NPS Data Hub

A Web–based Community Driven

Analytical Data Repository for

New Psychoactive Substances

Aaron Urbas

Forensics @ NIST, Nov 8, 2018
Outline

 NPS Data Hub Concept

 NPS DH Inner Workings

 Where We Are So Far with the NPS DH

 NPS Related Activities

 NMR Spin System Analysis for Data

Verification

 Mixture Analysis with Raman Spectroscopy 
NPS Data Hub Concept

 Web-based data repository for

analytical data associated

with novel psychoactive

substances

 Goal is to be supported and

maintained by experts in the 

international forensic community

 Data integrity based on both peerreview and, when feasible,

objective data evaluations (e.g. 

Structure verification/confirmation

tools)

 Built on web-based ELN platform

Basic Database Architecture
Browsing Molecules and Search Results
Molecule Search Result Page (Detail View)
Adding New Molecules
Analytical Data Browsing
Integration with CSEARCH

 Evaluation of proposed structure 

with associated 13C assignments

 Based on SDF file format

(chemical structure + peak 

assignments)

 “Robot-referee” provides a fully 

automated, detailed report (HTML) 

evaluating proposed structure and 

associated 13C assignments.

 Report includes a qualitative 

valuation to accept, revise or 

completely reject proposed 

structure assignments. 

 Report stored along with analytical 

data 

http://nmrpredict.orc.univie.ac.at/ Predicted/Experimental Comparison Excerpt
Where Are We So Far 

 Approximately 400 registered users

 Database contains data related to 800+ substances

 Varying amounts of data, some compounds with 

NMR, EI-MS data, some with NMR, MS, IR/Raman,

some with MS peak tables only (RESPONSE)

 Compiling/collecting analytical data

(NMR, Raman so far) on a number (65)

of fentanyl analogs

 Currently sifting through data from >200

molecules provided by DEA STL

 Refining the interface to improve

usability

 ENFSI Drug Working Group on Databases

considering using Data Hub 
Can We Get More From 1H NMR Spectra?

 Wealth of structural information 

available

 Proton counts

 Chemical shift structure correlations

 Connectivity via couplings and coupling 

constants

 Indirect heteronuclear information 

through coupling, e.g. 19F

1

N

2

3

4

O

5

6

H C3

7

8

9

10

11

12

13

14

N

15

16

17

18

19

20

21

22

23

24

25

F

26

Predicted Chemical Shifts &

Coupling Constants

Para-fluorofentanyl

...
Outline

 NPS Data Hub Concept

 NPS DH Inner Workings

 Where We Are So Far with the NPS DH

 NPS Related Activities

 NMR Spin System Analysis for Data

Verification

 Mixture Analysis with Raman Spectroscopy 
Predicted 1H NMR Spectra

Measured

Predicted

δ(ppm)

Measured vs Predicted Para-Fluorofentanyl H Spectra (600 MHz)
1

N

2

3

4

O

5

6

H C3

7

8

9

10

11

12

13

14

N

15

16

17

18

19

20

21

22

23

24

25

F

26

Quantum Mechanic Spectral Analysis (QMSA)

......

Predicted Chemical Shifts &

Coupling Constants

Fit Chemical Shifts &

Coupling Constants

There are a total of 117 

chemical shifts and couplings 

being fit for this molecule, the 

tables only represent a subset.

Para-fluorofentanyl

Long story short....
1H QM Spectral Analysis @ 600 MHz Intensity

N

O

H C3

N

F

ClH

δ(ppm)

Para-fluorofentanyl
Field Translation of 1H Spectra

 Chemical shift (δ) is a unitless 

frequency ratio expressed in 

ppm that is independent of 

magnetic field strength

 Coupling constants (Hz) are 

field strength independent

 The End Result:

While the chemical shift of a 

proton resonance remains 

constant in ppm, the 

couplings and associated 

splitting patterns do not

 The QM spin system analysis 

is field independent and thus 

portable to any field for 

reproducing the spectral 

information

600

400

300

200

100

62

MHz

(1H)_

δ(ppm)

QM Model Evaluated at Various Field Strengths
Isomer Differentiation

On a Benchtop NMR 

ortho-fluorofentanyl

meta-fluorofentanyl

para-fluorofentanyl

• 600 MHz QMSA 1H Spectra

Translated to 62 MHz

• Experimental 62 MHz 1H Spectra
Butyrl Fentanyl Isomers (1H NMR, 62 MHz)
Raman Spectroscopy, Fluorofentanyl Isomers

ortho-fluorofentanyl (HCl)

meta-fluorofentanyl (HCl)

para-fluorofentanyl (HCl)

1064 nm Raman Spectra
Raman Mixture Analysis

r2 

0.948

0.928

0.931

0.959

0.963

0.937

Pure Component Spectra

Raman Data Set of Six

Component Cutting Agent Blend

Multivariate Curve

Resolution (MCR)

Extracted Spectra
Acknowledgements

NPS Data Hub

Torsten Schoenberger (Federal Criminal Police Office of Germany, BKA)

Charlotte Corbett (Drug Enforcement Administration, STRL)

Katrice Lippa (Chemical Sciences Division, NIST)

Felix Rudolphi (Sciformation Consulting Gmb, Bad Vilbel, Germany)

Wolfgang Robien (Department for Organic Chemistry, University of Vienna)

NMR QMSA & Benchtop NMR Work

Jonathan Duffy (Department of Forensic Sciences, George Washington University)

Ioan Marginean (Department of Forensic Sciences, George Washington University)

Matthias Niemitz (NMR Solutions Oy, Kuopio Finland)

Raman Spectroscopy

Peter Trask (Chemical Sciences Division, NIST)

Funding

NIST Special Programs Office

Thank You!