managers want visibility to lab processing. Lab leaders must
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METRC Integration
As samples are received and processed, the LIMS shouldinterface with METRC to signal that the sample is undergoing testing. Likewise, the system should share results
and auto-populate invoices. Such integration contributes
to a more efficient workflow between the grower, the lab,
and regulators.
Industry-Standard Testing
A cannabis LIMS must support industry-standard testing,such as American Herbal Pharmacopoeia-recognized analytical test methods.
A purpose-built cannabis LIMS works in lockstep withlab teams, from initial request through final invoicing, in a
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For a white paper and information on LabVantage Cannabis, a cannabis-specific LIMS platform, visit labvantage.com/cannabis.

Grower Portal
Because cannabis testing labs serve a wide range of growers, a portal into the system is a desirable feature. It provides growers with a frictionless mechanism for preparing
and submitting requests for the lab.
Growers must be able to easily enter details about the
sample; specify which tests are needed and when; provide
details such as METRC ID or the mass of each batch; andtrack all of their harvest lot requests at various stages. The
system must deliver a certificate of analysis that is modifiable for different lab results.

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

LabVantage Solutions, Inc.
265 Davidson Avenue, Suite 220,
Somerset, NJ 08873
tel. (908) 707-4100; fax (732) 560-0121
website: www.labvantage.com

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ANALYTICALINSTRUMENTSANALYTICALTESTING LAB

CULTIVATION/GROWINGEXTRACTION

2018

MANUFACTURING& PROCESSING

PACKAGING &SUPPLIES

Supplier

Profiles

ISSUE

OTHER
SERVICES

Evgeniy - stock.adobe.com
obe.com

CONSULTING

64

Supplier ProﬁleAdvion & Advion BioServices
COMPANY DESCRIPTIONANALYTICALINSTRUMENTSANALYTICALTESTING LAB

Advion’s nearly three-decade dedication to serving scientists yields customer-focused life science solutions. Our deep scientific, engineering, and customer workflow knowledge spawns an
unrivaled solution portfolio. We work directly with, train, and passionately advocate for our customers to ensure their success. Dedicated to Science—Dedicated to You.

CHIEF SERVICES SUPPORTEDTERRITORIES SERVED

Advion develops, manufactures, and globally supports mass spectrometers, novel sample introduction and assay solutions, chipbased ion sources, chromatography systems,
and consumables for life science and relatedindustries. Advion also offers expanded fullservice contract research testing facilities forcannabis, hemp, and biological samples.

Global instrumentation provider with contractlab services for US and Canadian markets.

MAJOR PRODUCTS• expression compact mass spectrometer• SOLATION ICP-MS• Plate Express TLC plate reader• AVANT (U)HPLC chromatography series• TriVersa NanoMate nanoelectrosprayionization source

Advion &Advion BioServices
61 Brown Road, Suite 100
Ithaca, NY 14850
USA
TELEPHONE

Toll free: 1-877-523-8466(607) 266-9162
Fax: (607) 257-5761
EMAIL

info@advion.com
LOCATIONS OF OTHEROFFICES AND FACILITIESHarlow, United Kingdom
Germany
KEY PERSONNEL

North America: Gary Williams,
gwilliams@advion.com
Europe: Mark Allen,mallen@advion.com
Central Europe: Andreas
Wiesner, awiesner@advion.com

www.advion.com

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Supplier Proﬁle65

CEM Corporation
COMPANY DESCRIPTIONANALYTICALINSTRUMENTS

EXTRACTION

CEM Corporation is a leading global company specializing in scientific solutions for critical laboratory applications. We design and manufacture systems for analytical laboratories, life sciences, and processing plants worldwide. Our product portfolio includes innovative instrumentation
for sample preparation for elemental and chromatographic analysis.
We have been deeply involved in the cannabis industry for many years and are familiar withtesting procedures and regulations. We are founding members of many cannabis committees
that are working on standardization of testing and reporting of data. We are passionate abouttranscribing this information into systems to help your business grow and have the knowledge
to support you along the way.

CHIEF SERVICES SUPPORTEDWorld-class application and service support
are what set CEM apart from other instrument
manufacturers. Our mission is to simplify yourtesting procedures with easy-to-use systems
that do the work for you. With built in methods, onboard support videos, and live applications and service support ready to help
when you need it most, CEM is your partnerin sample prep.

• MARS 6: Microwave digestion system fortrace metals sample prep of all cannabis
and cannabis containing products.

STATES SERVED
Nationwide

MAJOR PRODUCTS• EDGE: Automated extraction systemfor potency, pesticides, terpenes, andmycotoxins. The EDGE automatically
performs solvent addition, sample
extraction, filtration, and coolingin as little as 5 minutes.

CEM Corporation
3100 Smith Farm Road
Matthews, NC 28104
USA
TELEPHONE

Toll free: (800) 726-3331(704) 821-7015
Fax: (704) 821-7894
EMAIL

info@cem.com
LOCATIONS OF OTHEROFFICES AND FACILITIESFrance, Germany, Ireland,
Italy, Japan, United Kingdom,
Local agency representatives
in all world regions

www.cem.com

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CANNABIS SCIENCE AND TECHNOLOGY

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Supplier ProﬁleChem Service, Inc.
COMPANY DESCRIPTIONANALYTICALINSTRUMENTS

Established in 1962, Chem Service is accredited for ISO Guide 34:2009 and ISO/IEC 17025:2005
and registered and certified to the ISO 9001:2008 Quality Management System for the design,development, production, distribution, and servicing of organic neat and synthetic referencematerials.

CHIEF SERVICES SUPPORTED
MANUFACTURING& PROCESSINGOTHERSERVICES

Chem Service, Inc., produces high purity
chemicals for use as reference materials andfor other laboratory purposes. More than 95%
of their standards grade materials have a certified purity of 98.0% or greater. Standardsgrade chemicals are clearly labeled with an
expiration date that is based on years of experience in handling and testing. Products arepackaged in small quantities to minimize storage, waste, and disposal requirements. Organic and inorganic chemicals, solutions, andmixtures are available to meet a wide range of
specialized laboratory needs.

MAJOR PRODUCTS• Pesticide residue standards• Cannabis pesticide standards• Residue solvent standards• Flame retardants/PBDE• Metabolite standards• EPA standards• USP standards• ISO standards• DIN standards• Explosive residues• PCB congeners• Petroleum hydrocarbons• Fatty acid methyl esters• High purity inorganics• Surfactants• Anti-oxidants• Ultraviolet inhibitors• Plasticizers• Biological stains• Phthalate standards• Polynuclear aromatics• Vitamins• Carbohydrates standards• Forensic standards• Personal care product standards

STATES SERVED
US and international

Chem Service, Inc.
600 Tower Lane
West Chester, PA 19380
USA
TELEPHONE

Toll free: (800) 452-9994(610) 692-3026
Fax: (610) 692-8729
EMAIL

info@chemservice.com

www.chemservice.com

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Supplier Proﬁle67

Frontier Laboratories
Edibles quick and easy by EGA/PY 3030D Multi-Mode Pyrolyzer

ANALYTICALINSTRUMENTS

COMPANY DESCRIPTION
Frontier Laboratories, Ltd., was founded in 1991 by Dr. Chu Watanabe. His experience working atHewlett-Packard’s Analytical Division and Dow Chemical made him uniquely qualified to design
and market analytical instruments for materials characterization. Dr. Watanabe, with the support ofpolymer scientists at Nagoya University in Japan, developed a pyrolyzer based on a vertical microfurnace design. Today the patented fourth generation vertical microfurnace serves as the cornerstone for the 3000 Series of products developed and marketed worldwide by Frontier Laboratories.

CHIEF SERVICES SUPPORTEDSTATES SERVED

Research, development, and manufacture ofanalytical equipment.

Nationwide for the U.S. and Canada, as well
as Asia/Oceania, Europe, Middle East/Africa,
and Russia.

MAJOR PRODUCTS
Frontier Laboratories, Ltd., designs and manufactures analytical instruments for materials
characterization. The main products, supported by a number of accessories and software,
include the EGA/PY-3030D Multi-functional Pyrolysis System, the PY-3030S Single-Shot
Pyrolyzer, the Rx-3050 series of Rapid Screening Reactors for catalyst screening, and a lineof Ultra ALLOY® stainless steel capillary columns. Frontier Labs’ products are compatible with most gas chromatographs and mass
spectrometers from major manufacturers.

Frontier Laboratories
North American
Technology Center:
5141 Lone Tree Way,
Antioch, CA 94531
TELEPHONE(925) 813-04980
LOCATIONS OF OTHEROFFICES AND FACILITIES

4-16-20 Saikon
Koriyama, Fukushima
963-8862, JapanKEY PERSONNEL

Rojin Belganeh, Technical
Director- North America
Itsuko Iwai, Senior Research
Chemist- North America
William Pipkin, Global
Consulting

www.frontier-lab.com

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Supplier ProﬁleRestek Corporation
COMPANY DESCRIPTIONANALYTICALINSTRUMENTS

CONSULTING

For more than 30 years, Restek has been a leader in developing technologies and manufacturing
products for gas and liquid chromatography (GC and LC), including columns, reference standards, sample preparation materials, accessories, and more. We have decades of hands-on practical experience in chemistry, chromatography, and engineering, and our reputation for going theextra mile with our Plus 1 customer service and top-performing products is well known throughout the chromatography community. Restek has been providing the cannabis market with testing
consumables and services since 2010 for both product safety and product quality. This includes
supporting testing for potency, pesticides, residual solvents, mycotoxins, and terpenes.

CHIEF SERVICES SUPPORTEDOTHERSERVICES

Whether you are part of a well-establishedquality assurance lab or starting a new lab,
Restek has the products and expertise youneed for successful cannabis analysis. Beingan employee-owned and independent chromatography company, every employee atRestek has a vested interest in your success.
We design the best solutions for your lab, regardless of the instrumentation and techniques used.
• LC
• GC
• Sample preparation• Reference standards

solvents, mycotoxins, and terpenes. Our
chemists develop LC and GC columns, reference standards, and sample preparation
products that streamline cannabis testing.
Restek’s Rxi columns deliver more accurate,
reliable results than any other fused silica column on the market. Our Raptor LC columns
are ideal for cannabis testing because theyquickly separate your target compounds, providing higher sample throughput. Restek isalso continually expanding our product line
in order to meet the evolving needs of thecannabis industry. Restek’s certified reference materials are manufactured and quality
control tested under ISO 17034 and ISO/EIC
17025 accreditations.

MAJOR PRODUCTS
We offer a range of chromatography consumables for potency, pesticides, residual

STATES SERVED
Nationwide and North America.

Restek Corporation
110 Benner Circle
Bellefonte, PA 16823
USA
TELEPHONE

Toll free: 1-800-353-1300
EMAIL

support@restek.com
KEY PERSONNEL

Ashlee Gerardi,
Business Development
Manager - Cannabis
Colton Myers, Applications
Chemist – GC Solutions
Justin Steimling, Applications
Chemist – LC Solutions

www.restek.com

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Supplier Proﬁle69

Shimadzu Scientific Instruments
COMPANY DESCRIPTIONANALYTICALINSTRUMENTS

Shimadzu is one of the world’s leading providers of analytical instruments for applications in a
broad range of industries. In the United States, Shimadzu has been at the forefront of working
with cannabis testing laboratories and has a comprehensive understanding of the requirementsof this evolving industry. From seed to sale, from accurate potency testing and terpene profiling to contaminate testing for pesticides, residual solvents, heavy metals, and mycotoxins/aflatoxins, Shimadzu offers scalable solutions to meet your testing needs for today and tomorrow.

CHIEF SERVICES SUPPORTED
As medicinal and recreational cannabis markets continue to grow, analytical testing will
ensure that consumers are receiving accurately labeled products that are free from contamination. Shimadzu is ready to assist you as you
grow your laboratory. We offer a full suite of
testing instruments, research platforms, scientifically validated methods, and a variety of leasing programs to meet evolving requirements. In addition, our expert team ofscientists is readily available to help your cannabis testing laboratory succeed, assistingwith method development, instrument training, and maintenance to ensure your systems
operate at an exceptional level.

MAJOR PRODUCTS
Shimadzu offers a full suite of analytical instrumentation to help grow your lab. These instruments include:• HPLC• GC• GC–MS/MS• LC–MS/MS• AA• ICP-MS• Moisture balances• Online SFE-SFC-LC–MS/MS• MALDI-TOF MS• Consumables

STATES SERVED
Nationwide

Shimadzu Scientific
Instruments
7102 Riverwood Drive
Columbia, MD 21046
USA
TELEPHONE

Toll free: (800) 477-1227(410) 381-1227
Fax: (410) 381-1222
EMAIL

webmaster@shimadzu.com

www.GrowYourLab.com

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Supplier ProﬁlePixis LabsCOMPANY DESCRIPTIONANALYTICALTESTING LAB

Pixis Labs sets the standard for quality analytics in the CBD and hemp markets nationwide andraises the bar for Oregon cannabis laboratories. In partnership with Columbia Food Labs, andas a member of Tentamus Group, Pixis Labs boasts top-of-the-line instrumentation and nearly
40 years of analytical expertise. With low detection limits and robust methodologies, Pixis Labs
is ahead of the curve for changing requirements and emerging markets, offering services beyond compliance. We pride ourselves on building a community of sustainable business partnerships through detailed analyses and accurate reporting. Contact us for a custom service andprice quote.

CHIEF SERVICES SUPPORTEDMAJOR PRODUCTS

Pixis Labs offers you reliable data and turnaround times with transparent, professional
communication and competitive pricing.
• Potency HPLC (ISO 17025)• Pesticides by LC–MS (ISO 17025)• Heavy metals by MS/MS (ISO 17025)• Residual Solvents by GC–MS (ISO 17025)• Organic-equivalent pesticide screen (ISO17025), developed in-house, by LC–MS• Mycotoxins by LC–MS/MS (ISO 17025)• Moisture, water activity• Terpenes by GC–MS• Pathogens• Yeast and mold• Nutritional lab: FDA Labels, allergens,vitamins, supplements, shelf life, and more

Pixis Labs offers accurate and clear reporting,catered to your market and industry.
Consultation services are available uponrequest.

STATES SERVED
Pixis Labs’ services are available nationally forhemp and CBD analyses, as well as nutritional, environmental, and microbiological testing.
We are proud to serve the Oregon cannabis
market for compliance and R&D testing.

Pixis Labs
12423 NE Whitaker Way
Portland, OR 97230
USA
TELEPHONE(503) 254 1794
EMAIL

customerservice@
pixislabs.com
KEY PERSONNEL

Derrick Tanner,
General Manager
Jen Stiles, Operations
Manager
Kelly O’Connor, Sales Rep

www.columbiafoodlab.com

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Supplier Proﬁle71

SPEX CertiPrep
COMPANY DESCRIPTIONANALYTICALTESTING LABANALYTICALINSTRUMENTS

EXTRACTION

MANUFACTURING& PROCESSING

SPEX CertiPrep has been servicing the scientific community since 1954. We are a leading
manufacturer of certified reference materials (CRMs) and calibration standards for analytical
spectroscopy and chromatography. We offer a full range of inorganic and organic CRMs. We
are certified by DQS to ISO 9001:2015 and are proud to be accredited by A2LA to ISO/IEC
17025:2005 and ISO 17034:2016. The scope of our accreditation is the most comprehensive in theindustry and encompasses all our manufactured products.

MAJOR PRODUCTS
We offer analytical standards for medicinaland recreational cannabis testing. SPEX
CertiPrep offers ISO 17034 CRMs for all of
the common contaminants such as pesticide
residues, residual solvents, and heavy metals
as well as qualitative analysis CRMs such as
terpenes and cannabinoids. As the industry
demands change and regulations are put
into place, we continually update our productofferings.

STATES SERVED
Nationwide for the US and Canada.

SPEX CertiPrep
203 Norcross Avenue
Metuchen, NJ 08840 USA
TELEPHONE

Toll free: (800) 522-7739(732) 549-7144
Fax: (732) 494-1747
EMAIL

crmsales@spex.com
LOCATIONS OF OTHEROFFICES AND FACILITIESStanmore, UK+44 (0) 208 204 6656
KEY PERSONNEL

Christy Greene,
Territory Manager
Jeff Akers, Territory Manager
Rebekah Biermann,
Territory Manager

www.spexcertiprep.com

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Supplier ProﬁleVividGro
COMPANY DESCRIPTIONCULTIVATION/GROWINGMANUFACTURING& PROCESSING

VividGro is a pioneer in the AgTech space. Tailored to support the automation and efficiency
needs of the indoor agriculture and horticultural markets, VividGro implements solutions that
help growers maximize yields and reduce costs. The state-of-the-art, customized lighting product line delivers optimized PAR to maximize plant growth and PAR efficacy. Our control automation systems and data collection strategies are able to measure and modify growing to help
growers learn how to use their resources more efficiently. It is not the lights you use; it is how you
use them. Learn more at VividGro.com.

CHIEF SERVICES SUPPORTEDCONSULTING• Custom LED grow lights,
automation, and controls• FlowerMax (6 channel)• FlowerMax Pro (8 channel)• GroNet (automation and control system)

MAJOR PRODUCTS

STATES SERVED• GroBar X (single channel)• GroMax (3 channel)

Nationwide

VividGro
113 N. May St.
Chicago, IL 60607
USA
EMAIL

sales@vividgro.com
LOCATIONS OF OTHEROFFICES AND FACILITIES

Cocoa Beach, FL
KEY PERSONNEL

Randy Shipley, VP of SalesDavid Friedman, CEO
Dawn Pogue, Customer
Experience Manager

vividgro.com

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FRITSCH Milling & Sizing, Inc.
COMPANY DESCRIPTIONMANUFACTURING& PROCESSINGANALYTICALINSTRUMENTSFRITSCH is an internationally respected German manufacturer of laboratory and production-scale instruments used for milling, particle size analysis, and sample handling. Serving abroad range of industries, including food, pharmaceuticals, agriculture, and nano-technology,
FRITSCH has worked closely with the medical cannabis industry to optimize a range of solutions
for use in production, quality control, and R&D.

PRIMARY APPLICATIONS SUPPORTEDREGIONS SERVED• Production milling—optimize particle
size to maximize extraction yield,
homogenize solid extracts andingredients, create Premium prerolls.
• Quality control—homogenize
edibles and plant samples to allow
representative subsampling• Particle size analysis of milled materials

Global

MAJOR PRODUCTS• PULVERISETTE 19—Precision
cutting mill system• PULVERISETTE 0—Vibratory
micro mill with cryoBox• ANALYSETTE 22 NanoTec—
Laser particle size analyzer

FRITSCH Milling& Sizing, Inc.
57 Grant Drive, Suite G
Pittsboro, NC 27312
USA
TELEPHONE(919) 229-0599
EMAIL

info@fritsch-us.com
LOCATIONS OF OTHEROFFICES AND FACILITIESGlobal Headquarters:
Idar-Oberstein, Germany
Company Offices:
USA, France, Russia,
Singapore, China
Local agency representatives
in all world regions

www.fritsch-us.com
www.cannabis-milling.com
FOUNDING SPONSOR

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Supplier Proﬁle

LGC Standards
COMPANY DESCRIPTIONMANUFACTURING& PROCESSINGLGC Standards is a global manufacturer and distributor of high quality reference materials witha portfolio of more than 100,000 certified reference materials, standards, and proficiency testing schemes for the pharmaceutical (Mikromol™), environmental (Dr. Ehrenstorfer™), cannabis,
food and beverage, forensic, clinical, industrial, and petrochemical markets. Our ISO accreditations include: ISO 9001, ISO 17034/ISO Guide 34, GMP/GLP, ISO 13485, ISO/IEC 17025, and ISO/IEC 17043.
As a designated National Measurement Institute (NMI) for chemical and bio-measurement, LGC
works in partnership with governments, intermediaries, and private sector organizations to address the measurement needs of key industries including healthcare, food, environmental, security, and energy.

MAJOR PRODUCTS
Dr. Ehrenstorfer™ offers a broad range ofstate-by-state cannabis impurity standards
as well as a full list of terpenes to meet yourstate’s requirements. We manufacture standards for the analysis of pesticide, solvent,heavy metal, mycotoxin, bacteria, and growth
regulator residues. All of our Dr. Ehrenstorfer™ brand mixes are certified reference materials manufactured in accordance with ISO
17034 requirements. Custom mixes are our
specialty.

STATES SERVED
Global

LGC Standards
276 Abby Road
Manchester, NH 03103
USA
TELEPHONE

Toll free: (888) 622-7660(603) 622-7660
Fax: (603) 622-5180
EMAIL

lgcusa@lgcstandards.com
KEY PERSONNELDon Shelly, Food andEnvironmental ProductManager
Adam Ross, Environmental,
Cannabis, Food &Beverage Specialist

https://us.lgcstandards.com

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Supplier Proﬁle75

PRO Scientific Inc.
COMPANY DESCRIPTIONMANUFACTURING
AND PROCESSINGANALYTICALINSTRUMENTS

PRO Scientific is a global leader in the manufacturing of homogenizers for both laboratory andindustrial labs requiring sample preparation. PRO homogenizers are able to homogenize various forms of cannabis material fast and efficiently.
From micro sample volumes to larger multi-liter processing, there is a PRO Homogenizer tosuit your needs. PRO Scientific even offers homogenizing solutions to address automated multi-sample homogenizing and OEM homogenizer needs too. All products manufactured by PRO
Scientific are backed with over 25 years of technical experience, unmatched customer support,
and made in the USA.

CHIEF SERVICES SUPPORTEDOTHERSERVICES

PRO Scientific is the ideal source for highquality homogenizing products for sample
preparation within the cannabis industry, providing assistance for both small startup andestablished labs with their cannabis testingand quality control. PRO Scientific homogenizers are precision homogenizers to assist in
determining and monitoring the cannabinoid
potency and pesticide residue. PRO Scientific Homogenizers are also ideal for the extraction of cannabis for the development of cannabis infused products. Homogenization of
cannabis samples allows for a stable emulsion
to be created that is shelf stable.

reliable, reproducible results that are required
for this industry. A range of setups are available depending upon your budget and processing requirements. Whether high speed
shearing to dispersing, homogenizing, emulsifying, mixing, or blending.
• Economical homogenizing package kits
• Handheld or stand mounted
homogenizer models• Digital and programmablebenchtop homogenizer models• Automated and semi-automatedhomogenizing systems• Precision crafted generator probes

STATES SERVEDMAJOR PRODUCTS
Our PRO Homogenizers and generator
probes are precision designed to provide

PRO Scientific supports labs in various industries that require sample preparation throughout the United States as well as internationally.

PRO Scientific Inc.
99 Willenbrock Road
Oxford, CT 06478
USA
TELEPHONE

Toll free: (800) 584-3776(203) 267-4600
Fax: (203) 267-4606
EMAIL

sales@proscientific.com
KEY PERSONNEL

Holly Yacko-Archibald,
Vice President
Brian Archibald, Business
Development Manager

www.proscientific.com

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Supplier ProﬁleVitalis Extraction Technology
COMPANY DESCRIPTIONMANUFACTURING& PROCESSINGEXTRACTION

Vitalis Extraction Technology Inc.© (Vitalis) is a
privately-owned, Kelowna-based engineeringand manufacturing company, producing thehighest-flowing industrial supercritical CO2
extraction systems for the cannabis industry.
Renowned for their reliability, scalability, andcontinuous operation, Vitalis systems are designed and manufactured in accordance withASME and CSA Standards for Boiler, Pressure
Vessel and Pressure Piping Code. The vessels are stamped with a CRN and NB registration number confirming that the vessels meetcode and have been examined by an Authorized Inspector. With systems on three continents, Vitalis has the most deployments of industrial CO2 supercritical extractors into thecannabis industry.

MAJOR PRODUCTS

Vitalis Extraction
Technology#102-480 Neave Court
Kelowna, BC
V1V 2M2
CanadaVitalis Extraction Technology is the leading
manufacturer of the most sophisticated industrial Supercritical CO2 extraction systems
in the world. Vitalis is Canada’s first and only
American Society of Mechanical Engineers(ASME) certified extraction original equipment manufacturer (OEM) in the cannabis

industry. Vitalis’ award-winning systems focus
on the key needs of any large-scale extraction business: reliability, component certification, and continuous 24/7 operation. Vitalis
systems were engineered to balance all threefundamentals, and the result is the highest
output of the purest full-spectrum oil possible
in the shortest amount of time in the CO2 extraction industry.
Vitalis produces three lines of CO2 extraction equipment: The F-Series, the Q-Series,
and the R-Series. The R-Series’ R-400 allows
for processing of up to 500 pounds of topquality material per day. With a heavy-duty
hydraulic pump, dual extraction lines, industrial grade CO2 recovery system, TrueCyclonic separation technology, and modular assembly for future scalability, the Vitalis system isbuilt for heavy-duty workloads, massive capacity, and continual growth. With a strict
focus on quality as well as a commitment toconstant research and development, Vitalis provides certified Supercritical CO2 extraction equipment that is redefining the capabilities of traditional extraction methodologies.

STATES SERVED
Global—systems deployed across North
America, South America, and Europe.

TELEPHONE

Toll free: (844) 248-2326(250) 864-4015
EMAIL

info@vitaliset.com
LOCATIONS OF OTHEROFFICES AND FACILITIESSales Office3314 Appaloossa Road
Kelowna, BC
V1V 2W5
Operations & Assembly
591 Gaston Avenue
Kelowna, BC
V1Y 7E6
KEY PERSONNEL

Pete Patterson, COO,
Cofounder
Joel Sherlock, Chairman,
Cofounder
James Seabrook,
CTO, Cofounderhttps://vitaliset.com/

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

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Supplier Proﬁle77

COMPLED Solutions GmbHCOMPANY DESCRIPTIONOTHERSERVICESCOMPLED was founded in 2010 and has become one of the pioneers in LED horticulture lighting. Since then COMPLED has been in the forefront of LED horticulture lighting for science applications. We develop, manufacture, and test exclusively in Germany. We have always been
focused on tunable light spectra because that’s the mayor advantage of LED technology. By dynamically tuning the spectrum it is possible to optimize yields as well as cannabinoid and terpene profiles. Furthermore, it is also crucial to align lighting recipes to all other relevant environmental parameters such as CO2, temperature, and so forth, and that’s actually also possible
with our technology.

CHIEF SERVICES SUPPORTED
Besides horticulture lighting design we alsooffer support in the development of lighting
and growing recipes, data science, and biological research related to lighting. Even customized lighting devices or spectra are available upon request. Please have a look at ourreferences(www.compled.de/pages/references.html).

MAJOR PRODUCTS
Our main product line is called the SUNsim
platform (www.compled.de/pages/products.
html#research_jump). It was designed especially for researchers who are interested in theimpact of the quantity and quality of light on
the development of plants. We offer several
solutions from 24 LED channels down to six
LED channels.
In addition, we are proud to offer our first
LED horticulture lighting platform especiallydesigned for cannabis cultivation, the HashCropter platform (www.hashcropter.com). It’s
the most flexible and effective LED lighting
platform for cannabis cultivation.
Spectral tuning is always obligatory andboth platforms are combinable.

STATES SERVED
Nationwide and worldwide.

COMPLED
Solutions GmbH
Dresden, Saxony, D-01324
Germany
TELEPHONE+49-351-873234-00
Fax: +49-351-873234-01
EMAIL

sales@compled.de
KEY PERSONNEL

Christoph Schubert, CEOwww.compled.de

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Supplier Proﬁle

LEAP PAL Parts +Consumables
COMPANY DESCRIPTIONOTHERSERVICESANALYTICALINSTRUMENTSANALYTICALTESTING LABMANUFACTURING& PROCESSING

PACKAGING &SUPPLIES

LEAP PAL Parts + Consumables has been helping customers in the lab instrumentation and liquid handling business for more than 25 years. We represent the highest quality products thatmeet strict quality assurance (QA) standards and work with the best manufacturers to offer innovative products at the most competitive prices. We provide same day shipping of all in-stock
products to avoid instrument downtime as well as reduce your on-hand inventory levels. Our
mission statement is: Be Good. Just that simple. Be good to our customers, our suppliers, ourcommunity, and to each other. Let us show you what thousands of customers already know.

CHIEF SERVICES SUPPORTED
We offer a complete range of consumables
for high pressure liquid chromatography, gas
chromatography, headspace, and sample
preparation. In addition to consumables, weoffer instrument specific small parts. As an
added service we also provide technical assistance by certified PAL, PAL-XT, PAL 3 service
technicians if you need urgent assistance withyour instruments.

MAJOR PRODUCTS
We provide syringes and syringe components, vials, caps and inserts including our
own L-MARK brand, instrument parts and accessories, valve components including rotors, valves, tubing, fittings and sample loops
as well as plates and cap mats. Our suppliers

include CTC Analytics, VALCO Instruments,
IDEX/Rheodyne, La-Pha-Pack and manyothers.

STATES SERVED
We serve all 50 states and Canada. Providing
products internationally and domestically, tocustomers in the following industries:• Biotechnology• Pharmaceutical• Clinical• Food and beverage• Environmental• Petrochemical• Cannabis analysis• Forensics• Toxicology

LEAP PAL Parts+Consumables
4216 Atlantic Ave.
Raleigh, NC 27604
USA
TELEPHONE

Toll free: 1-877-725-1007(919) 322-4208
Fax: (888) 589-9475
EMAIL

orders@palparts.com
KEY PERSONNEL

Lamar Jones, President
Kate Holub, VP of Sales
Angie Buchholz,
Marketing Director

www.palparts.com

CANNABIS SCIENCE AND TECHNOLOGY | www.CannabisScienceTech.com

VOL 1 • NO 4 • NOVEMBER/DECEMBER 2018

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