NISTIR 7880-26 

NIST Micronutrients Measurement 

Quality Assurance Program 

Winter, Spring, and Fall 1998 

Comparability Studies 

Results for Round Robin XLII, XLIII, and XLIV 

Fat-Soluble Vitamins and Carotenoids in Human Serum 

and Round Robin 11 Ascorbic Acid in Human Serum 

David L. Duewer 

Margaret C. Kline 

Sam A. Margolis (Retired) 

Katherine E. Sharpless 

Jeanice B. Thomas 

 

 

 

 

 

 

NISTIR 7880-26 

NIST Micronutrients Measurement 

Quality Assurance Program 

Winter, Spring, and Fall 1998 

Comparability Studies 

Results for Round Robin XLII, XLIII, and XLIV 

Fat-Soluble Vitamins and Carotenoids in Human Serum 

and Round Robin 11 Ascorbic Acid in Human Serum 

David L. Duewer 

Sam A. Margolis (Retired) 

Katherine E. Sharpless 

Jeanice B. Thomas 

Chemical Sciences Division 

Materials Measurement Laboratory 

Margaret C. Kline 

Biomolecular Measurement Division 

Material Measurement Laboratory 

July, 2013 

U.S. Department of Commerce 

Penny Pritzker, Secretary 

National Institute of Standards and Technology 

Patrick D. Gallagher, Under Secretary of Commerce for Standards and Technology and Director 
(This page intentionally blank) 

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Abstract 

The National Institute of Standards and Technology coordinates the Micronutrients Measurement 

Quality Assurance Program (MMQAP) for laboratories that measure fat- and water-soluble vitamins 

and carotenoids in human serum and plasma. This report describes the design of and results for the 

Winter, Spring and Fall 1998 MMQAP measurement comparability improvement studies: 1) Round 

Robin XLII Fat-Soluble Vitamins and Carotenoids in Human Serum, 2) Round Robin XLIII FatSoluble Vitamins and Carotenoids in Human Serum, 3) Round Robin XLIV Fat-Soluble Vitamins 

and Carotenoids in Human Serum, and 4) Round Robin 11 Ascorbic Acid in Human Serum. The 

materials for Round Robin XLII were shipped to participants in February 1998; participants were 

requested to provide their measurement results by April 3, 1998. The materials for Round Robin 

XLIII were shipped to participants in May 1998; participants were requested to provide their 

measurement results by June 22, 1998. The materials for Round Robin XLIV were shipped to 

participants in August 1998; participants were requested to provide their measurement results by 

October 9, 1998. The sample materials for Round Robin 11 were distributed in September 1998 

with results due by October 20, 1998. 

Keywords 

Human Serum
 

Retinol, α-Tocopherol, γ-Tocopherol, Total and Trans-β-Carotene
 

Ascorbic Acid, SRM 970
 

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Table of Contents 

Abstract............................................................................................................................................... iii
 

Keywords ............................................................................................................................................ iii
 

Table of Contents ............................................................................................................................... iv
 

Introduction......................................................................................................................................... 1
 

Round Robin XLII: Fat-Soluble Vitamins and Carotenoids in Human Serum .......................... 1
 

Round Robin XLIII: Fat-Soluble Vitamins and Carotenoids in Human Serum......................... 2
 

Round Robin XLIV: Fat-Soluble Vitamins and Carotenoids in Human Serum ......................... 2
 

Round Robin 11: Vitamin C in Human Serum............................................................................... 3
 

References ............................................................................................................................................ 3
 

Appendix A. Shipping Package Inserts for RR42........................................................................ A1
 

Appendix B. Final Report for RR42 ..............................................................................................B1
 

Appendix C. “All-Lab Report” for RR42 ......................................................................................C1
 

Appendix D. “Individualized Report” for RR42 ......................................................................... D1
 

Appendix E. Shipping Package Inserts for RR43 ......................................................................... E1
 

Appendix F. Final Report for RR43............................................................................................... F1
 

Appendix G. “All-Lab Report” for RR43...................................................................................... G1
 

Appendix H. “Individualized Report” for RR43 .......................................................................... H1
 

Appendix I. Shipping Package Inserts for RR44 ........................................................................... I1
 

Appendix J. Final Report for RR44 ................................................................................................ J1
 

Appendix K. “All-Lab Report” for RR44..................................................................................... K1
 

Appendix L. “Individualized Report” for RR44........................................................................... L1
 

Appendix M. Shipping Package Inserts for RR11 ....................................................................... M1
 

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Introduction 

Beginning in 1988, the National Institute of Standards and Technology (NIST) has coordinated the 

Micronutrients Measurement Quality Assurance Program (MMQAP) for laboratories that measure 

fat- and water-soluble vitamins and carotenoids in human serum and plasma. The MMQAP 

provides participants with measurement comparability assessment through use of interlaboratory 

studies, Standard Reference Materials (SRMs) and control materials, and methods development and 

validation. Serum-based samples with assigned values for the target analytes (retinol, alphatocopherol, gamma/beta-tocopherol, trans- and total beta-carotene, and total ascorbic acid) and 

performance-evaluation standards are distributed by NIST to laboratories for analysis. 

Participants use the methodology of their choice to determine analyte content in the control and 

study materials. Participants provide their data to NIST, where it is compiled and evaluated for 

trueness relative to the NIST value, within-laboratory precision, and concordance within the 

participant community. NIST provides the participants with a technical summary report concerning 

their performance for each exercise and suggestions for methods development and refinement. 

Participants who have concerns regarding their laboratory’s performance are encouraged to consult 

with the MMQAP coordinators. 

All MMQAP interlaboratory studies consist of individual units of batch-prepared samples that are 

distributed to each participant. For historical reasons these studies are referred to as “Round 

Robins”. The MMQAP program and the nature of its studies are described elsewhere. [1,2] 

Round Robin XLII: Fat-Soluble Vitamins and Carotenoids in Human Serum 

Participants in the MMQAP Fat-Soluble Vitamins and Carotenoids in Human Serum Round Robin 

XLII comparability study (hereafter referred to as RR42) received four lyophilized human serum test 

samples for analysis. Unless multiple vials were previously requested, participants received one vial 

of each serum. These sera were shipped on dry ice to participants in February 1998. The 

communication materials included in the sample shipment are provided in Appendix A. 

Participants are requested to report values for all fat-soluble vitamin-related analytes that are of 

interest to their organizations. Not all participants report values for the target analytes, and many 

participants report values for non-target analytes. 

The final report delivered to every participant in RR42 consists of three documents: 

•	 A cover letter for the current study, a brief description of the other document, and a 

discussion of our analysis of the overall results that may be of broad interest. This cover 

letter is reproduced as Appendix B. 

•	 The “All-Lab Report” that lists all of the reported measurement results, a number of 

consensus statistics for analytes reported by more than one participant, and the mean median 

and pooled SD from any prior distributions of the serum. This report also provides a 

numerical “score card” for each participant’s measurement comparability for the more 

commonly reported analytes. This report is reproduced as Appendix C. 

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•	 An “Individualized Report” that graphically analyzes each participant’s results for selected 

analytes. This report also provides a graphical summary of their measurement comparability. 

The graphical tools used in this report are described in detail elsewhere [3]. An example 

“Individualized Report” is reproduced as Appendix D. 

Round Robin XLIII: Fat-Soluble Vitamins and Carotenoids in Human Serum 

Participants in the MMQAP Fat-Soluble Vitamins and Carotenoids in Human Serum Round Robin 

XLIII comparability study (hereafter referred to as RR43) received four lyophilized human serum 

test samples for analysis. Unless multiple vials were previously requested, participants received one 

vial of each material. These sample materials were shipped on dry ice to participants in June 1998. 

The communication materials included in the sample shipment are provided in Appendix E. 

Participants are requested to report values for all fat-soluble vitamin-related analytes that are of 

interest to their organizations. Not all participants report values for the target analytes, and many 

participants report values for non-target analytes. 

The final report delivered to every participant in RR43 consists of three documents: 

•	 A cover letter for the current study, a brief description of the other document, and a 

discussion of our analysis of overall results that may be of broad interest. This cover letter is 

reproduced as Appendix F. 

•	 The “All-Lab Report” that lists all of the reported measurement results, a number of 

consensus statistics for analytes reported by more than one participant, and the mean median 

and pooled SD from any prior distributions of the serum. This report also provides a 

numerical “score card” for each participant’s measurement comparability for the more 

commonly reported analytes. This report is reproduced as Appendix G. 

•	 An “Individualized Report” that graphically analyzes each participant’s results for selected 

analytes. This report also provides a graphical summary of their measurement comparability. 

The graphical tools used in this report are described in detail elsewhere [3]. An example 

“Individualized Report” is reproduced as Appendix H. 

Round Robin XLIV: Fat-Soluble Vitamins and Carotenoids in Human Serum 

Participants in the MMQAP Fat-Soluble Vitamins and Carotenoids in Human Serum Round Robin 

XLIV comparability study (hereafter referred to as RR44) received four lyophilized human serum 

test samples for analysis. Unless multiple vials were previously requested, participants received one 

vial of each material. These sample materials were shipped on dry ice to participants in August 

1998. The communication materials included in the sample shipment are provided in Appendix G. 

Participants are requested to report values for all fat-soluble vitamin-related analytes that are of 

interest to their organizations. Not all participants report values for the target analytes, and many 

participants report values for non-target analytes. 

The final report delivered to every participant in RR43 consists of three documents: 

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•	 A cover letter for the current study, a brief description of the other document, and a 

discussion of our analysis of overall results that may be of broad interest. This cover letter is 

reproduced as Appendix H. 

•	 The “All-Lab Report” that lists all of the reported measurement results, a number of 

consensus statistics for analytes reported by more than one participant, and the mean median 

and pooled SD from any prior distributions of the serum. This report also provides a 

numerical “score card” for each participant’s measurement comparability for the more 

commonly reported analytes. This report is reproduced as Appendix I. 

•	 An “Individualized Report” that graphically analyzes each participant’s results for selected 

analytes. This report also provides a graphical summary of their measurement comparability. 

The graphical tools used in this report are described in detail elsewhere [3]. An example 

“Individualized Report” is reproduced as Appendix H. 

Round Robin 11: Vitamin C in Human Serum 

Participants in the MMQAP Vitamin C in Human Serum Round Robin 11 comparability study 

(hereafter referred to as RR11) received four frozen serum test samples and a solid ascorbic acid 

control material for analysis. The four test samples were stated to be duplicate ampoules of Levels 1 

and 2 of candidate SRM 970 Ascorbic Acid in Human Serum. These sample materials were shipped 

on dry ice to participants in September 1998. The communication materials included in the sample 

shipment are provided in Appendix M. 

The test materials were prepared by adding equal volumes of 10 % metaphosphoric acid (MPA) to 

human serum that had been spiked with ascorbic acid. Participants were asked to provide two 

results for each vial. Participants were also asked to prepare and evaluate a standard solution of 50 

μmol ascorbic acid (AA) per L solution of 5 % by mass metaphosphoric acid. 

No report on participant results was prepared for RR11 itself. A combined report on the results 

obtained in RR11 and/or in Round Robin 12 was prepared and reported to participants in August of 

1999. This report is presented in full in Appendix J in NISTIR 7880-25; Table 2 of this report is 

equivalent to the usual “All Lab Report” for RR11. 

References 

1 Duewer DL, Brown Thomas J, Kline MC, MacCrehan WA, Schaffer R, Sharpless KE, May WE, 

Crowell JA. NIST/NCI Micronutrients Measurement Quality Assurance Program: Measurement 

Repeatabilities and Reproducibilities for Fat-Soluble Vitamin-Related Compounds in Human 

Sera. Anal Chem 1997;69(7):1406-1413. 

2 Margolis SA, Duewer DL. Measurement Of Ascorbic Acid in Human Plasma and Serum: 

Stability, Intralaboratory Repeatability, and Interlaboratory Reproducibility. Clin Chem 

1996;42(8):1257-1262. 

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3 Duewer DL, Kline MC, Sharpless KE, Brown Thomas J, Gary KT, Sowell AL. Micronutrients 

Measurement Quality Assurance Program: Helping Participants Use Interlaboratory Comparison 

Exercise Results to Improve Their Long-Term Measurement Performance. Anal Chem 

1999;71(9):1870-1878. 

4
 
Appendix A. Shipping Package Inserts for RR42 

The following two items were included in each package shipped to an RR42 participant: 

• Cover letter 

• Datasheet 

The cover letter and datasheet were enclosed in a sealed waterproof bag along with the 

samples themselves. 

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~~·r~o ,STA1ES DEP.4RTMENT OF O'V'M~~c;E 

Natio1:ial 'h:mstitute of ~J:a ards and Te-chnalogy 

Gaithersburg, MatYland 20889-0001 

February 4, 1998 

Dear Colleague: 

Enclosed is the set of samples for the first quality assurance round robin exercise (Round Robin XLII) 

for FY98. You will find one vial of each of four lyophilized serum samples for analysis along with a 

form for reporting your results. When reporting your res_μlts, ptease stlbrflit one value for each analyte 

for a given serum sample. If an obtained value is below your limit of quantitation, please indic~te this 

result on the form by using NQ (Not Quantitated). For analytes not measured, please leave a blank. 

Results are due to NIST by April 3, 1998. Results received two weeks after the. due date will not be 

included in the summi:i.cy report for this round robin study. Written feedback concerning the study will 

be provided around April 30. 

Samples should be re~qfistitμted with l ,O mL of HPLC-grade water or equivalent. We recommend that 

dissolution be facilitated w~th 3 to 5 min agitation in an ultrasonic bath or at least 30 min. at room 

temp·eratμre with intetifiittent swirling. (CA:UTIClN: Vigorous shaking will cause fo~Uig 4P-d 

possibly in't fe~e wi~ accurate ~e~sll;retnent. The ru'Qqer stopp~ conprips phthalate esters that will 

leach iμto· the . s~inple 1:1poi1 ifi~~nrutteht cop.fact of the liquid· s~pJe with the ~opper. Th7se ·esters 

absorb strohgiy in the UV region a:ild elute very neat retifiol in i:n"ost UC systems creatii:tg analytical 

problems.) Pipette a known volume of setlim frotn the vial for analysis. (The final volume of the 

reconstituted sample is greater than 1.0 mL.). For consiste·ncy, we request that laboratories use the 

following absorptivities (E 1 % cm) ih ethanol: retinol, 1843 at 325 nm; retinyl .pl!,lμiitate, 975 at 325 

nm; a-tocopherol, 75.8 at 292 nm; y-tocbpJ"l.erol, 91.4 at 298 nm; a --carotene, 28'oo at 4_44 nfn (in 

hex~~e); ~--carotene, 2560 at 450 nm (in ethanol), 2592 at 452 run (in heXane); lycopehe, 3450 at 472 

nm (in hexane). 

Please mail or fax your results for Round Robin XLII to: 

Micronutrients Measurement Quality Assurance Program 

NIST , , . 

Bldg. 222, Rm. B208 

Gaithersburg, Mb 20899 

Fax: (301) 977--0685 

If you have questions regarding this round robin exercise, please call me at (301) 975-3120; 

e-mail me atjeanice.brownthomas@ilist.gov; or mail/fax queries to the above address. 

s~·-.cerely, 1 [}. _ fb· ~ ]k~ ~ Je' ; ce Brown Thonias 

Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

Enclosures . 

cc: S. Wise NUiil 

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NIST 

Micronutrients Measurement Quality Assurance Program 

Round Robin XLII Results from Laboratory #_____ 

Serum 

Analyte 239 240 241 242 Units* 

retinol 

retinyl palmitate 

α-tocopherol 

γ-tocopherol 

δ-tocopherol 

total β-carotene 

trans-β-carotene 

total cis-β-carotene 

total α-carotene 

trans-α-carotene 

total lycopene 

trans-lycopene 

β-cryptoxanthin 

α-cryptoxanthin 

lutein 

zeaxanthin 

lutein&zeaxanthin 

Other Analytes?
 

* We prefer mg/mL 

Today's Date: 

Comments? 

Mail: MMQAP, 222/B208 

NIST Please return results on-or-before Fax: 301-977-0685 

Gaithersburg, MD 20899 April 3, 1998 Email: David.Duewer@NIST.gov 

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Appendix B. Final Report for RR42 

The following eight pages are the final report as provided to all participants: 

•	 Cover letter 

•	 An information sheet that: 

o	 describes the contents of the “All-Lab” report 

o	 describes the nature of the test samples and details any previous distributions 

o	 summarizes aspects of the study that we believe may be of interest to the 

participants 

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May 28, 1998 

Dear Colleague: 

UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899-0001 

Enclosed is the summary report of the results for Round Robin XLII (RR42). Included in this 

report are: a summary of data for all laboratories; the measurement comparability summary for 

evaluating laboratory performance; a summary of individual laboratory performance for the past 

three years; a summary of the interlaboratory accuracy and precision over the same period of 

time for the measurement ofretinol, a- and y-tocopherol, and trans- and total ~-carotene; and a 

graphical summary of the NIST assigned value (NA V) vs. your laboratory value for these 

analytes. As in previous reports, the NIST assigned values are derived from the equally 

weighted results from the analyses performed by NIST and the laboratories that participated in 

this interlaboratory comparison exercise. 

We regret the delay in issuing this report. This year has been marked by both the sorrow of 

endings--Dave's mother passed away in late April-and the joy ofbeginnings--Kathy and her new 

baby are doing well! An interim report of interlaboratory median values was faxed (on April 10, 

about two weeks after the closing date) to all participants who had by then submitted quantitative 

values. 

The experimental design for this interlaboratory comparison exercise (RR42) is summarized in 

the attached report. The four serum samples (Sera 239-242) distributed are all new samples that 

were used to further evaluate our analyte augmentation techniques. These samples, however, 

were from an aged (about 10 years) serum pool which apparently caused some of the observed 

interferences. About 10% of the reporting laboratories indicated that they saw interferences in 

the retinol and/or tocopherol chromatographic region. As indicated in the attached report, we 

believe the interference is plasticizers extracted from one or more of the bags used to store the 

plasma units. While plasticizer contamination of samples is not an unexpected problem, 

recognition of such a contamination is an important consideration for method development and 

validation. We apologize for any incovenience that this may have caused. 

Data for evaluating laboratory performance in RR42 are provided in the comparability summary 

(Score Card) on page 6 of the "All Lab Report." Due to the observed interferences noted in this 

round robin exercise, the criteria used to evaluate laboratory performance are as follows: results 

rated A (within 1 SD of the assigned value) indicate EXCEPTIONAL performance, results rated 

B (within 2 SD) indicate ACCEPTABLE performance, results rated C (greater than 2 SD of the 

assigned value) are MARGINAL relative to the current state-of-the-practice for these 

measurements. 

If you have concerns regarding your laboratory performance, we suggest that you obtain a unit of 

SRM 968b, Fat-Soluble Vitamins and Cholesterol in Human Serum, and analyze all three levels. 

If, with minor modifications, your measured values do not agree with the certified values, we 

suggest that you contact us for consulta~on. 

NISI B2
 
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As you are aware, the intercomparison exercises for fat-soluble vitamins in human serum in 

which you are currently participating have been supported in part by the National Cancer 

Institute (NCI). Last September, our interagency agreement with NCI for the Micronutrient 

Measurement Quality Assurance (QA) Program expired. To date, NCI has not expressed interest 

in continuing support for this program. Because of the uncertainty of the funding since last 

October, NIST has committed to continue the intercomparison exercises through FY 98. We will 

keep you informed concerning the status of QA activities beyond 1998. 

Samples for RR43 were shipped during the first week of May. Results are due July 10; feedback 

to labs will be provided during the first week of August. 

If you have any questions regarding this report, please contact me at 301/975-3120; FAX: 

301/977-0685; e-mail: j eanice.brownthomas@nist.gov. 

sm:: i~JLmw ~ce Brown Thomas 

Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

cc: S. Wise 

Enclosures 

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Analysis of Results Round Robin XLII: Sera 239-242 

Analysis of NIST M2QAP Round Robin XLII Results: Sera 239 to 242 

Background. Four samples were distributed in RR42. 

Serum 239:a new serum, prepared from a composite of three plasma units purchased several 

years ago and stored since then at -80°C. The combined pool was mixed thoroughly and 

twice-filtered, but was otherwise unadulterated - at least by us! 

Page 1 

Serum 24l:a new serum, prepared from the same base material as Serum 239 but spiked with: 

retinyl palmitate, y-tocopherol, 0-tocopherol, trans-~-carotene, trans-ex-carotene, 

zeaxanthin, and trans-lycopene. 

Serum 242:a new serum, prepared from the same base material as Serum 239 but spiked with: 

retinal, retinyl palmitate, n-tocopherol, 0-tocopherol, trans-~-carotene, trans-a-carotene, 

lutein, and trans-~-cryptoxanthin. 

Serum 240: a new serum, prepared as a 1: 1 by volume blend of Sera 241 and 242. 

The spiking procedure used with Sera 241 and 242 adds no organic solvent and does not 

create non-extractable analyte-protein associations; however, it does dilute the non-spiked 

analytes by approximately 20% and may modify the lipoprotein composition. 

Qualitative Results. 

Interferences: About 20% of participants reported, either spontaneously or after we issued a 

"heads up" in the interim report, some degree of interference in the retinal and tocopherol 

retention zone of their chromatograms. The magnitude of the reported problems ranged 

from "we can't analyze these samples" to "an unusual baseline." Funher, two participants 

volunteered "We see nothing unusual." (On retrospective examination, our 

chromatograms have a "humpogram" baseline in the retinol/tocopherol retention zone.) 

From the preparation history, the quite diverse impact of the interferences, and 

examination of the chromatograms kindly provided by the afflicted participants, we 

believe the interference is plasticizers extracted from one or more of the bags the plasma 

units were supplied I stored I thawed in. Unfonunately, the bags themselves are long since 

disposed of so this must remain a working hypothesis. The erratic impact of the 

plasticizer is attributed to differences among your extraction, chromatography, and 

detection systems. 

Action: Plasticizer contamination of samples is a "not unexpected" problem. Whether or 

not quantitative results can be obtained in the presence of interferences, 

recognition of such problems is an imponant consideration for method 

development and validation. Everyone who recognized that their results for these 

samples were questionable deserves a gold star! 

While we apologize for having the same interferences in all four samples, we 

consider all four to be "valid." Serum 239 is no more, but you may see Sera 240, 

241, and 242 again (but not all at the same time!). Now that we know what to 

look for, we intend to examine the historical data/archived chromatograms for 

evidence interference in previous samples. 

In recognition of the unusual nature of the four sera distributed in RR42, we have 

modified our "grading scheme" from four levels (1-4) to three (A-C). 

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Analysis of Results Round Robin XLII: Sera 239-242 Page 2 

"Lutein&Zeaxanthin": One of our participants recently tried to make sense of the various 

"Lutein'', "Zeaxanthin", and "Lutein&Zeaxanthin" data we've been reponing and found it 

all very confusing. About half of the panicipants who repon the composite analyte 

"Lutein&Zeaxanthin" do not repon either of the component analytes. Only about half of 

the participants who do repon both "Lutein" and "Zeaxanthin" also explicitly repon 

"Lutein&Zeaxanthin". While some of these participants clearly estimate the composite 

independently, others appear to calculate it as the simple sum of the components. 

Action: As we stated some time ago, we calculate "Lutein&Zeaxanthin" results as the 

simple sum of the constituents whenever both "Lutein" and "Zeaxanthin" are 

reponed. As of RR 42, we distinguish between explicitly reponed values for 

"Lutein&Zeaxanthin" and values that~ calculate from the components: the 

explicitly reponed values are in standard font, our calculated values are italicized. 

Quantitative Results. The following NIST Data and V alue/Uncenainty Assignments table 

presents all NIST data, summary statistics for the NIST data, summary results for RR42, and 

the NIST assigned values and uncertainties. Since one of the two NIST analysts had higher 

priority responsibilities during the past several months, these statistics reflect results from only 

one NIST chromatographic system. The entries are defined as follows: 

NIST Data and Summary Statistics 

A: 1 to C:2 two aliquots ("I" and "2") of three vials (A, B, and C) of each serum were 

extracted and analyzed. 

n number of quantitative values for this analyte for this serum 

MeanNIST arithmetic average 

SD simple standard deviation 

SDrcp within-vial pooled standard deviation, reflecting variation in extraction, 

chromatography, peak integration, etc. 

SDhci among-sample standard deviation, reflecting heterogeneity in preparing and 

reconstituting the serum samples 

SDNIST ~SD~+ SD~e1 , total standard deviation. 

CV NIST 100 x SDNisrfMeanNisT 

Round Robin XLII Summary Statistics 

nn number of non-NIST laboratories reponing quantitative values for this analyte 

for this serum in this Round Robin 

Mediann median of the reponed values 

eSDn 0.741 x InterQuartile Range (IQR) 

SD11bs ~eSD! - SD~sT, the residual non-NIST interlaboratory biases after correction 

for measurement-, sample-, and NIST-analyst-related sources of variance. When 

SDNIST is greater than eSDn, SD1.bs = 0. 

CV 1.abl 100 x SD11bc/Medial\ 

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Analysis of Results Round Robin XLII: Sera 239-242 

NIST Assi~ned Yalues and Uncertainties 

NA V (Mean11.1s-r + Mediann) I 2, our best guess of the "true" analyte level 

NAU Maximum(0.05 x NAV, ~SD~ST + SD~11s ), our best guess for the "true" 

interlaboratory standard deviation characterizing measurement, sample 

heterogeneity, inter-analyst, and interlaboratory sources of variation. 

CV lOOx NAU /NAY 

Expected Interlaboratory Uncertainties 

Page 3 

eCV 100 x ~L~c + (~ 0 x NA V~1 )

2 /NA V where Lqc• , and 1 are empirical constants 

describing historical results (Duewer et al, Anal Chem 1997:69;1406-1413.) 

Measurement Performance Summary. 

Measurement Variability: The observed CVs are larger than expected for y-tocopherol, trans­ ~-carotene, and total a-carotene. They are about as expected for retinol, a-tocopherol, 

total ~-carotene, and ~-cryptoxanthin. The approximately 100% increase in theytocopherol CV is likely related to plasticizer interference. The 50% increase in the a.­

carotene CV is less plausibly related to plasticizers, and may represent interferences from 

one or more of the spiking solutions and/or underestimation of the "true" expected 

analytical variability. 

Expected Results: The design of the analyte spiking protocol allows the prediction of relative 

analyte levels among the sera. The expected levels are: 

retinol, a-tocopherol, ~-cryptoxanthin, and lutein ... 

Serum 242 ... highest level (from analyte-specific spikes) 

Serum 241. .. lowest level (from -15% dilution by spikes of other analytes) 

Serum 240 ... average of Serum 242 and Serum 241 levels 

Serum 239 ... somewhere between levels of Serum 241 and Serum 240 

y-tocopherol, trans-lycopene, and zeaxanthin ... 

Serum 242 ... lowest level (from -21 % dilution by spikes of other analytes) 

Serum 241. .. highest level (from analyte-specific spikes) 

Serum 240 ... average of Serum 242 and Serum 241 levels 

Serum 239 ... somewhere between levels of Serum 241 and Serum 240 

retinyl palmitate, 8-tocopherol, trans-~arotene, and "lutein&zeaxanthin" ... 

Serum 242 ... highest level (larger analyte-specific spikes) 

Serum 241 ... next-to-lowest level (smaller analyte-specific spikes) 

Serum 240 ... average of Serum 242 and Serum 241 levels 

Serum 239 ... lowest level 

trans-a-carotene ... 

Serum 242 ... next-to-lowest level (smaller analyte-specific spike) 

Serum 241 ... highest level (larger analyte-specific spike) 

Serum 240 ... average of Serum 242 and Serum 241 levels 

Serum 239 ... lowest level 

any other analyte you may have analyzed ... 

Serum 242 ... lowest level (-21 % dilution) 

Serum 241. .. next to highest level (-15% dilution) 

Serum 240 ... average of Serum 242 and Serum 241 levels 

Serum 239 ... highest level 

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[ 

D 

[ 

[ 

[ 

c 

c 

c 

[ 

[ 

Analysis of Results Round Robin XLII: Sera 239-242 Page 4 

Observed Results: Too few results are available to evaluate retinyl palmitate, o-tocopherol, 

and the "any other" analytes. For those analytes displayed in the boxplot comparisons 

(pages 2 and 3 of your Individualized Report), the observed results are as follows: 

Fully as expected..... retinol, a-tocopherol, y-tocopherol, ~-cryptoxanthin 

Nearly as expected .. . ~-carotene, a-carotene, lutein, and "lutein&zeaxanthin". The 

median analyte levels in Serum 240 are slightly larger than the average of medians 

for Sera 241 and 242. Further, the observed "high spike" analyte levels were less 

than expected. 

Unexpected ............ lycopene, where the levels are virtually are the same for all 

sera, and zeaxanthin, where the Serum 240 level is highest. 

Actions: Some.iraction of the carotenoid analytes continue to be lost and/or nonextractably bound in "high spike" sera, keeping us from achieving our 95% 

population targets. If analytical resources become available, we will continue to 

(attempt to) refine our augmentation techniques. 

The lycopene spike either was irrecoverably bound or degraded 

before/during/after lyophilization. If analytical resources become available, we 

will address this problem before attempting any further multi-analyte 

augmentation. 

The elevated Serum 240 zeaxanthin result is inexplicable. All analysts reporting 

zeaxanthin uniformly found a higher level in Serum 240 .than in either of it's 

constituent components! In our chromatograms the putative "lutein" and 

"zeaxanthin" peaks are well resolved, more-or-less typically shaped, and have 

characteristic retention times, thus we do not believe that chromatographic 

resolution is the cause of the problem (although it may contribute to the 

increased variability of the Serum 240 result relative to Sera 241 and 242). If 

analytical resources become available, we will certainly pursue this puzzle! 

Right now, though, we're clueless as to what might be going on. Any ideas? 

"\_, 

J-""'r-l~~A.._ - ~tu_,1.,v~ 

Dave Duewer 

Research Chemist 

David.Duewer@NIST.gov 

__.~, , ._///~ 

/ / /r~/Z{U....-

Margaret Kline 

Research Biologist 

Margaret.Kline@NIST.gov 

B7
 
r: Ll LJ LJ [-=:J LJ lJ LJ CJ ~ ITJ rJ ~ lJ CJ 

NIST Data and Value/Uncertainty Assignments 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n. 

MeanNJST 

SD 

SDn:o 

SD11c, 

239 

Retinol 

NIST I 

240 241 242 

0.536 0.697 0.412 0.976 

0.529 0.711 0.402 0.973 

0.545 0.680 0.414 0.914 

0.531 0.705 0.431 0.881 

0.544 0.638 0.419 1.095 

0.507 0.696 0.410 0.884 

6 6 6 6 

0.532 0.688 0.415 0.954 

0.014 0.027 0.010 0.081 

O.Dl 7 0.026 0.009 0.087 

0.006 0.019 0.008 0.049 

SDNIST 0.018 0.032 0.012 0.100 

CVNIST 3.3 4.7 2.9 11 

RRXLil 

239 240 241 242 

n. 44 44 44 44 

Median. 0.507 0.704 0.436 0.909 

eSD. 0.047 0.053 0.045 0.088 

a-Tocopherol 

NISTl 

239 240 241 242 

7.35 14.9 6.63 19.8 

7.26 14.7 5.76 20.0 

7.34 14.3 6.49 19.2 

6.87 14.2 6.62 20.5 

6.92 13.4 6.85 23.8 

7.27 14.0 7.42 17.3 

6 6 6 6 

7.17 14.2 6.63 20.1 

0.22 0.5 0.54 2.1 

0.24 0.2 0.43 2.7 

0.12 0.5 0.47 0.4 

0.27 0.6 0.64 2.7 

3.8 4.2 9.7 13 

RRXLII 

239 240 241 242 

44 44 44 44 

7.83 14.2 6.42 20.9 

0.64 1.3 0.50 1.7 

SD1ai.r·043 0.042 0.044 

~II ~! 1.1 0 

~I 7.9 0 CV • 1 8.5 5.9 IO 

NA V 0.520 0.696 0.425 0.931 7.50 14.2 6.52 20.5 

NAU 0.047 0.053 0.045 0.100 0.64 1.3 0.64 2.7 

CV 9.0 7.6 11 11 8.5 9.0 9.8 13 

eCV 8.8 8.8 8.9 9.0 7.7 7.3 8.2 7.7 

y-Tocopherol 

NISTl 

239 240 241 242 

1.78 3.19 3.55 1.76 

l.58 2.50 3.53 1.86 

1.64 2.82 3 .60 2.19 

l.75 2.76 3.37 l.83 

l.72 2.89 3.18 1.94 

l.74 2.78 3.32 l.96 

6 6 6 6 

l.70 2.82 3.43 1.92 

0.07 0.22 0.16 0.15 

0.09 0.29 0.11 0.15 

0.02 0.03 0.15 0.10 

0.09 0.29 0.19 0.19 

5.5 10 5.5 9.7 

RRXLII 

239 240 241 242 

21 21 21 21 

1.58 2.89 3.65 1.67 

0.24 0.43 0.53 0.25 

Total f3-Carotene 

NISTI 

239 240 241 242 

0.089 0.522 0.196 0.798 

0.094 0.526 0.194 0.849 

0.086 0 638 . TU/ 0.684 

0.086 0.657 0.194 0.711 

0.087 0.600 0.192 0.769 

0.088 0.631 0.188 0.709 

6 6 5 6 

0.088 0.595 0.193 0.753 

0.003 0.058 0.003 0.063 

0.002 0.015 0.002 0.034 

0.003 0.064 0.003 0.064 

0.004 0.066 0.003 0.073 

4.0 11 1.7 9.6 

RRXLII 

239 240 241 242 

29 29 29 29 

0.073 0.472 0.173 0.626 

0.016 0.059 0.034 0.082 

0.22 0.33 0.50 0.17 I 0.016 

14 11 14 10 22 

0 0.034 0.0371 

0 20 5.9 

1.64 2.86 3.54 1.80 0.081 0.534 0.183 0.690 

0.24 0.43 0.53 0.25 0.016 0.066 0.034 0.082 

15 15 15 14 20 12 19 12 

9.3 7.8 7.5 8.9 23 15 19 14 

trans

239 2

0.081 0

0.082 0

0.077 0

0.078 0

0.087 0

0.081 0

6 

0.081 0

0.003 0

0.002 0

0.003 0

0.004 0

4.8 

239 2

8 

0.074 0

0.004 0

0.000 0

0.7 

0.077 0

0.004 0

5.1 

12 

B8
rJ ll ll LJ r-J LJ Ll r=J CJ LJ IT:1 [ ~ c-=-1 c-::i Cl 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

Total a-Carotene 

NISTI 

239 240 241 242 

nd 0.225 0.288 0.073 

nd 0.231 0.291 0.081 

nd 0.250 0.206 0.067 

nd 0.239 0.255 0.072 

nd 0.192 0.301 0.062 

nd 0.224 0.280 0.077 

0 6 6 6 

0.227 0.270 0.072 

0.020 0.035 0.007 

0.014 0.021 0.007 

0.018 0.034 0.004 

NIST Data and Value/Uncertainty Assignments 

13-Cryptoxanthin 

NIST3 -

239 240 241 242 

0.067 0.141 0.070 0.178 

0.064 0.147 0.068 0.186 

0.065 0.146 0.067 0.170 

0.066 0.149 0.075 0.168 

0.065 0.138 0.078 0.184 

0.063 0.146 0.072 0.178 

6 6 6 6 

0.065 0.144 0.072 0.177 

0.001 0.004 0.004 0.007 

0.002 0.005 0.004 0.004 

0.001 0.003 0.003 0.007 

"Lutein" 

NIST3 -

239 240 241 242 

0.060 0.312 0.051 0.553 

0.061 0.313 0.047 0.521 

0.063 0.300 0.059 0.517 

0.059 0.296 0.049 0.484 

0.063 0.279 0.050 0.597 

0.059 0.296 0.054 0.488 

6 6 6 6 

0.061 0.299 0.052 0.527 

0.002 0.013 0.004 0.043 

0.002 0.007 0.005 0.048 

0 001 . 0.012 0.002 0.023 

239 

"Zeaxanthin" 

NIST3 -

240 241 242 

0.037 0.236 0.126 0.064 

0.037 0.223 0.126 0.048 

0.029 0.233 0.153 0.057 

0.029 0.218 0.123 0.051 

0.029 0.225 0.122 0.053 

0.025 0.220 0.124 0.048 

6 6 6 6 

0 031 . 0.226 0.129 0.053 

0.005 0.007 0.012 0.006 

0.002 0.008 0.012 0.007 

0.005 0.004 0.008 0.003 

"Lu

239 

0.09

0.0

0.09

0.0

0.09

0.0

0.09

0.00

0.00

0 00. 

n, 

MeanNIST 

SD 

SD,.. 

so .... s~ 

CVNIST 

0.023 0.041 0.008 0.002 0.005 0.005 0.008 0.002 O.ot5 0.005 0.053 0.005 0.009 0.014 0.008 0.00

10 15 11 2.7 3.6 7.3 4.5 4.1 4.9 10 10 18 4.0 11 15 6

RRXLII RRXLII RRXLII RR XL II 

239 240 241 242 239 240 241 242 239 240 241 242 239 240 241 242 239 

n. 21 24 24 24 24 24 24 24 12 12 12 11 10 10 10 8 2

Median,. 0.013 0.230 0.304 0.086 0.072 0.111 0.060 0.142 0.062 0.241 0.046 0.397 0.028 0.171 0.108 0.050 0.09

eSD, 0.006 0.076 0.100 0.028 0.016 0.022 0.013 0.034 0.010 0.026 0.014 0.041 0.005 0.080 0.025 0.013 0.0

sni... o.006 0.012 o.092 0.021 0.016 0.021 0.012 0.033 0.010 0.022 0.013 0 0 0.080 0.021 0.011 0.00

cvlaba 46 31 30 31 22 19 20 23 15 8.9 29 0 0 47 19 21 9

NA V 0.013 0.229 0.287 0.079 0.069 0.128 0.066 0.160 0.061 0.270 0.049 0.462 0.029 0.199 0.118 0.052 0.09

NAU 0.006 0.076 0.100 0.028 0.016 0.022 0.013 0.034 0.010 0.026 0.014 0.053 0.005 0.080 0.025 0.013 O.oI 

CV 46 33 35 35 23 17 20 21 16 9.6 29 12 18 40 21 26 

eCV 37 25 25 27 26 23 26 22 

B9
 

 

Appendix C. “All-Lab Report” for RR42 

The following six pages are the “All-Lab Report” as provided to all participants, with two 

exceptions: 

• the participant identifiers (Lab) have been altered. 

• the order in which the participant results are listed has been altered. 

The data summary in the “All-Lab Report” has been altered to ensure confidentiality of 

identification codes assigned to laboratories. The only attributed results are those 

reported by NIST. The NIST results are not used in the assessment of the consensus 

summary results of the study. 

C1
 
 

Round Robin XLII Laboratory Results 

All values in μg/mL 

Lab 239 

Retinol 

240 241 242 

Retinyl Palmitate α-Tocopherol γ-Tocopherol δ-Tocopherol 

FSV-BA 0.501 0.727 0.432 0.93 

FSV-BD 0.512 0.697 0.442 0.91 

FSV-BE 0.510 0.700 0.400 0.88 

FSV-BF 0.549 0.725 0.513 0.94 

FSV-BG 0.538 0.756 0.452 0.98 

FSV-BH 0.537 0.715 0.455 0.96 

FSV-BI 0.476 0.658 0.390 0.87 

FSV-BJ 0.472 0.690 0.412 0.90 

FSV-BK 0.491 0.707 0.437 0.87 

FSV-BL 0.520 0.720 0.460 0.92 

FSV-BM 0.537 0.694 0.430 0.92 

FSV-BN 0.458 0.667 0.392 0.84 

FSV-BO 0.444 0.616 0.358 0.80 

FSV-BP 0.357 0.624 0.326 0.57 

FSV-BQ 0.568 0.724 0.475 0.98 

FSV-BR 0.530 0.720 0.430 0.92 

FSV-BS 0.507 0.647 0.446 0.83 

FSV-BU 0.645 0.693 0.475 0.92 

FSV-BV 0.610 0.810 0.470 0.99 

FSV-BW 0.475 0.688 0.380 0.90 

FSV-BZ 

FSV-CB 0.417 0.632 0.360 0.80 

FSV-CBa 0.560 0.830 0.560 0.98 

FSV-CC 0.507 0.699 0.499 0.87 

FSV-CD 0.453 0.669 0.433 0.85 

FSV-CE 0.507 0.707 0.434 0.91 

FSV-CF 0.526 0.750 0.454 1.00 

FSV-CH 0.421 0.552 0.395 0.80 

FSV-CI 0.570 0.770 0.450 0.99 

FSV-CK 0.696 0.736 0.516 1.17 

FSV-CL 0.363 0.469 0.307 0.62 

FSV-CM 

FSV-CN 0.506 0.718 0.418 0.97 

FSV-CP 

FSV-CQ 0.500 0.713 0.443 0.97 

FSV-CR 0.520 0.700 0.460 0.80 

FSV-CS 0.464 0.636 0.365 0.87 

FSV-CT 0.541 0.777 0.459 1.06 

FSV-CU 0.458 0.643 0.394 0.80 

FSV-CX 0.500 0.750 0.420 0.93 

FSV-DB 0.518 0.757 0.502 1.02 

FSV-DF 0.510 0.800 0.460 1.03 

FSV-DJ 0.510 0.720 0.430 0.92 

FSV-DK 0.450 0.650 0.360 0.85 

FSV-DP 0.485 0.677 0.425 0.89 

FSV-DR 0.532 0.751 0.440 0.97 

FSV-DW 0.493 0.663 0.440 0.86 

FSV-EM 0.570 0.800 0.550 0.89 

FSV-ES 0.475 0.696 0.406 0.88 

FSV-FG 0.610 0.830 0.640 1.02 

FSV-FH 

239 240 241 242 

0.059 0.070 0.056 0.067 

0.037 0.054 0.035 0.068 

nq nq nq nq 

nd nd nd nd 

nq nq nq nq 

0.013 0.035 0.023 0.045 

nq 0.016 nq 0.017 

0.070 0.111 0.109 0.131 

0.070 0.080 0.070 0.090 

0.058 0.068 0.054 0.071 

0.050 0.070 0.050 0.050 

0.004 0.006 nq 0.005 

239 240 241 242 

7.9 13.8 6.0 20.6 

6.7 13.1 5.3 19.4 

7.6 13.5 6.2 19.7 

8.0 14.1 6.2 21.7 

8.2 14.9 6.8 22.2 

8.2 14.9 6.7 21.7 

7.3 13.8 6.0 20.1 

8.3 14.7 6.5 21.7 

7.5 14.7 6.2 20.0 

8.2 15.1 5.6 21.5 

7.7 14.5 6.3 21.3 

8.0 15.4 6.4 22.2 

6.7 11.8 5.2 17.3 

7.4 9.8 6.5 12.8 

7.9 14.2 6.9 20.9 

7.2 13.1 6.5 20.4 

8.6 15.8 6.7 22.1 

7.4 14.0 5.3 20.6 

8.4 13.8 8.1 20.9 

5.6 11.5 4.7 16.2 

7.4 14.5 6.4 20.4 

7.5 14.2 6.3 20.7 

8.2 14.8 6.7 22.1 

8.4 15.3 6.4 21.5 

8.5 14.1 6.9 21.9 

6.8 11.6 6.3 18.3 

6.8 12.4 5.4 18.7 

10.5 15.1 7.8 26.2 

7.8 12.5 6.8 18.8 

4.1 13.7 5.0 19.6 

7.3 15.6 6.4 23.1 

7.9 13.8 6.4 20.0 

7.9 15.2 6.6 21.6 

6.6 11.7 5.4 18.5 

7.5 14.8 6.5 22.3 

9.5 16.8 7.2 27.2 

7.1 13.3 5.4 17.9 

8.0 15.9 6.6 22.2 

8.5 15.3 7.1 23.0 

9.2 16.0 7.2 21.0 

7.5 13.8 5.9 20.3 

8.0 14.7 6.5 22.0 

8.6 14.8 7.0 20.0 

7.2 12.8 5.5 18.3 

8.1 14.7 6.6 21.4 

6.6 12.6 5.2 17.8 

nq : Interfering peaks 

239 240 241 242 

1.56 2.84 3.32 1.78 

1.40 2.70 3.50 1.50 

1.55 2.88 3.65 1.66 

1.61 3.02 3.85 1.67 

1.83 3.55 4.57 1.99 

1.41 2.69 3.40 1.61 

1.67 3.14 4.16 1.84 

1.34 2.71 3.35 1.40 

1.67 2.71 3.51 1.59 

1.73 3.59 4.20 1.78 

1.73 3.40 4.16 1.75 

2.30 3.10 4.60 3.20 

1.41 2.77 3.61 1.49 

1.05 2.09 2.91 1.19 

2.08 3.30 5.08 2.17 

1.14 1.91 2.96 0.80 

1.23 2.81 3.45 1.23 

1.75 3.20 3.72 2.14 

1.34 2.89 3.51 1.64 

1.58 3.48 4.16 1.98 

1.61 3.41 4.18 1.73 

239 240 241 242 

nq 0.301 0.105 0.587 

<0.3 0.400 0.400 0.800 

0.030 0.530 0.010 0.840 

n 47 47 47 47 8 9 7 9 46 46 46 46 21 21 21 21 1 3 3 

Min 0.357 0.469 0.307 0.57 0.004 0.006 0.023 0.005 4.1 9.8 4.7 12.8 1.05 1.91 2.91 0.80 0.301 0.010 0.587 

Median 0.507 0.707 0.437 0.91 0.054 0.068 0.054 0.067 7.8 14.2 6.4 20.8 1.58 2.89 3.65 1.67 0.030 0.400 0.105 0.800 

Max 0.696 0.830 0.640 1.17 0.070 0.111 0.109 0.131 10.5 16.8 8.1 27.2 2.30 3.59 5.08 3.20 0.530 0.400 0.840 

eSD 0.046 0.059 0.037 0.08 0.024 0.021 0.024 0.033 0.7 1.2 0.5 1.7 0.25 0.31 0.49 0.26 

eCV 9 8 8 9 44 31 44 49 8 9 8 8 16 11 13 15 

NISTa 0.532 0.688 0.415 0.95 7.2 14.2 6.6 20.1 1.70 2.82 3.43 1.92
 

NAV
 0.520 0.698 0.426 0.93 0.054 0.068 0.054 0.067 7.5 14.2 6.5 20.4 1.64 2.86 3.54 1.80
 

NAU
 0.049 0.060 0.045 0.10 0.024 0.021 0.024 0.033 0.8 1.2 0.7 2.8 0.26 0.44 0.56 0.31 

All Lab Report C2 Page 1 / 6 

3 
 

Round Robin XLII Laboratory Results 

All values in μg/mL 

Total β-Carotene trans-β-Carotene Total cis-β-Carotene Total α-Carotene 

Lab 239 240 241 242 239 240 241 242 239 240 241 242 239 240 241 242 

FSV-BA 0.088 0.45 0.180 0.63 0.081 0.436 0.172 0.60 0.007 0.018 0.008 0.027 0.013 0.153 0.235 0.077 

FSV-BD !0.099 !0.66 !0.256 !0.86 

FSV-BE 0.099 0.56 0.145 0.63
 

FSV-BF
 0.074 0.42 0.120 0.63 0.018 0.340 0.494 0.121 

FSV-BG 0.090 0.61 0.205 0.70 0.022 0.021 0.308 0.089 

FSV-BH 0.073 0.47 0.190 0.67 0.073 0.449 0.190 0.65 nq 0.019 nq 0.024 0.014 0.268 0.439 0.123 

FSV-BI 0.072 0.53 0.169 0.68 0.012 0.197 0.280 0.086 

FSV-BJ 0.098 0.50 0.195 0.73 nq 0.163 0.242 0.082 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.103 0.60 0.204 0.56 0.077 0.560 0.189 0.52 0.002 0.013 0.003 0.014 0.006 0.194 0.245 0.065 

FSV-BO 0.048 0.44 0.101 0.41 nq 0.164 0.251 0.068 

FSV-BP 0.100 0.48 0.288 0.58
 

FSV-BQ
 

FSV-BR
 

FSV-BS
 0.095 0.51 0.186 0.71 0.020 0.248 0.377 0.060 

FSV-BU 0.071 0.49 0.181 0.63 0.017 0.253 0.343 0.097 

FSV-BV 0.071 0.41 0.150 0.67 0.021 0.290 0.500 0.126 

FSV-BW 0.048 0.36 0.110 0.59 0.013 0.230 0.420 0.102 

FSV-BZ >0.087 >0.480 >0.190 >0.430 0.087 0.480 0.190 0.43 nd nd nd 0.010 0.027 0.230 0.250 0.086 

FSV-CB 0.052 0.39 0.136 0.41 0.013 0.159 0.230 0.067 

FSV-CBa 

FSV-CC 

FSV-CD 0.060 0.42 0.160 0.61 0.011 0.157 0.210 0.065 

FSV-CE 0.092 0.62 0.208 0.80
 

FSV-CF
 

FSV-CH
 0.059 0.50 0.167 0.68 0.002 0.255 0.357 0.074 

FSV-CI
 

FSV-CK
 0.081 0.38 0.129 0.61 0.021 0.279 0.301 0.118 

FSV-CL 0.071 0.41 0.142 0.54 0.018 0.249 0.404 0.109 

FSV-CM 

FSV-CN >0.073 >0.570 >0.177 >0.784 0.073 0.570 0.177 0.78 nq 0.258 0.348 0.083 

FSV-CP 0.079 0.50 0.191 0.74 0.012 0.268 0.346 0.100 

FSV-CQ 0.067 0.46 0.164 0.75
 

FSV-CR
 

FSV-CS
 0.071 0.57 0.188 0.70 0.064 0.523 0.169 0.64 0.007 0.045 0.019 0.054 0.013 0.305 0.425 0.113 

FSV-CT 0.077 0.50 0.186 0.75
 

FSV-CU
 0.066 0.44 0.138 0.59
 

FSV-CX
 0.060 0.39 0.180 0.48 0.010 0.150 0.280 0.080 

FSV-DB 0.049 0.34 0.137 0.49
 

FSV-DF
 

FSV-DJ
 

FSV-DK
 0.077 0.47 0.173 0.62 0.006 0.119 0.215 0.047 

FSV-DP 

FSV-DR 0.078 0.47 0.176 0.61 

FSV-DW 0.090 0.45 0.157 0.43 0.085 0.427 0.149 0.40 0.005 0.019 0.008 0.026 0.025 0.160 0.330 0.120 

FSV-EM >0.074 >0.386 >0.174 >0.572 0.074 0.386 0.174 0.57 0.028 0.156 0.277 0.294 

FSV-ES >0.072 >0.476 >0.172 >0.472 0.072 0.476 0.172 0.47
 

FSV-FG
 

FSV-FH
 

n 30 30 30 30 9 9 9 9 4 5 4 6 22 25 25 25 

Min 0.048 0.34 0.101 0.41 0.064 0.386 0.149 0.40 0.002 0.013 0.003 0.010 0.002 0.021 0.210 0.047 

Median 0.074 0.47 0.171 0.63 0.074 0.476 0.174 0.57 0.006 0.019 0.008 0.025 0.014 0.230 0.308 0.086 

Max 0.103 0.62 0.288 0.80 0.087 0.570 0.190 0.78 0.007 0.045 0.019 0.054 0.028 0.340 0.500 0.294 

eSD 0.020 0.07 0.031 0.09 0.004 0.069 0.007 0.11 0.001 0.010 0.007 0.089 0.093 0.028 

eCV 27 14 18 14 6 15 4 20 8 39 49 39 30 33 

NISTa 

NAV 

NAU 

0.088 0.60 0.193 0.75 0.081 0.551 0.182 0.72 0.007 0.045 0.011 0.035 nd 0.227 0.270 0.072 

0.081 0.53 0.182 0.69 0.077 0.513 0.178 0.65 0.007 0.032 0.012 0.030 0.014 0.229 0.289 0.079 

0.020 0.11 0.037 0.12 0.012 0.083 0.021 0.16 0.020 0.021 0.006 0.073 0.098 0.031 

All Lab Report C3 Page 2 / 6 
 

Round Robin XLII Laboratory Results 

All values in μg/mL 

Total Lycopene trans-Lycopene Total β-Cryptoxanthin Total α-Cryptoxanthin 

Lab 239 240 241 242 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 

FSV-BI 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 

FSV-BO 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BS 

FSV-BU 

FSV-BV
 

FSV-BW
 

FSV-BZ
 

FSV-CB
 

FSV-CBa
 

FSV-CC
 

FSV-CD
 

FSV-CE
 

FSV-CF
 

FSV-CH
 

FSV-CI 

FSV-CK 

FSV-CL 

FSV-CM 

FSV-CN 

FSV-CP 

FSV-CQ 

FSV-CR 

FSV-CS 

FSV-CT 

FSV-CU 

FSV-CX 

FSV-DB 

FSV-DF 

FSV-DJ 

FSV-DK 

FSV-DP 

FSV-DR 

FSV-DW 

FSV-EM 

FSV-ES 

FSV-FG 

FSV-FH 

0.426 0.44 0.46 0.38 

0.527 0.50 0.51 0.43 

0.556 0.60 0.66 0.50 

0.563 0.57 0.62 0.54 

0.436 0.47 0.45 0.41 

0.630 0.65 0.70 0.63 

0.552 0.65 0.63 0.54 

0.496 0.48 0.39 0.42 

0.355 0.37 0.41 0.37 

0.509 0.52 0.56 0.43 

0.431 0.46 0.45 0.37 

0.490 0.45 0.49 0.43 

0.410 0.54 0.50 0.64 

0.092 0.11 0.12 0.10 

0.451 0.56 0.53 0.55 

0.376 0.39 0.43 0.34 

0.354 0.47 0.30 0.40 

0.419 0.51 0.49 0.48 

0.400 0.50 0.44 0.40 

0.259 0.29 0.30 0.22 

0.483 0.59 0.53 0.50 

0.430 0.51 0.52 0.43 

0.471 0.37 0.40 0.31 

0.155 0.15 0.16 0.13 

0.671 0.52 0.80 0.61 

0.365 0.40 0.44 0.36 

239 240 241 242 

0.289 0.32 0.340 0.303 

0.314 0.37 0.419 0.286 

0.304 0.42 0.417 0.324 

0.215 0.26 0.302 0.182 

0.480 0.56 0.600 0.410 

0.310 0.37 0.421 0.285 

0.610 0.58 0.660 0.560 

0.099 0.10 0.111 0.082 

0.230 0.28 0.314 0.227 

239 240 241 242 

0.095 0.118 0.074 0.165 

0.063 0.082 0.043 0.111 

0.069 0.094 0.054 0.126 

0.089 0.124 0.082 0.173 

0.101 0.141 0.086 0.184 

0.087 0.128 0.073 0.175 

0.078 0.114 0.063 0.142 

0.066 0.086 0.057 0.114 

0.141 0.135 0.113 0.204 

0.071 0.098 0.058 0.124 

0.078 0.109 0.057 0.142 

0.064 0.089 0.049 0.122 

0.037 0.073 0.036 0.083 

0.084 0.112 0.071 0.142 

0.100 0.122 0.077 0.160 

0.053 0.073 0.047 0.099 

0.067 0.116 0.074 0.176 

0.085 0.107 0.066 0.138 

0.070 0.100 0.058 0.120 

0.062 0.084 0.045 0.099 

0.070 0.140 0.060 0.180 

0.090 0.124 0.075 0.165 

0.071 0.101 0.055 0.132 

0.065 0.111 0.060 0.148 

0.073 0.111 0.057 0.144 

239 240 241 242 

0.034 0.029 0.026 0.032 

0.032 0.036 0.029 0.039 

0.051 0.051 0.040 0.057 

0.040 0.037 0.036 0.037 

n 

Min 

Median 

Max 

eSD 

eCV 

NISTa 

NAV 

NAU 

26 26 26 26 

0.092 0.11 0.12 0.10 

0.434 0.49 0.47 0.43 

0.671 0.65 0.80 0.64 

0.097 0.10 0.09 0.11 

22 20 19 25 

0.434 0.49 0.47 0.43 

0.097 0.11 0.10 0.10 

9 9 9 9 

0.099 0.10 0.111 0.082 

0.304 0.37 0.417 0.286 

0.610 0.58 0.660 0.560 

0.110 0.13 0.153 0.087 

36 36 37 31 

0.304 0.37 0.417 0.286 

0.063 0.11 0.086 0.072 

25 25 25 25 

0.037 0.073 0.036 0.083 

0.071 0.111 0.060 0.142 

0.141 0.141 0.113 0.204 

0.012 0.019 0.016 0.034 

17 17 27 24 

0.065 0.144 0.072 0.177 

0.068 0.128 0.066 0.160 

0.018 0.035 0.017 0.041 

4 4 4 4 

0.032 0.029 0.026 0.032 

0.037 0.037 0.033 0.038 

0.051 0.051 0.040 0.057 

All Lab Report C4 Page 3 / 6 
 

Round Robin XLII Laboratory Results 

All values in μg/mL 

Total Lutein Total Zeaxanthin Total Lutein&Zeaxanthin 

Lab 239 240 241 242 239 240 241 242 239 240 241 242 

FSV-BA 0.152 0.53 0.196 0.72 

FSV-BD 0.053 0.225 0.048 0.40 0.029 0.172 0.102 0.062 0.082 0.40 0.150 0.46 

FSV-BE 

FSV-BF 0.092 0.43 0.141 0.49 

FSV-BG 0.069 0.225 0.065 0.36 0.022 0.068 0.017 0.110 0.091 0.29 0.082 0.47 

FSV-BH 0.059 0.239 0.045 0.44 0.028 0.129 0.104 0.050 0.087 0.37 0.149 0.49 

FSV-BI 0.061 0.245 0.045 0.43 0.028 0.197 0.112 0.050 0.089 0.44 0.157 0.48 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.064 0.211 0.034 0.37 0.040 0.349 0.140 0.083 0.083 0.47 0.158 0.42 

FSV-BO 0.087 0.45 0.172 0.39 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BS 0.091 0.45 0.118 0.37 

FSV-BU 0.103 0.54 0.192 0.57 

FSV-BV 0.091 0.33 0.137 0.37 

FSV-BW 

FSV-BZ 0.078 0.270 0.144 0.43 

FSV-CB 0.047 0.243 0.045 0.40 0.028 0.264 0.143 nd 0.075 0.51 0.188 0.40 

FSV-CBa 

FSV-CC 

FSV-CD 0.072 0.35 0.133 0.34 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CI 

FSV-CK 0.165 0.30 0.199 0.56 

FSV-CL 0.066 0.26 0.103 0.29 

FSV-CM 

FSV-CN 0.060 0.198 0.046 0.039 0.302 0.158 0.099 0.50 0.204 0.47 

FSV-CP 0.110 0.41 0.179 0.51 

FSV-CQ 

FSV-CR 

FSV-CS 0.091 0.39 0.133 0.42 

FSV-CT 0.076 0.265 0.064 0.45 0.024 0.170 0.098 0.047 0.100 0.44 0.162 0.50 

FSV-CU 

FSV-CX 0.030 0.180 0.020 0.34 0.010 0.130 0.060 0.020 0.040 0.31 0.080 0.36 

FSV-DB 0.087 0.41 0.167 0.40 

FSV-DF 

FSV-DJ 

FSV-DK 0.095 0.317 0.121 0.40 

FSV-DP 

FSV-DR 

FSV-DW 0.068 >0.200 0.061 >0.200 0.049 0.191 0.145 0.073 0.117 >0.391 0.206 >0.273 

FSV-EM 0.127 0.43 0.211 0.56 

FSV-ES 0.062 0.254 0.047 0.44 0.032 0.167 0.112 0.051 0.094 0.42 0.159 0.49 

FSV-FG 

FSV-FH 

n 13 12 13 11 11 11 11 9 24 23 24 23 

Min 0.030 0.180 0.020 0.34 0.010 0.068 0.017 0.020 0.040 0.26 0.080 0.29 

Median 0.062 0.241 0.047 0.40 0.028 0.172 0.112 0.051 0.091 0.42 0.158 0.47 

Max 0.095 0.317 0.144 0.45 0.049 0.349 0.158 0.110 0.165 0.54 0.211 0.72 

eSD 0.010 0.030 0.019 0.05 0.007 0.062 0.042 0.017 0.013 0.07 0.038 0.11 

eCV 17 12 40 12 23 36 37 33 14 17 24 24 

NISTa 

NAV 

NAU 

0.061 0.299 0.052 0.53 0.031 0.226 0.129 0.053 0.092 0.53 0.181 0.58 

0.061 

0.014 

0.270 0.049 

0.068 0.015 

0.46 

0.13 

0.029 0.199 0.120 0.052 

0.008 0.072 0.035 0.017 

0.091 

0.020 

0.47 

0.12 

0.169 

0.042 

0.53 

0.13 

All Lab Report C5 Page 4 / 6 
Round Robin XLII Laboratory Results
 

Analytes Reported By One Laboratory
 

Values in μg/mL 

Term 

N Number of (non-NIST) quantitative values reported for this analyte

Min 

Median 

Max 

 Median (non-NIST) quantitative value reported

 Maximum (non-NIST) quantitative value reported

 Minimum (non-NIST) quantitative value reported 

eSD 

eCV 

 Estimated standard deviation, calculated from the median absolute deviation

 from the median of the non-NIST results

 Coefficient of Variation for (non-NIST) results: 100*eSD/Median

NAV 

NAU NIST Assigned Uncertainty, our estimate of the total (serum hetergeniety and

 inter- and intra-laboratory) standard deviation

 For details on how we assign these quantities, see the "Analysis of Results."

 NIST Assigned Value, our estimate of the "true" analyte concentration 

nd 

nq 

<x 

>x 

! 

 Concentration greater great that x

 Discrepant value: heterogeneous serum, damaged sample, malfunction, etc.

 Not detected (i.e., no detectable peak for analyte)

 Detected but not quantitatively determined

 Concentration at or below the limit of quantification, x

italics Not explicitly reported but calculated by NIST from reported values

Analyte Code 239 240 241 242 

Coenzyme Q10 FSV-CH 0.441 0.376 0.339 0.421 

Phytoene FSV-CL 0.071 0.064 0.058 0.078 

Phytofluene FSV-CL 0.042 0.028 0.032 0.021 

Total Carotenoids FSV-EM 1.01 2.26 1.41 2.74 

trans-α-Carotene FSV-ES 0.021 0.235 0.336 0.092 

Table Legend 

Definition

All Lab Report C6 Page 5 / 6 
 

 

 

 

Round Robin XLII Laboratory Results 

Lab 

FSV-BA
 

FSV-BD
 

FSV-BE
 

FSV-BF
 

FSV-BG
 

FSV-BH
 

FSV-BI
 

FSV-BJ
 

FSV-BK
 

FSV-BL
 

FSV-BM
 

FSV-BN
 

FSV-BO
 

FSV-BP
 

FSV-BQ
 

FSV-BR
 

FSV-BS
 

FSV-BU
 

FSV-BV
 

FSV-BW 

FSV-BZ 

FSV-CB 

FSV-CBa 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CI
 

FSV-CK
 

FSV-CL
 

FSV-CM
 

FSV-CN
 

FSV-CP
 

FSV-CQ
 

FSV-CR
 

FSV-CS
 

FSV-CT
 

FSV-CU
 

FSV-CX
 

FSV-DB
 

FSV-DF
 

FSV-DJ
 

FSV-DK
 

FSV-DP
 

FSV-DR
 

FSV-DW 

FSV-EM 

FSV-ES 

FSV-FG 

NISTa 

n 

StS 

A 

B 

C 

All Lab Report 

R aT gT bC tbC 

A A A A 

A B 

A A A A 

B A A B 

A A A A 

A A B A 

A A A A A 

A A B A A 

A A 

A B B 

A A 

B B B B 

B C C 

C C C 

B A 

A 

A A 

C A A A 

B B B B 

B B B B 

C C 

C C C 

C A A 

B A 

B A A B 

A B A 

A B 

C C C B 

B B 

C C C B 

C B C B 

C 

A B B 

A B A 

A A A 

B C 

B A B A 

B C A A 

B B B 

A B B B 

B B B 

B B 

A C 

B A B A B 

A 

A A A 

A B C 

C B A 

A A 

C B B 

A A A A A 

47 46 21 30 9 

% Observed 

47 43 33 50 56 

34 35 48 37 44 

19 22 19 13 0 

Comparability Summary 

 Definition 

 Participant code 

 "Standard Score" for Retinol 

"Standard Score" for α-Tocopherol 

"Standard Score" for γ-Tocopherol 

"Standard Score" for Total β-Carotene 

"Standard Score" for trans-β-Carotene 

 number of laboratories providing data for this analyte for at least one serum 

"Standard Score" 

Given that our knowledge of the shapre, location, and width of the measurement 

distributions is approximate and that a limited number of laboratories are involved, we 

summarize comparability with the following 3-level "Standard Score" (StS)... 

Label

Lab 

R 

aT 

gT 

bC 

tbC 

n 

StS

A 

B 

C 

where: 

StV 

NAV 

NAU 

t (1-α,n-1) 

Expected 

68.3 % 

27.2 % 

4.6 % 

 Definition 

 All StV within ±t (1-0.683,n-1) (i.e., ±1 SD) 

 All StV within ±t (1-0.954,n-1) (i.e., ±2 SD) 

 At least one StV > ±t (1-0.954,n-1) (i.e., ≥2 SD) 

Standardized Value, the distance in standard deviation units your value is from 

the "true" concentration: StV = (your value - NAV) / NAU 

NIST Assigned Value, our estimate of the "true" analyte concentration 

NIST Assigned Uncertainty, our estimate of the total (serum heterogeneity and 

inter- and intra-laboratory measurement) standard deviation 

Two-tailed Student's t for coverage of ±1 and ±2 NAU about NAV assuming a 

normal population of size n 

 These are the observed and normal-population-expected proportions 

 of each Standard Score (StS), based upon each laboratory's largest 

 StV for the four sera. 

C7 Page 6 / 6 
 

Appendix D. Representative “Individualized Report” for RR42 

Each participant in RR42 received an “Individualized Report” reflecting their reported 

results. Each report included a detailed analysis of the results they reported for the 

following analytes: 

• Total Retinol 

• α-Tocopherol 

• γ-Tocopherol 

• Total β-Carotene 

• trans-β-Carotene 

• Total α-Carotene 

• trans-Lycopene 

The following eight pages are the “Individualized Report” for the analytes evaluated by 

participant FSV-BA. 

Note 

The design file and program used to generate the original RR42 “Individualized 

Reports” are no longer available. The following pages were produced using the 

2013 version of the program (a linear descendant of that used in 1998) and a 

re-created design file. 

D1
 

 Set 1 of 51 

Individualized Round Robin XLII Report: FSV-BA 

Summary 

Serum 239 Serum 240 Serum 241 Serum 

Analyte You NAV n You NAV n You NAV n You N

Retinol 0.501 0.520 47 0.727 0.698 47 0.432 0.426 47 0.934 0

Retinyl Palmitate 0.059 0.054 8 0.070 0.068 9 0.056 0.054 7 0.067 0

α-Tocopherol 7.89 7.50 46 13.8 14.2 46 6.0 6.5 46 20.60 20

γ-Tocopherol 1.56 1.64 21 2.84 2.86 21 3.32 3.54 21 1.78 1

Total β-Carotene 0.088 0.081 30 0.454 0.533 30 0.180 0.182 30 0.625 0

trans-β-Carotene 0.081 0.077 9 0.436 0.513 9 0.172 0.178 9 0.598 0

Total cis-β-Carotene 0.007 0.007 4 0.018 0.032 5 0.008 0.012 4 0.027 0

Total α-Carotene 0.013 0.014 22 0.153 0.229 25 0.235 0.289 25 0.077 0

trans-Lycopene 0.289 0.304 9 0.323 0.365 9 0.340 0.417 9 0.303 0

Total β-Cryptoxanthin 0.095 0.068 25 0.118 0.128 25 0.074 0.066 25 0.165 0

Total Lutein&Zeaxanthin 0.152 0.091 24 0.534 0.473 23 0.196 0.169 24 0.719 0

D2

You : Your reported values for the listed analytes (micrograms/milliliter)
 

NAV : NIST Assigned Values, here equal to this RR's median
 

n : Number of non-NIST laboratories reporting quantitative values for this analyte in this serum 

Please check our records against your records. Send corrections and/or updates to... 

Micronutrients Measurement Quality Assurance Program 

National Institute of Standards and Technology Tel: (301) 

100 Bureau Drive Stop 8392 Fax: (301) 

Gaithersburg, MD 20899-8392 USA Email: david.duewer

Individualized Report 
 

 Set 1 of 51 

Individualized RR XLII Report: FSV-BA 

Retinol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

239241240242 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

For the construction and interpretation of these plots, see the Final Report for
 

"Round Robin" XL, August 1997
 

Serum Comments History 

#239 Lyophilized, native, multi-donor New 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinyl palmitate, #241 New 

γ- and δ-tocopherol, trans-α- and β-carotene, zeaxanthin, and trans-lycopene 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinol, 

#242 retinyl palmitate, α- and δ-tocopherol, trans-α- and β-carotene, lutein, and trans-β- New 

cryptoxanthin 

#239 Lyophilized, prepared as a 1;1 by volume blend of the Sera 241 and 242 serum pools New 

Individualized Report Page 2 / 8 

D3
 

 Set 1 of 51 

Individualized RR XLII Report: FSV-BA 

α-Tocopherol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

239241240242 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

For the construction and interpretation of these plots, see the Final Report for
 

"Round Robin" XL, August 1997
 

Serum Comments History 

#239 Lyophilized, native, multi-donor New 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinyl palmitate, #241 New 

γ- and δ-tocopherol, trans-α- and β-carotene, zeaxanthin, and trans-lycopene 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinol, 

#242 retinyl palmitate, α- and δ-tocopherol, trans-α- and β-carotene, lutein, and trans-β- New 

cryptoxanthin 

#239 Lyophilized, prepared as a 1;1 by volume blend of the Sera 241 and 242 serum pools New 

Individualized Report Page 3 / 8 

D4
 

 Set 1 of 51 

Individualized RR XLII Report: FSV-BA 

γ-Tocopherol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

239241240242 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

For the construction and interpretation of these plots, see the Final Report for
 

"Round Robin" XL, August 1997
 

Serum Comments History 

#239 Lyophilized, native, multi-donor New 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinyl palmitate, #241 New 

γ- and δ-tocopherol, trans-α- and β-carotene, zeaxanthin, and trans-lycopene 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinol, 

#242 retinyl palmitate, α- and δ-tocopherol, trans-α- and β-carotene, lutein, and trans-β- New 

cryptoxanthin 

#239 Lyophilized, prepared as a 1;1 by volume blend of the Sera 241 and 242 serum pools New 

Individualized Report Page 4 / 8 

D5
 

 Set 1 of 51 

Individualized RR XLII Report: FSV-BA 

Total β-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

239241240242 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

For the construction and interpretation of these plots, see the Final Report for
 

"Round Robin" XL, August 1997
 

Serum Comments History 

#239 Lyophilized, native, multi-donor New 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinyl palmitate, #241 New 

γ- and δ-tocopherol, trans-α- and β-carotene, zeaxanthin, and trans-lycopene 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinol, 

#242 retinyl palmitate, α- and δ-tocopherol, trans-α- and β-carotene, lutein, and trans-β- New 

cryptoxanthin 

#239 Lyophilized, prepared as a 1;1 by volume blend of the Sera 241 and 242 serum pools New 

Individualized Report Page 5 / 8 

D6
 

 Set 1 of 51 

Individualized RR XLII Report: FSV-BA 

trans-β-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

239241240242 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

For the construction and interpretation of these plots, see the Final Report for
 

"Round Robin" XL, August 1997
 

Serum Comments History 

#239 Lyophilized, native, multi-donor New 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinyl palmitate, #241 New 

γ- and δ-tocopherol, trans-α- and β-carotene, zeaxanthin, and trans-lycopene 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinol, 

#242 retinyl palmitate, α- and δ-tocopherol, trans-α- and β-carotene, lutein, and trans-β- New 

cryptoxanthin 

#239 Lyophilized, prepared as a 1;1 by volume blend of the Sera 241 and 242 serum pools New 

Individualized Report Page 6 / 8 

D7
 

 Set 1 of 51 

Individualized RR XLII Report: FSV-BA 

Total α-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

239241240242 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

For the construction and interpretation of these plots, see the Final Report for
 

"Round Robin" XL, August 1997
 

Serum Comments History 

#239 Lyophilized, native, multi-donor New 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinyl palmitate, #241 New 

γ- and δ-tocopherol, trans-α- and β-carotene, zeaxanthin, and trans-lycopene 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinol, 

#242 retinyl palmitate, α- and δ-tocopherol, trans-α- and β-carotene, lutein, and trans-β- New 

cryptoxanthin 

#239 Lyophilized, prepared as a 1;1 by volume blend of the Sera 241 and 242 serum pools New 

Individualized Report Page 7 / 8 

D8
 

 Set 1 of 51 

Individualized RR XLII Report: FSV-BA 

trans-Lycopene, μg/mL 

239241240242 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

For the construction and interpretation of these plots, see the Final Report for
 

"Round Robin" XL, August 1997
 

Serum Comments History 

#239 Lyophilized, native, multi-donor New 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinyl palmitate, #241 New 

γ- and δ-tocopherol, trans-α- and β-carotene, zeaxanthin, and trans-lycopene 

Lyophilized, prepared from the Serum 239 serum pool, augmented with: retinol, 

#242 retinyl palmitate, α- and δ-tocopherol, trans-α- and β-carotene, lutein, and trans-β- New 

cryptoxanthin 

#239 Lyophilized, prepared as a 1;1 by volume blend of the Sera 241 and 242 serum pools New 

Individualized Report Page 8 / 8 

D9
Appendix E. Shipping Package Inserts for RR43 

The following two items were included in each package shipped to an RR43 participant: 

• Cover letter 

• Datasheet 

The cover letter and datasheet were enclosed in a sealed waterproof bag along with the 

samples themselves. 

E1
~ 

n 

(1 

D 

D 

[J 

0 

c 

0 

D 

[ 

D 

0 

0 

JJ 

c 

[ 

UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899-0001 

May4, 1998 

Dear Colleague: 

Enclosed is the set of samples for the second quality assurance round robin exercise (Round Robin 

XLill) for FY98. You will find one vial of each of four lyophilized serum samples for analysis along 

with a form for reporting your results. When reporting your results, please submit one value for each 

analyte for a given serum sample. If an obtained value is below your limit of quantitation, please 

indicate this result on the form by using NQ (Not Quantitated). For analytes not measured, please leave 

a blank. Results are due to NIST by June 22, 1998. Results received two weeks after the due date will 

not be included in the summary report for this round robin study. Written feedback concerning the study 

will be provided around July 31. 

Samples should be reconstituted with 1.0 mL of HPLC-grade water or equivalent. We recommend that 

dissolution be facilitated with 3 to 5 min agitation in an ultrasonic bath or at least 30 min at room 

temperature with intermittent swirling. (CAUTION: Vigorous shaking will cause foaming and possibly 

interfere with accurate measurement. The rubber stopper contains phthalate esters that will leach into the 

sample upon intermittent contact of the liquid sample with the stopper. These esters absorb strongly in 

the UV region and elute very near retinal in most LC systems creating analytical problems.) Pipette a 

known volume of serum from the vial for analysis. (The final volume of the reconstituted sample is 

greater than 1.0 mL.). For consistency, we request that laboratories use the following absorptivities (E 

1 % cm) in ethanol: retinal, 1843 at 325 nm; retinyl palmitate, 975 at 325 nm; cx-tocopherol, 75.8 at 292 

nm; y-tocopherol, 91.4 at 298 nm; a-carotene, 2800 at 444 nm (in hexane); P-carotene, 2560 at 450 nm 

(in ethanol), 2592 at 452 nm (in hexane); lycopene, 3450 at 472 nm (in hexane). 

Please mail or fax your results for Round Robin XLIII to: 

Micronutrients Measurement Quality Assurance Program 

NIST 

Bldg.222,Rm.B208 

Gaithersburg, MD 20899 

Fax: (301) 977-0685 

If you have questions regarding this round robin exercise, please call me at (301) 975-3120; 

e-mail me atjeanice.brownthomas@nist.gov; or mail/fax queries to the above address. 

i"\ ~I 

~~ncerely, • j; . 

~J 1.'1 .' u '~ 1" \. Y': 11 t(f /1 ./'. I . , .. " .. ~ 

Jeanice Brown Thomas ._,_, I J 

Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

Enclosures 

cc: S. Wise 

E2

NISI 
 

 

 

 

NIST 

Micronutrients Measurement Quality Assurance Program 

Round Robin XLIII Results from Laboratory #_____ 

Serum 

Analyte 243 244 245 246 Units* 

retinol 

retinyl palmitate 

α-tocopherol 

γ-tocopherol 

δ-tocopherol 

total β-carotene 

trans-β-carotene 

total cis-β-carotene 

total α-carotene 

trans-α-carotene 

total lycopene 

trans-lycopene 

β-cryptoxanthin 

α-cryptoxanthin 

lutein 

zeaxanthin 

lutein&zeaxanthin 

Other Analytes?
 

* We prefer mg/mL 

Today's Date: 

Comments? 

Mail: MMQAP, 222/B208 

NIST Please return results on-or-before Fax: 301-977-0685 

Gaithersburg, MD 20899 June 22, 1998 Email: David.Duewer@NIST.gov 

E3
 

 

Appendix F. Final Report for RR43 

The following 13 pages are the final report as provided to all participants: 

•	 Cover letter 

•	 An information sheet that: 

o	 describes the contents of the “All-Lab” report 

o	 describes the nature of the test samples and details any previous distributions 

o	 summarizes aspects of the study that we believe may be of interest to the 

participants 

F1
August 28, 1998 

Dear Colleague: 

,. 

UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899-0001 

Enclosed is the summary report of the results for Round Robin XLIII. (RR43). Inch,1ded in this report 

are: a summary of data for all laboratories; the measurement comparability summary for evaluating 

laboratory perfo~ce; a summary of,Jndi"'.idual laboratory performance for ¢e past three years; a 

summary of the interlaboratory acGuracy and p~ecision over the same period of time for the 

measurement of retinal, a- and ')'-tocopherol, and trans- and total 13-carotene; and a graphical summary 

of the NIST assigned value (NA V) v~. yo).Jr laboratory value for these analytes. As in previous 

reports, the NIST assigned values are derived from the equally weighted results from the analyses 

performed by NIST anc,Lthe laboratori~s tha~ parti~ipat~d in this interlaboratory comparison exercise. 

Since ~ere were a number of cqrrectiqns, we have also included a new "All Laboratory" repgrt for 

RR42. Please note that there are no changes which impact any of the conclusions or value assignments · 

previously made for RR42. 

. , "I • i I 

A de~iled s~mmary of the experimen~l design fo~ this interlaboratory comparison exercis~ is provided 

in the attached report. All four serum samples (Sera 243-246) were distributed in two previous round 

robins. Each sample contained moderate to very low levels of the analytes of interest and were 

selected for ~~is~ibution to proyi~e further documentation of i) $e stability of low-carotenoid 'sera 

and 2) the limits of quantitative interlaboratory comparison. Sefl!m 243 is a native serum that was 

augmented with retinyl palmitate and originally distributed as Serum 181 (RR28) and later as Serum 

222 (RR37). Sera 244, 24,5, and 246 are dilution series originally.distributed as sera .195, 197, and 

198 (RR31), respectively, and later as Serum 214, 211 .. (\nd 21;l (RR35), respectively. Serum 246, the 

high level of the series, is a native serum that was augmented with retinal, retinyl palmitate, and a.­

tocopherol. Serum 244 is a 50:50 volumetric mix of delipidized serum with the serum used for Serum 

198. Serum 245 is a 75:25 volumetric mix of the same materials. 

There were no significant changes in the observed median analyte concentration for any of the four 

sera. There is some evidence of increased measurement variability. With the ppssibl~ exception of 

total a-carotene, none of the increased variability seems related to extremely low analyte 

concentrations. In contrast to the sera-blend experiment in RR42, both lutein and zeaxanthin show the 

expected decreases in the delipidized serum dilutions. · 

Data for evaluating laboratory performance in RR42 are provided in the comparability summary (~re 

Card) on page 6 of the "All Lab Report." The criteria used to evaluate laboratory performance are as 

follows: results rated 1 (within 1 SD of the assigned value) indicate EXCEPTIONAL perfomiance;i 

results rated 2 (within 2 SD) indicate ACCEPT ABLE performance, results rated 3 (within 3 SD of the 

assigned v~lue) are MARGINAL, and those rated 4 (>3 SD from the assigned value) indicate POOR 

performance relative to the current state-of-the-practice for these measurements. 

If you have concerns regarding your laboratory performance, we suggest that you obtain a unit of SRM 

968b, Fat-Soluble Vitamins and Cholesterol in Human Serum, and analyze all three levels. If your 

measured values do not agree with .the certified values, we suggest that you contact us for consultation, 

N151 

F2
Plans regarding the continuance of the QA program beyond FY 98 are still being discussed. We will 

keep you informed as decisions are finalized. Due to the lack of funding, we will not hold the "Fatsoluble Vitamin and Carotenoid Tutorial" session this fall. This tutorial has been held in past years 

primarily for new laboratories or personnel, and for those currently experiencing difficulties with their 

analysis. We plan to hold the next QA workshop as a pre-meeting in April at Experimental Biology '99 

in Washington, DC if the program continues in FY 99. 

Samples for RR44 were shipped during the second week of August. Results are due by October 9; 

feedback to labs will be provided -by the second 1

week of November. 

For your information, please note the following related·publications: 

- Granado F, Olmedilla B, Gil-Martinez E, Blanco·!, Millan I, Rojas-Hidalgo E. 

Carotenoids, retinal and tocopherols in patients with insulin-dependent diabetes rnellitus and their 

immediate relatives. Clin Sci (Colch) 1998Feb;94(2):189-195 

- Granado F, Olmedilla B, Blanco I, Gil-Martinez E, Rojas-Hidalgo E. Variability in the 

intercomparison of food carotenoid content data: a user's point of view. Crit Rev ·Food Sci Nutr 1997 

Nov;37(7): 621-633 -

Another source for clinical-related publications that we have found to be useful is via the worldwide 

web at: http://www.ncbi.nlrn.nih.gov/pubmed/. 

If you have any questions regarding this report, please contact me at 301/975-3120; 

FAX: 301/977-0685; e-mail: jeanice.brownthomas@nist.gov. 

§

rely, jl .J,(ll~ t "VY\ :f)'ll<P 

ce Brown Thomas 

Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

cc: S. Wise 

Enclosures 

F3
.. 

The attached NIST M2QAP Round Robin XLill (RR43) feedback report includes: 

Pae 

1-4 

Sa 

Sb 

6 

Pae 

1 

2, 3 

4 

5 

6 

7-9 

"All Lab" Re ort Conteqts 

A listing of all results and statistics for analytes reported by at least two laboratories 

A list of results for the four analytes reported by only one laboratory 

A legend for the above two lists 

The "Measurement Comparability Summary" (or "Score Card") 

"Individualized" Re ort Contents 

Your values, our assigned values, and the % bias between the two 

"Comparison" plots for: retinal; a.-, y-tocopherol; total, trans-f3-carotene; total a.­

carotene; total lycopene; P-cryptoxanthiil; lutein; zeaxanthin; lutein & zeaxnthin 

"Z-Score Concordance" plots for this RR's: retinal; a-, y-tocopherol; total and trans-13-

carotene; total a-carotene; total and trans-lycopene 

% Bias Accuracy/Precision Summary of your last 3 years' results for: retinal; a-, ytocopherol; total P-carotene and trans-f3-carotene 

NIST assigned value versus your value scatterplots of your last 3 years' results for: 

retinal; a-, y-tocopherol; and/or total and trans-f3-carotene 

% Bias bar chart of your last 3 year's results for: retinal, a-, y-tocopherol, and/or total' 

and trans-f3-carotene 

F4
Analysis of Resulls Round Robin XLilI: Sera 243-246 Pagel 

Analysis of NIST M2QAP R9und Robin XLill Results: Sera 243 to 246 

Backgroli~d. Four "old", twice-before-~stributed samples were distributed in RR43. 

Serum 243:a native serui:p augmented in tetinyl palmitate. It was originally distributed as 181 

(RR28) and later as 2~2 (RR37). This serum has an unusually low p-carotene level. 

Serum 246: a native serum augiμented in retinal, retiQ.yl palmitate, ~d a-tocopherol. It was 

originally distributed as 198 (RR31) and later as 212 (RR35). This fairly "normal" serum 

is the high-level of a 2x-dilution series. 

Serum 244: a 1:1 volumetric blend of the #198 native serum and delipidiz~d serum, originally 

distributed as 195 (RR31) and later as 214 (RR35). This is the mid-level of a 2x-dilution 

series. 

Serum 245: a 1 :3 volumetric blend of the #198 native serum and delipidized serum, originally 

distributed as 197 (RR31) and later as 211 (RR35). This is the low-level of a 2x-dilution 

series. 

Quali.tative Results. 

Interferences: Five analysts reported a peak between retinal and the retinyl acetate or tocol 

internal stan~d in serum 243. Two analysts. (not exactly o.verlapping the previous set) 

reported ~ sm~lf peak co-eluting wi~ reti~ol. in sera 244, 245, ~d 246. These 'peaks appear to 

again; be p,lasuci~!-related, suggesting that tJtis ·may pe ~more general problem with 

cobimerciajly o}>tainea sera th'iμt we preYiou_sly thought. Alternatively, they could be related 

to "the retinyl pallltitate spike. We're adding this to oiir list of "things to worry about if we 

ever get'the time/opportunity." 

Solids: 0.Qe analyst reported a small "lump" remaining in serum 245, the low concentration 

member.of fue ·dilution ·series, after extreme reconstitution effort. We have no clue as to why 

one of 209 vials can gl~tch like this; fortunately, the analysis results for this vial did not seem 

to be affected by th'e undissolved solids. 

Quantitative Results The followin_g NIST Data and Value/Uncertainty Assignments table 

presents all NIST data, summary statistics for the NIST data, summary results for RR43, and 

the NIST assigned values and uncertainties. The entries are defined as follows: , 

Individual NIST Analyst Data and Summazy Statistics 

A: 1 to C:2 two aliquots (" 1" and "2") of three vials {A, B, and C) of each se~m were 

extracted and analyzed. Each analyst analyzed a separate set of three vials. 

n., number of quantitative values for this analyte for this serum for this analyst 

Mean., arithmetic average 

SD~ simple standard deviation 

SDrcpx within-vial pooled stand_ard deviation, reflecting variation in extraction, 

chromatography, peak integration, etc. 

SDbeta. among-sample standard devia~on, reflecting heterogeneity in preparing and 

reconstituting the serum samples 

SDNISTa. ~SD';. + SD!ci.. 'total standard deviation. This value is:::?: SD.,, as sample 

replicates reduce the true degrees of freedom. 

F5
Analysis of Results Round Robin XLilI: Sera 243-246 

CV NISTx 100 x SD NIST/Meanx 

NIST Summa:ry Statistics (for analytes reported by both NISTl and NIST3) 

n number of quantitative values for this analyte for this serum 

Mean (MeanNISTt + MeanNisn)/2 

SD rep within-vial pooled standard deviation 

SDhcl a.n:iong-sample standard deviation · 

SDan1 between-analyst standard deviation. This is the residual standard deviation for 

regression of NIST3' s Meanx values to NISTl 's. The model used to determine 

SDani is defined to the right of this block. Details include: model used, 

parameters and standard errors on the parameters, and R2 • 

SDNIST ~SD~+ SD~Cl +SD~, total standard deviation for NIST analyses .. 

CV NIST 100 x SD !'.lST/Mean 

Summary Statistics for Previous Distributions 

RR Round Robin in which this serum was first distributed 

Serum Sample identification number of the initially distributed serum 

Page2 

nP number of non-NIST laboratories reporting quantitative values for this analyte 

for this serum in the initial distribution ~ 

MedianP median of the reported values in the initial distribution 

eSDP 0.741 x InterQuartile Range in the initial distribution 

Summary Statistics for RR43 

~ number of non-NIST laboratories reporting quantitative values for this analyte 

for this serum in this Round Robin 

Mediann median of the reported values in this Round Robin 

eSDn 0.741 x InterQuartile Range in this Round Robin 

( 

!Mediann - Median l~nn + n - 2 ) P(n=p) IDIST P P , nP+nn-2, 2-tail 

( (nn - l)eSD~ + (nP - l)eSD! )(_!._ + _!._J 

nn np 

This is the approximate probability that the current median is the same as it was 

previously. Where the hypothesis that Medi~ = MedianP can be rejected with 

95% confidence, the P(n=p) value is flagged with an"*". IDIST is Excel~'s 

student's t function. 

( eSD2 

) P(n<p) FOIST ~. nn-1, nP-1 

eSD0 

This represents the approximate probability that the current interlaboratory 

F6
Analysis of Results Round Robin XLIII: Sera 243-246 

variance is the same as it was previously. Where the hypothesis that eSDn = 

eSDP can be rejected with 95% confidence, the P(n<p) value is flagged with an 

"*". FDIST is Excel®'s F-distribution function. 

Page 3 

SD1abs ~eSD~ - SD~'IsT, the residual non-NIST interlaboratory biases after correction 

for measurement-, sample-, and NIST-analyst-related sources of variance. When 

SDNIST is greater than eSD0 , SDtabs = 0. 

CV 1a1is 100 x SD1a1i./Medifil\i 

NIST Assigned Values and Uncertainties 

NA V (Mean + Median0 ) I 2, our best guess of the "true" an-alyte level 

NAU Maximum(0.05 x NAV, ~sn-:.iST + SD~bo ), our best guess for the "true" 

interlaboratory standard deviation characterizing measurement, sample 

heterogeneity, among-analyst, and among-laboratory sources of variation. When 

SD1

."" could not be determined, NAU is estimated as 

Maximum(0.10 x NAV, ~2 sn-:.iST ). 

CV lOOxNAU/NAV 

Measurement Performance Summary. 

Measurement Stability: There are no statistically significant changes in the median 

concentration observed for any analyte in any of the four sera. The ~ -cryptoxanthin levels 

in all four sera are somewhat reduced, but - judging from the among-RR pattern of ~ 

changes - this may be more to changes in measurement procedure than to changes in 

analyte level. .. 

There is some evidence for increased measurement variance, but the analyte/serμm 

increases do not make an interpretable pattern: y-tocopherol in serum 243, total ~-carotene 

in serum 246, and trans-lycopene in serum 244. Only for total a-carotene in sera 244, 

245, and 246 is the change systematic. We hypothesize that long-term storage may induce 

slow changes in the "background stuff' rather than in the analytes themselves, thus 

creating a variety of measurement-system-specific problems rather than a single obvious 

loss of signal. This, again, goes on our "to-worry-about-sometime" list 

Dilution series: All analytes show the expected two-fold (serum 244) and four-fold (serum 

245) reduction from the level in the native serum 246, including zeaxanthin. 

DaveDuewer 

Research Chemist 

David.Duewer@NIST.gov 

7/1~~~ ~!!d~' ' (/ Margaret Kline 

Research Biologist 

Margaret.Kline@NIST.gov 

F7
Analysis of Results Round Robin XLIII: Sera 243-246 Page4 

NIST Data and Value/Uncertainty Assignments 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n, 

Mean. 

so. 

SD....,. 

SD11ea 

Retinal 

NISTl NIST3 

243 244 245 246 243 244 245 246 

0.417 0.362 0.195 0.7-26 0.467 0.392 0.191 0.736 

0.462 0.338 0.180 0.786 0.454 0.395 0.192 0.743 

0.472 0.329 0.153 0.759 0.422 0.351 0.192 0.706 

0.412 0.355 0.182 0.736 0.431 0.347 0.193 0.689 

0.452 0.390 0.189 0.714 0.439 0.359 0.682 

0.458 0.373 0.192 0.714 0.446 0.358 0.213 0.691 

6 6 6 6 6 6 5 6 

0.445 0.358 0.182 0.739 0.443 0.367 0.196 0.708 

0.025 0.022 0.015 0.029 0.016 0.021 ' 0.009 0.026 

0.031 0.016 0.013 0.026 0.007 0.002 0.001 0.008 

0.008 0.021 0.012 0.023 0.017 0.023 0.012 0.028 

a,. Tocopherol 

NISTl NIST3 

243 244 245 246 243 244 245 246 

7.06 7.13 3.79 14.2 6.10 7.21 2.89 14.1 

7.92 7.20 4.00 14.4 6.50 7.47 2.94 14.2 

7.47 6.73 nq 14.7 6.93 7.03 - 3.20 14.3 

7.05 7.54 3.56 14.3 6.65 6.93 3.19 14.1 

655 6.52 454 14.9 7.50 7.11 14.8 

7.45 7.33 3.73 14.6 7..34 6.94 3.66 14.8 

6 6 5 6 6 6 5 6 

7.25 7.08 3.92 14.5 6.84 7.12 3.18 14.4 

0.47 0.38 0.38 0.3 0.53 0.20 0.31 0.3 

0.54 0.47 0.34 0.2 0.21 0.13 0.02 0.1 

0.25 0.13 0.29 0.2 0.56 0.19 0.38 0.3 

SDNIST. 0.032 0.026 0.018 O.Q35 0.018 0.024 0.012 0.029 059 0.49 0.45 0.3 0.60 0.24 0.38 0.3 

cvNIST. 1.2 1.2 10 4.7 4.1 6.4 6.2 4.1 8.1 6.9 11 2.2 8.7 3.3 12 2.4 

n 

Mean 

SD rep 

so_, 

so. 

SIJmsr 

CV NIST 

n,, 

·Median,, 

eSD. 

NIST 

12 12 11 

0.444 0.362 0.189 

0.022 0.011 0.009 

0.012 0.019 0.011 

0.005 0.005 0.005 

0.026 0.023 0.015 

5.8 6.3 8.0 

-RRXLill 

243 244 245 

47 47 46 

0.479 0.376 0.193 

0.035 0.040 0.016 

12 

0.724 

0.019 

0.022 

0.005 

0.030 

4.1 

246 

47 

0.723 

0.066 

P(n=p) 0.99 0.99 0.98 1.00 

P(n<p) 1.00 0.47 0.99 0.59 

SDi.i. 0.024 0.032 0.005 0.059 

CV1a1oo 5.0 8.6 2.8 8.2 

NAV 0.462 0.369 0.191 0.723 

NAU 0.035 0.040 0.016 0.066 

CV 7.6 11 8.4 9.2 

NISTI=a+b*NISTl 

a: 0.034 ±-0.006 

b: 0.914 ±-0.013 

R2

: 0.987 

xxvm XXXl XXXI 

181 195 197 

·44 38 38 

0.483 0.378 0.195 

0.064 0.039 0.024 

XXXI 

198 

39 

0.725 

0.067 

XXXVII XXXV XXXV XXXV 

222 214 211 212 

45 44 44 44 

0.470 0385 0.198 0.740 

0.050 0.034 0.021 0.069 

NIST 

12 12 10 

7.04 7.10 355 

0.41 0.35 0.24 

0.39 0.27 0.31 

0.34 0.34 0.34 

0.66 0.55 0.52 

9.4 7.8 15 

RRXLill 

243 244 245 

47 48 47 

6.98 7.23 3.51 

059 053 0.49 

0.98 0.99 0.97 

054 1.00 0.91 

0 0 0 

0 . o 0 

7.01 7.16 353 

0.66 055 052 

9.4 7.7 15 

12 

14.4 

0.2 

0.3 

0.3 

0.5 

3.2 

246 " 

47 

14.2 

1.3 

1.00 

0.60 

1.21 

8.7 

14.3 

1.3 

9.2 

NIST3=a+b*NIST1 

a: -0.68 ±-0.40 

b: 1.04 ±-0.04 

R2

: 0.987 

XXVIII XXXI XXXI XXX1 

181 195 197 198 

44 39 39 40 

7,11 7.18 3.63 14.2 

0.53 0.83 053 1.0 

xxxvn xxxv xxxv xxxv 

222 214 211 212 

42 45 45 44 

7.06 7.14 3.62 14.2 

0.60 0.82 0.59 1.4 

F8
 
Analym ofResulu Round Robin XLIII: Sera 243-246 Page S 

NIST Data and Value/Uncertainty Assignments 

'Y· Tocopherol 

NISTl NIST3 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n, 

Mean, 

so. 

SD..,,. 

.SDhc .. 

s~"ISI'• 

CVNIST:x 

h 

Mean 

SDrep 

s~I 

243 244 245 

2.59 nd nd 

1.84 nd nd 

2.05 nd nd 

2.12 nd nd 

2.11 nd nd 

2.34 nd nd 

6 0 0 

2.18 

0.26 

032 

0.08 

0.33 

15 

NIST 

12 6 5 

2.211.265 0.664 

0.23 0.009 0.009 

0.08 0.038 0.062 

246 

2.67 

2.72 

2.79 

2.66 

2.71 

2.71 

6 

2.71 

0.05 

0.06 

0.01 

0.06 

2.2 

12 

2.63 

0.04 

0.09 

SD11111 .__ _____ ___, 

s~ 0.240.039 0.062 0.10 

CV NIST 11 3.1 9.4 4.0 

n,, 

Median,, 

eSD. 

RRXLIII 

243 244 245 

23 23 22 

2.311.280 0.685 

0.280.102 0.101 

246 

22 

251 

0.15 

P(n=p) 1.00 0.87 0.95 0.82 

P(n<p) •0.02 0.99 0.95 0.97 

so.. 0.13 0.094 0.079 0.11 

cvbl» 5.8 7.4 12 4.3 

NAV 2.261.272 0.674 2.57 

NAU 0.280.102 0.101 0.15 

CV 12 8.0 15 5.8 

243 244 

2.11 1.290 

2.211.2% 

2.25 1.289 

2.24 1.270 

2.29 1.226 

2.33 1.216 

6 6 

2.241.265 

0.08 0.035 

0.040.009 

0.08 0.038 

0.09 0.039 

3.9 3.1 

XXVIII XXXI 

181 195 

16 15 

2.28 1350 

0.16 0.184 

245 246 

0.626 2.52 

0.628 2.54 

0.650 2.53 

0.671 2.51 

2.56 

0.746 2.59 

5 6 

0.664 2.54 

0.049 0.03 

0.009 0.02 

0.062 0.03 

0.062 0.04 

9.4 1.4 

XXXl XXXI 

197 198 

15 16 

0.707 2.62 

0.149 0.14 

xxxvu xxxv xxxv xxxv 

222 214 211 212 

22 21 22 21 

2.311330 0.711 2.70 

0.17 0.066 0.136 0.23 

B· Tocopherol 

NISTl NIST3 

243 244 245 246 

0 0 0 0 

NIST 

6 6 5 6 

0.149 0.087 0.051 0.166 

0.009 0.011 0.004 0.003 

0.005 0.007 0.009 0.004 

0.011 0.013 0.010 0.005 

7.1 15 20 3.2 

RRXLIII 

243 244 245 246 

3 3 3 3 

0.238 0.152 0.074 0.285 

0.097 0.0320.013 0.081 

0.48 

0.09 

0.096 0.029 0.007 0.081 

40 19 10.0 28 

0.193 0.119 0.063 0.226 

0.097 0.032 0.013 0.081 

50 26 20 36 

243 244 245 246 

0.143 0.0910.0540.162 

0.158 0.089 0.052.0.167 

0.137 0.081 0.040 0.172 

0.149 0.103 0.049 0.170 

0.1460.070 0.165 

0.158 0.087 0.063 0.160 

6 6 5 6 

0.149 0.087 0.051 0.166 

0.008 0.0110.0080.005 

0.009 0.011 o.004 0.003 

0.005 0.007 0.009 0.004 

0.011 0.013 0.010 0.005 

7.1 15 20 3.2 

xxvm XXXI XXXI XXXI 

181 195 197 198 

0 0 0 0 

XXXVII XXXV XXXV XXXV 

222 214 211 212 

5 1 1 1 

0.170 0.015 0.047 0.330 

0.045 

F9
Analysis of Results Round Robin XLlll: Sera 243-246 Page6 

NIST Data and Value/Uncertainty Assignments 

Total ~-Carotene 

NISTl NIST3 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

Ds 

Means 

SDs 

SDren 

sohc .. 

243 244 

0.072 0.396 

0.079 0.380 

0.066 0.393 

O.Q78 0.402 

0.078 0.386 

0.080 0.394 

6 6 

0.076 0.392 

0.006 0.008 

0.006 0.008 

0.003 0.005 

245 246 

0.147 0.64 

0.139 0.64 

0.155 0.65 

0.152 0.62 

0.142 0.61 

0.153 0.60 

6 6 

0.148 0.63 

0.006 0.02 

0.006 0.02 

0.005 0.02 

SDmm 0.007 0.010 0.008 0.03 

CVNISTx 9.1 2.4 5.2 4.0 

n 

Mean 

SD..., 

so.... 

SD..i 

s~ 

CV NIST 

NIST 

6 12 6 

0.076 0.383 0.148 

0.006 0.012 0.006 

0.003 0.013 0.005 

0.007 O.Q18 0.008 

9.1 4.6 5.2 

12 

0.69 

0.02 

0.07 

0.07 

11 

243 

nq 

nq 

nq 

nq 

nq 

nQ 

0 

xxvm 

181 

33 

0.087 

0.022 

244 

0.389 

0.382 

0.360 

0.393 

0.354 

0.364 

6 

0.374 

0.016 

0.014 

0.013 

0.020 

5.2 . 

XXXI 

195 

30 

0.338 

0.047 

245 

nq 

nq 

nq 

nq 

nq 

nQ 

0 

XXXI 

197 

30 

0.150 

0.029 

trans-~· Carotene 

NISTl NIST3 

246 243 244 245 246 243 244 245 246 

0.73 0.070 0.348 0.140 0.593 0.059 0.345 0.073 0.663 

0.77 0.073 0.343 0.135 0.617 0.056 0.342 0.065 0.691 

0.77 0.060 0.331 0.140 0.629 0.074 0.324 0.120 0.693 

0.75 0.077 0.354 0.131 0.584 0.069 0.339 0.098 0.674 

0.76 0.073 0.333 0.118 0.590 0.072 0.321 0.689 

0.77 O.Q78 0.342 0.132 0.572 0.068 0.322 0.120 0.697 

6 6 6 6 6 6 6 5 6 

0.76 0.072 0.342 0.133 0.598 0.066 0.332 0.095 0.685 

0.02 0.007 0.009 0.008 0.021 0.007 O.Ql 1 0.026 0.013 

0.02 0.007 0.010 0.007 0.022 0.003 0.006 0.010 0.014 

O.Ql 0.003 0.004 0.007 0.014 0.008 O.Ql 1 0.027 0.008 

0.02 0.008 0.011 0.010 0.026 0.008 0.013 0.029 0.016 

2.7 11 3.2 7.4 4.4 12 3.8 30 2.4 

NIST 

12 12 11 12 

0.069 0.337 0.114 0.641 

0.006 0.008 0.008 0.019 

0.016 0.018 0.019 O.Q15 

0.033 0.033 0.033 0.033 

0.037 0.038 0.039 0.041 

54 11 34 6.4 

XXXl 

198 

31 

0.68 

0.08 

a: -0.048 ±0.028 

b: 1.198 ±0.080 

R2

: 0.987 

XXVlll XXXl XXXI 

181 195 197 

5 7 7 

XXXI 

198 

7 

0.085 0.332 0.160 0.628 

0.005 0.026 0.021 0.006 

RRXLIII xxxvu xxxv xxxv xxxv RRXLIII xxxvn xxxv xxxv xxxv 

n,, 

Median,, 

eSD,, 

243 

32 

0.073 

0.011 

244 

32 

0.336 

0.030 

245 246 

31 31 

0.144 0.66 

0.027 0.12 

P(n=p) 0.92 0.99 0.96 0.96 

P(n<p) 1.00 0.99 0.90 *0.01 

so.... 0.009 0.024 0.026 0.09 

CVw. 12 7.1 18 14 

NAV 0.074 0.359 0.146 0.68 

NAU 0.011 0.030 0.027 0.12 

CV 15 8.3 19 18 

222 214 211 212 

28 34 33 33 

0.077 0.360 0.167 0.70 

0.012 0.034 0.034 0.06 

243 244 245 246 222 214 211 212 

11 11 11 i'l 14 12 12 12 

0.071 0.308 0.150 0.631 0.072 0.337 0.159 0.642 

0.010 0.022 0.017 0.038 0.010 0.034 0.021 0.066 

0.97 0.68 0.85 0.96 

0.60 0.92 0.74 0.95 

0 0 0 

0 0 0 ~I 0.070 0.323 0.132 0.636 

0.037 0.038 0.039 0.041 

53 12 29 6.4 

F10
Analysu ofRC5ults Round Robin XLIII: Sera 243-246 

NIST Data and Value/Uncertainty Assignments 

Total a-Carotene trans-a-Carotene 

NISTl NIST3 NISTl NIST3 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n, 

Mean, 

SD, 

SD,_ 

SDi.:u 

SDms,-, 

CYNISl'x 

n 

243 

nd 

nd 

nd 

nd 

nd 

nd 

0 

0 

244 245 

0.026 nd 

0.027 nd 

0.029 nd 

0.030 nd 

0.026 nd 

0.023 nd 

6 

0.027 

0.002 

0.001 

0.002 

0.003 

9.9 

NIST 

6 

246 

0.046 

0.040 

0.054 

0.042 

0.043 

0.037 

0 6 

0.044 

0.006 

0.006 

0.004 

0.007 

16 

0 12 

Mean .__--........._ 0.027 __ ___;,,,,;,.;;........;..i 0.047 

SD~ 

SDi..i 

0.001 

0.002 

0.005 

0.004 

SDw ....__ ______ ____, 

s~ 

CVNJST 

0.003 

9.9 

0.007 

14 

243 244 245 

nq nq nq 

nq nq nq 

nq nq nq 

nq nq nq 

nq nq nq 

TUI TUI TUI 

0 0 0 

xxvm XXXI XXXI 

181 195 197 

15 

O.D18 

0.006 

246 243 244 245 246 243 244 245 

0.044 0.013 0.019 nq 

0.052 0.012 0.016 nq 

0.053 0.014 O.D15 nq 

0.049 0.014 O.D18 nq 

0.050 0.017 O.D15 nq 

0.051 0.014 0.016 no 

6 0 0 0 0 6 6 0 

0.050 0.014 0.016 

0.003 0.001 0.001 

0.004 0.001 0.002 

0.001 0.001 0.001 

0.004 0.002 0.002 

7.6 13 11 

NIST 

6 6 0 6 

0.014 0.016 0.032 

0.001 0.002 0.002 

0.001 0.001 0.001 

0.002 0.002 0.002 .. 13 11 6.4 

XXXI xxvm XXXI XXXI 

198 181 195 197 

0 0 0 

Page7 

246 

0.030 

0.032 

0.033 

0.029 

0.033 

0.033 

6 

0.032 

0.002 

0.002 

0.001 

0.002 

6.4 

~ 

XXXl 

198 

0 

RRXLilI xxxvn xxxv xxxv xxxv RRXLIII XXXVII XXXV XXXV XXXV 

n,. 

Median,. 

eSD. 

P(n=p) 

P(n<p) 

243 244 245 

24 24 20 

0.014 O.Dl8 0.010 

0.003 0.008 0.004 

0.88 0.99 

o.99 •o.oo 

0.94 

0.06 

246 

25 

0.032 

0.012 

0.91 

•0.01 

~~ I ... __ o_.oo_4_~ ___ 0.0~~1 ............ 

NAU 0.008 0.012 

NAV I 0.022 .__ _______ ___. 0.0391 

CV 36 31 

222 214 ill 

21 26 23 

0.016 0.018 0.009 

0.005 0.004 0.003 

212 243 244 245 246 222 214 211 212 

26 1 1 0 1 0 0 0 0 

0.036 0.014 0.014 0.023 

0.008 

0.014 0.015 0.027 

0.002 0.003 0.003 

18 17 10 

F11
Analysis of Results Round Robin XLIII: Sera 243-246 Page 8 

NIST Data and Value/Uncertainty Assignments 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

nx 

Meanx 

SDx 

so ....... SD11o .. 

SDmsT. 

CVNJSTa 

n 

Mean 

SD..,.. 

S~, 

SDIDI 

SI>msr 

CVmsr 

243 

0 

6 

0.52 

0.01 

0.05 

0.06 

11 

Total Lycopene 

NISTl NIST3 

244 245 246 243 244 245 246 

0.46 nq nq 0.184 

0.46 nq nq . 0.189 

0.55 nq nq 0.209 

0.52 nq nq 0.194 

0.56 nq nq 0.227 

0.57 nq nq 0.215 

0 0 0 6 0 0 6 

0.52 0.203 

0.05 0.017 

0.01 0.008 

0.05 0.017 

0.06 0.019 

11 9.4 

NIST 

0 0 6 

0.203 

0.008 

0.017 

0.019 

9.4 

xxvm XXXI XXXI XXXI 

181 195 197 198 

16 20 19 22 

0.47 0.06 0.02 0.118 

0.10 0.02 O.Ql 0.049 

RRXLIII XXXVII XXXV XXXV XXXV 

n,, 

Median,, 

eSD. 

243 

29 

0.43 

0.14 

244 

28 

0.07 

0.03 

245 246 

23 27 

0.03 0.122 

0.01 0.043 

P(n=p) 0.95 0.98 0.96 0.98 

P(n<p) 0.11 0.51 0.37 0.75 

S:Diu.I 0.12 

CYw. 29 0.0~~1 

NAVI 0.47 

NAU 0.14 

0.1631 

0.043 

CV 29 26 

222 214 211 212 

24 23 23 24 

0.45 0.07 0.03 0.142 

0.04 0.03 0.01 0.047 

243 

0 

6 

0.234 

0.010 

0.025 

0.027 

12 

243 

9 

0.292 

0.067 

0.89 

0.62 

0.061 

21 

0.263 

0.067 

25 

trans-Lycopene 

NISTl NIST3 

244 245 246 243 244 245 246 

0.198 0.037 nq o.o69 

0.211 0.037 nq 0.075 

0.260 0.040 nq 0.o75 

0.240 0.037 nq 0.076 

. 0.247 0.037 nq 0.075 

0 0 0 

NIST 

6 0 6 

0.037 0.075 

0.002 0.003 

0.002 0.003 

0.003 0.004 

7.6 5.2 

RRXLIII 

244 245 246 

9 9 9 

0.035 0.017 0.067 

0.013 0.004 0.022 

0.58 0.60 0.61 

*0.02 0.98 0.28 

0.012 0.022 

35 33 

0.036 0.071 

0.013 0.022 

35 31 

0.248 0.032 

6 6 

0.234 0.037 

0.024 0.002 

p.010 0.002 

0.025 0.002 

0.027 0.003 

12 7.6 

xxvm XXXI 

181 195 

0 1 

0.041 

no 

0 

XXXI 

197 

1 

0.015 

0.080 

6 

0.075 

0.003 

0.003 

0.003 

0.004 

5.2 

'1 

.. 

XXXI 

198' 

1 

0.070 

XXXVII XXXV XXXV XXXV 

222 214 211 212 

7 6 6 6 

0311 0.046 0.024 0.087 

0.074 0.004 0.010 0.017 

F12
.. . 

0 Analysu of Results Round Robin Xl.IlI: Sera 243-246 Page 9 

NIST Data and Value/Uncertainty Assignments 

~-Cryptoxanthin 

NISTl NIST3 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n, 

Mean, 

SD, 

SD,_ 

SDbou 

243 244 

0.047 O.Ql5 

0.044 0.017 

0.043 0.017 

0.039 0.017 

0.040 0.017 

0.044 O.Ql8 

6 6 

0.043 0.017 

0.003 0.001 

0.002 0.001 

0.002 0.001 

SDNIST. 0.003 0.001 

cvNIST. 8.1 6.o 

245 

nd 

nd 

nd 

nd 

nd 

nd 

NIST 

n 12 12 

Mean 0.045 0.012 

SD"" 0.005 0.001 

SD,,., 0.005 0.005 

0 

0 

246 243 244 

0.023 0.037 0.007 

0.024 0.043 0.006 

0.026 0.057 0.008 

0.023 0.046 0.007 

0.026 0.056 0.009 

0.027 0.046 0.007 

6 6 6 

0.025 0.047 0.007 

0.002 0.008 0.001 

0.001 0.007 0.001 

0.002 0.007 0.001 

0.002 0.009 0.001 

8.5 20 17 

12 

0.020 

0.001 

0.005 

SDw.__~~~~~~--

S~ 0.007 0.005 

CVNIST 16 44 

0.005 

25 

XXYIIl 

181 

11 

0.070 

0.012 

XXXI 

·195 

13 

0.013 

0.007 

245 

nd 

nd 

nd 

nd 

nd 

nd 

0 

XXXI 

197 

12 

0.008 

0.003 

NISTl 

246 243 244 245 

0.016 0.064 0.023 0.012 

0.016 . 0.069 0.021 nd 

0.016 0.068 0.017 0.012 

0.017 0.068 0.023 nd 

0.016 0.068 0.020 nd 

0.015 0.062 0.021 0.012 

6 6 6 3 

0.016 0.067 0.021 0.012 

0.001 0.003 0.002 0.000 

0.001 0.003 0.003 

0.001 0.001 0.001 

0.001 0.004 0.003 

5.5 5.4 14 

NIST 

12 12 8 

0.078 0.024 0.013 

0.003 0.003 0.001 

0.009 0.002 0.001 

0.013 0.013 0.013 

"Lutein" 

NIST3 

246 243 244 245 246 

0.062 0.088 0.025 0.012 0.052 

0.062 0.088 0.030 0.012 0.051 

0.063 0.093 0.028 0.012 0.056 

0.068 0.087 0.027 0.015 0.055 

0.066 0.090 0.025 Q.054 

0.063 0.091 0.024 0.016 0.055 

6 6 6 5 6 

0.064 0.090 0.026 0.013 0.054 

0.002 0.002 0.002 0.002 0.002 

0.002 0.002 0.002 0.001 0.001 

0.002 0.001 0.002 0.002 0.002 

0.003 0.003 0.003 0.002 0.002 

4.6 3.2 11 15 4.0 

12 

0.059 

0.002 

0.010 

0.013 

NIST3=a+b*NIST1 

a: 0.000± 

b: 1.113 ±0.141 

R2:0.987 

0.016 0.014 0.014 0.017 

21 59 110 28 

XXXI XXYIIl XXXI XXXI XXXI 

198 181 195 197 198 

15 7 7 6 8 

0.024 0.068 0.020 0.011 0.057 

0.008 O.Ql5 0.003 0.002 0.019 

RRXLID xxxvn xxxv xxxv xxxv RRXLffi xxxvn xxxv xxxv xxxv 

n,, 

Median,, 

eSD. 

243 244 245 

27 22 17 

0.058 0.009 0.005 

0.016 0.002 0.002 

246 

24 

0.016 

0.004 

P(n=p) 0.84 0.77 0.70 0.68 

P(n<p) 0.79 1.00 1.00 0.99 

SDi.i,.I O.Ql5 0 

CV11111 25 0 ~I NAY 0.052 0.011 0.018 

NAU 0.016 0.005 0.005 

CV 32 50 28 

222 214 211 

i9 15 12 

0.070 0.014 0.009 

0.019 0.005 0.004 

212 

16 

0.026 

0.007 

243 244 245 246 

16 16 15 16 

0.081 0.028 0.013 0.050 

0.014 0.005 0.002 0.008 

1.00 0.86 0.72 0.86 

0.86 0.32 1.00 1.00 

0 

0 

0 

0 

0 

0 ~I 0.079 0.026 0.013 0.055 

0.016 0.014 0.014 O.Ql 7 

20 55 100 30 

222 214 211 212 

13 10 9 10 

0.081 0.030 0.016 0.054 

0.019 0.004 0.005 0.007 

F13
Analysis ofRcsulu Round Robin XL.III: Sera 243-246 Page 10 

NIST Data and Value/Uncertainty Assignments 

"Zeaxan th in" "Lutein&Zeaxanthin" 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

Il1 

Mean1 

SDI 

SDmsi 

243 

0.039 

0.034 

0.042 

0.042 

0.044 

0.043 

6 

0.041 

0.004 

0.002 

0.004 

NISTl 

244 245 246 

nd nd 0.026 

nd nd 0.021 

nd nd 0.026 

nd nd 0.023 

nd nd 0.027 

nd nd 0.020 

0 0 6 

0.024 

0.003 

0.004 

-0.000 

NIST3 NISTl 

243 244 245 246 243 244 245 

0.047 0.012 0.004 0.027 0.103 0.023 0.012 

0.047 O.D15 0.005 0.025 0.103 0.021 nd 

0.057 0.013 0.005 0.027 0.110 0.017 0.012 

0.054 0.012 0.007 0.027 0.111 0.023 nd 

0.053 0.014 0.026 0.112 0.020 nd 

0.052 0.011 0.005 0.024 0.106 0.021 0.012 

6 6 5 6 6 6 3 

0.052 0.013 0.005 0.026 0.107 0.021 0.012 

0.004 0.002 0.001 0.001 0.004 0.002 0.000 

0.002 0.002 0.001 0.001 0.003 0.003 

SDbca 0.004 0.001 0.001 0.001 0.004 0.001 

SDmsri 0.004 

CVNISTI 11 

0.004 0.004 0.002 0.001 0.002 0.005 0.003 

17 8.4 16 25 6.4 4.4 14 

n 

Mean 

SD""' 

so.... 

SD..i 

SDmsr 

CVNIST 

n,. 

Median,, 

eSD. 

12 

0.046 

0.002 

0.007 

0.007 

16 

243 

14 

0.031 

0.014 

NIST 

6 5 12 

0.013 0.005 0.025 

0.002 0.001 0.003 

0.001 0.001 0.001 

0.002 0.001 0.003 

16 25 13 

RRXLID 

244 245 246 

14 12 14 

0.008 0.005 0.017 

0.003 0.004 0.006 

P(n=p) 0.82 0.59 0.88 0.83 

P(n<p) 0.48 1.00 0.82 0.99 

S0..11o 0.012 0.002 0.003 0.005 

cv •• 37 26 66 29 

0.039 0.010 0.005 0.021 

0.014 0.003 0.004 0.006 

35 28 68 28 

NIST 

12 12 8 

0.124 0.030 0.016 

0.003 0.003 0.001 

0.010 0.008 0.003 

O.D18 O.D18 0.018 

0.021 0.020 0.019 

17 68 120 

xxvm XXXI XXXI XXXl 

181 195 197 198 

3 4 4 4 

0.026 0.017 0.009 0.025 

0.004 0.019 0.005 0.013 

XXXVII XXXV XXXV XXXV RRXLIII 

222 214 211 212 243 244 245 

10 6 6 6 27 27 24 

0.039 0.012 0.006 0.019 0.117 0.033 O.Q18 

0.013 0.002 0.003 0.004 0.030 0.007 0.005 

0.90 0.78 0.88 

0.93 0.98 1.00 

I o.o~~ 0 0 

0 0 

0.121 0.031 0,017 

0.030 0.020 0.019 

25 65 110 

NIST3 

246 243 244 245 246 

0.088 0.135 0.037 0.016 0.079 

0.083 0.136 0.046 0.017 0.076 

0.089 0.150 0.040 0.017 0.083 

0.090 0.141 0.038 0.022 0.082 

0.093 0.143 0.038 0.080 

0.082 0.143 0.035 0.021 0.079 

6 6 6 5 6 

0.088 0.141 0.039 0.019 0.080 

0.004 0.006 0.004 0.003 0.002 

0.005 0.004 0.004 0.002 0.001 

0.002 0.005 0.002 0.002 0.002 

0.005 0.007 0.005 0.003 0.003 

6.1 4.6 12 16 3.5 

12 

0.084 

0.004 

0.013 

O.Q18 

0.023 .. 27 .. 

XXVIII XXXI XXXI XXXI 

181 195 197 198 

7 12 12 13 

0.109 0.047 0.027 0.081 

0.020 0.011 0.016 0.013 

xxxvn xxxv xxxv xxxv 

246 222 214 211 212 

26 17 16 15 16 

0.067 0.101 0.040 0.020 0.074 

0.013 0.041 0.009 0.006 0.013 

0.87 

0.52 

~I 0.075 

0.023 

30 

F14
 

Appendix G. “All-Lab Report” for RR43 

The following six pages are the “All-Lab Report” as provided to all participants, with two 

exceptions: 

• the participant identifiers (Lab) have been altered. 

• the order in which the participant results are listed has been altered. 

The data summary in the “All-Lab Report” has been altered to ensure confidentiality of 

identification codes assigned to laboratories. The only attributed results are those 

reported by NIST. The NIST results are not used in the assessment of the consensus 

summary results of the study. 

G1
 
 

Round Robin XLIII Laboratory Results 

All Values in μg/mL 

Lab 243 

Retinol 

244 245 246 

Retinyl Palmitate α-Tocopherol γ-Tocopherol δ-Tocopherol 

FSV-BA 0.591 0.484 0.247 0.809 

FSV-BD 0.436 0.409 0.151 0.727 

FSV-BE 0.443 0.342 0.197 0.681 

FSV-BF 0.495 0.401 0.189 0.791 

FSV-BG 0.485 0.364 0.197 0.745 

FSV-BH 0.464 0.347 0.183 0.715 

FSV-BI 0.466 0.383 0.190 0.765 

FSV-BIa 0.485 0.364 0.197 0.745 

FSV-BJ 0.466 0.386 0.191 0.726 

FSV-BK 0.449 0.357 0.182 0.722 

FSV-BL 0.400 0.200 < 0.11 0.460 

FSV-BM 0.434 0.350 0.140 0.696 

FSV-BN 0.480 0.380 0.180 0.794 

FSV-BO 0.630 0.513 0.246 0.897 

FSV-BQ 0.488 0.435 0.237 0.777 

FSV-BR 0.480 0.390 0.200 0.750 

FSV-BS 0.516 0.427 0.212 0.718 

FSV-BT 0.439 0.346 0.354 0.596 

FSV-BU 0.516 0.415 0.188 0.765 

FSV-BV 0.490 0.350 0.130 0.570 

FSV-BW 0.488 0.373 0.191 0.710 

FSV-BX 0.550 0.396 0.208 0.840 

FSV-BZ 

FSV-CB 0.575 0.453 0.224 0.807 

FSV-CC 0.485 0.376 0.170 0.694 

FSV-CD 0.446 0.360 0.194 0.611 

FSV-CE 0.463 0.373 0.191 0.700 

FSV-CF 0.479 0.380 0.197 0.723 

FSV-CH 0.362 0.314 0.170 0.579 

FSV-CI 0.510 0.420 0.190 0.790 

FSV-CK 0.445 0.339 0.185 0.641 

FSV-CL 0.368 0.334 0.157 0.685 

FSV-CM 

FSV-CN 0.463 0.363 0.205 0.729 

FSV-CP 

FSV-CQ 0.463 0.355 0.200 0.748 

FSV-CR 0.490 0.420 0.210 0.790 

FSV-CS 0.446 0.376 0.189 0.731 

FSV-CT 0.519 0.427 0.217 0.881 

FSV-CU 0.466 0.389 0.200 0.694 

FSV-CX 0.440 0.380 0.210 0.690 

FSV-DA 0.454 0.389 0.203 0.706 

FSV-DB 0.500 0.369 0.195 0.734 

FSV-DF 0.500 0.410 0.200 0.800 

FSV-DJ 0.460 0.370 0.190 0.760 

FSV-DP 0.474 0.369 0.175 0.697 

FSV-DR 0.470 0.400 0.195 0.790 

FSV-DU 0.490 0.410 0.190 0.810 

FSV-DW 0.499 0.400 0.233 0.722 

FSV-EL 0.560 0.370 0.140 0.550 

FSV-EM 0.510 0.420 0.200 0.760 

FSV-ES 0.450 0.355 0.184 0.691 

FSV-FG 0.490 0.350 0.150 0.720 

FSV-FH 

243 244 245 246 

0.112 0.096 0.045 0.246 

0.090 0.097 0.061 0.236 

0.081 0.109 0.039 0.251 

0.135 0.131 0.052 0.321 

0.105 0.072 nd 0.283 

0.095 0.129 0.050 0.308 

0.110 0.109 0.075 0.280 

0.134 0.153 0.052 0.400 

0.161 0.162 0.082 0.401 

0.220 0.160 0.050 0.350 

0.139 0.095 0.052 0.222 

0.090 0.060 0.040 0.230 

0.137 0.086 0.060 0.247 

243 244 245 246 

7.22 7.09 3.35 14.4 

8.31 7.76 4.38 16.1 

6.88 7.39 3.78 13.3 

6.98 7.53 3.32 14.6 

6.99 6.41 3.40 13.9 

7.58 7.86 3.87 15.2 

6.79 7.26 3.61 15.0 

7.44 8.71 4.46 15.4 

6.63 6.92 3.27 13.3 

6.46 4.74 2.58 12.9 

7.80 7.20 3.40 14.4 

7.03 7.32 3.42 15.1 

5.69 5.81 2.84 11.8 

7.38 7.49 3.92 14.4 

6.57 6.23 2.68 12.3 

6.88 7.15 3.91 13.5 

6.29 6.60 3.00 12.3 

6.40 6.80 3.42 13.3 

7.14 7.29 3.76 14.4 

6.40 8.70 4.10 12.8 

7.50 7.86 3.66 14.9 

6.98 7.45 3.25 15.3 

7.57 7.50 3.81 14.1 

6.73 7.22 2.53 13.8 

7.90 7.70 3.80 15.6 

5.71 6.89 3.63 12.0 

5.90 6.20 2.70 11.8 

6.96 6.51 3.70 12.9 

8.06 8.28 4.38 16.5 

7.10 7.10 3.70 14.9 

6.95 7.09 3.25 14.2 

7.36 7.24 !2.29 !5.17 

6.60 6.75 3.51 16.3 

7.10 8.60 4.10 15.4 

6.23 7.39 2.70 15.4 

8.09 8.83 4.48 16.0 

6.99 7.14 3.36 13.6 

6.91 7.36 3.95 13.9 

7.71 7.80 3.95 14.3 

6.79 6.95 3.50 13.0 

8.30 8.50 4.90 16.4 

6.72 7.21 3.32 14.3 

7.34 7.54 4.39 14.9 

7.89 7.74 4.33 13.5 

6.24 7.12 3.01 12.8 

6.83 6.59 3.46 13.9 

5.80 5.80 2.15 12.8 

6.70 3.10 14.0 

243 244 245 246 

2.18 1.31 0.71 2.44 

2.36 1.37 0.77 2.62 

2.32 1.27 0.67 2.53 

2.31 1.20 0.69 2.52 

2.71 1.56 0.83 3.05 

2.13 1.28 0.76 2.52 

2.68 1.60 0.80 2.81 

1.98 1.13 0.64 2.40 

2.51 1.29 0.59 2.49 

2.99 1.55 1.10 2.69 

2.15 1.23 0.62 2.33 

2.27 1.25 0.68 2.48 

2.51 1.29 0.66 2.63 

1.50 1.40 0.98 2.50 

2.32 1.24 0.62 2.31 

1.63 1.09 0.56 1.72 

2.23 1.24 0.69 2.42 

2.14 1.26 0.65 2.63 

1.78 0.94 0.44 2.06 

2.51 1.37 !12.39 !0.90 

2.03 1.20 0.47 2.58 

2.54 1.52 0.74 2.95 

2.33 1.35 0.76 2.51 

243 244 245 246 

0.238 0.152 0.084 0.285 

0.382 0.153 0.051 0.349 

<0.3 <0.3 <0.3 <0.3 

0.122 0.079 0.074 0.136 

n 50 50 49 50 13 13 12 13 47 48 47 47 23 23 22 22 3 3 3 3 

Min 0.362 0.200 0.130 0.460 0.081 0.060 0.039 0.222 5.69 4.74 2.15 11.8 1.50 0.94 0.44 1.72 0.122 0.079 0.051 0.136 

Median 0.480 0.378 0.194 0.727 0.112 0.109 0.052 0.280 6.98 7.23 3.51 14.2 2.31 1.28 0.68 2.51 0.238 0.152 0.074 0.285 

Max 0.630 0.513 0.354 0.897 0.220 0.162 0.082 0.401 8.31 8.83 4.90 16.5 2.99 1.60 1.10 3.05 0.382 0.153 0.084 0.349 

eSD 0.030 0.034 0.015 0.054 0.033 0.033 0.011 0.060 0.59 0.57 0.53 1.3 0.29 0.12 0.11 0.16 

eCV 6 9 8 7 29 31 21 22 8 8 15 9 13 9 15 6 

NISTa 0.445 0.358 0.182 0.739 7.25 7.08 3.92 14.5 2.18 nd nd 2.71 

NISTb 0.443 0.367 0.196 0.708 6.84 7.12 3.18 14.4 2.24 1.26 0.66 2.54 0.149 0.087 0.051 0.166 

NAV 0.462 0.370 0.192 0.725 0.112 0.109 0.052 0.280 7.01 7.16 3.53 14.3 2.26 1.27 0.68 2.57 0.149 0.087 0.053 0.166 

NAU 0.047 0.038 0.020 0.061 0.033 0.033 0.011 0.060 0.66 0.63 0.62 1.3 0.29 0.16 0.10 0.27 

All Lab Report G2 Page 1 / 6 
 

Round Robin XLIII Laboratory Results 

All Values in μg/mL 

Total β-Carotene trans-β-Carotene Total cis-β-Carotene Total α-Carotene 

Lab 243 244 245 246 243 244 245 246 243 244 245 246 243 244 245 246 

FSV-BA 0.085 0.337 0.131 0.70 0.079 0.315 0.123 0.669 0.006 0.022 0.008 0.034 0.013 0.013 0.008 0.041 

FSV-BD 0.096 0.335 0.144 0.65
 

FSV-BE
 0.081 0.357 0.094 0.76
 

FSV-BF
 0.070 0.416 0.206 0.69 0.014 0.025 0.021 0.034 

FSV-BG 0.071 0.311 0.117 0.66 0.016 0.018 nq 0.032 

FSV-BH 0.071 0.340 0.169 0.68 0.071 0.315 0.155 0.633 nq 0.025 0.014 0.051 0.013 0.017 0.009 0.039 

FSV-BI 0.069 0.338 0.138 0.66 0.012 0.014 0.007 0.032 

FSV-BIa 

FSV-BJ 0.063 0.326 0.074 0.88 nd 0.013 nd nd 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.071 0.323 0.144 0.65 0.066 0.284 0.127 0.587 0.002 0.037 0.012 0.060 0.012 0.014 0.005 0.027 

FSV-BO 0.080 0.321 0.132 0.56 0.013 0.013 0.011 0.025 

FSV-BQ 

FSV-BR 

FSV-BS 0.091 0.320 0.140 0.48 0.038 0.040 0.032 0.043 

FSV-BT 0.056 0.310 0.145 0.57 0.063 0.288 0.134 0.536 0.002 0.022 0.010 0.039 0.017 0.012 0.005 0.024 

FSV-BU 0.069 0.323 0.155 0.65 0.021 0.026 0.165 0.048 

FSV-BV 0.072 0.316 0.156 0.61 0.012 0.190 0.010 0.038 

FSV-BW 0.087 0.358 0.126 0.74 0.013 0.011 nq 0.024 

FSV-BX 0.073 0.145 0.144 0.21 0.015 0.010 0.010 0.015 

FSV-BZ 0.005 0.009 0.003 0.020 0.020 0.020 0.015 0.028 

FSV-CB 0.051 0.291 0.122 0.45 0.009 0.019 0.007 0.033 

FSV-CC 

FSV-CD 0.070 0.310 0.128 0.55 0.014 0.012 0.005 0.023 

FSV-CE 0.096 0.388 0.060 0.90 

FSV-CF 

FSV-CH 0.104 0.322 0.201 0.55 0.016 0.023 0.031 0.024 

FSV-CI
 

FSV-CK
 0.113 0.445 0.174 0.87 0.021 0.024 0.010 0.044 

FSV-CL 0.046 0.346 0.158 0.63 0.011 0.026 0.011 0.043 

FSV-CM 

FSV-CN >0.063 >0.274 >0.094 >0.72 0.063 0.274 0.094 0.716 nq nq nq 0.029 

FSV-CP 0.075 0.333 !0.572 !0.22 0.010 0.016 !0.028 !0.012 

FSV-CQ 0.066 0.361 0.143 0.75 

FSV-CR 

FSV-CS 0.071 0.384 0.170 0.70 0.066 0.344 0.150 0.623 0.005 0.040 0.020 0.073 0.011 0.024 0.008 0.044 

FSV-CT 0.076 0.399 0.163 0.05 

FSV-CU >0.081 >0.308 >0.151 >0.67 0.081 0.308 0.151 0.666
 

FSV-CX
 0.070 0.300 0.160 0.56 0.010 <0.01 <0.01 0.030 

FSV-DA 0.085 0.350 0.179 0.72 0.076 0.304 0.153 0.637 0.009 0.046 0.026 0.081 0.014 0.018 0.008 0.037 

FSV-DB 0.079 0.401 0.161 0.86 

FSV-DF 

FSV-DJ 

FSV-DP 

FSV-DR 0.084 0.380 0.185 0.83 

FSV-DU >0.075 >0.270 >0.140 >0.28 0.075 0.270 0.140 0.280 

FSV-DW 0.087 0.341 0.184 0.70 0.082 0.310 0.161 0.631 0.005 0.031 0.023 0.067 0.047 0.024 0.013 0.049 

FSV-EL 

FSV-EM 0.035 0.238 0.043 0.64 <0.015 <0.015 <0.015 0.021 

FSV-ES >0.050 >0.318 >0.156 >0.61 0.050 0.318 0.156 0.613
 

FSV-FG
 

FSV-FH
 

n 32 32 31 31 11 11 11 11 7 8 8 8 24 24 20 25 

Min 0.035 0.145 0.043 0.05 0.050 0.270 0.094 0.280 0.002 0.009 0.003 0.020 0.009 0.010 0.005 0.015 

Median 0.073 0.336 0.144 0.66 0.071 0.308 0.150 0.631 0.005 0.028 0.013 0.056 0.014 0.018 0.010 0.032 

Max 0.113 0.445 0.206 0.90 0.082 0.344 0.161 0.716 0.009 0.046 0.026 0.081 0.047 0.190 0.165 0.049 

eSD 0.011 0.032 0.027 0.13 0.012 0.015 0.015 0.052 0.001 0.011 0.009 0.025 0.003 0.008 0.004 0.012 

eCV 16 9 19 19 16 5 10 8 30 40 68 45 25 44 41 37 

NISTa 

NISTb 

NAV 

NAU 

0.076 0.392 0.148 0.63 0.072 0.342 0.133 0.598 0.004 0.050 0.015 0.031 nd 0.027 nd 0.044 

>0.066 0.374 >0.095 0.76 0.066 0.332 0.095 0.685 nq 0.041 nq 0.073 >0.014 >0.016 nq 0.050 

0.072 0.359 0.133 0.68 0.070 0.323 0.133 0.636 0.004 0.037 0.014 0.054 0.014 0.020 0.010 0.039 

0.015 0.060 0.032 0.12 0.011 0.040 0.040 0.066 0.003 0.017 0.010 0.032 0.005 0.009 0.005 0.016 

All Lab Report G3 Page 2 / 6 
 

Round Robin XLIII Laboratory Results 

All Values in μg/mL 

trans-α-Carotene Total Lycopene trans-Lycopene Total β-Cryptoxanthin Total α-Cryptoxanthin 

Lab 243 244 245 246 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 

FSV-BI 

FSV-BIa 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 

FSV-BO 

FSV-BQ 

FSV-BR 

FSV-BS 

FSV-BT 

FSV-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-BZ 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CI 

FSV-CK 

FSV-CL 

FSV-CM 

FSV-CN 

FSV-CP 

FSV-CQ 

FSV-CR 

FSV-CS 

FSV-CT 

FSV-CU 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DF 

FSV-DJ 

FSV-DP 

FSV-DR 

FSV-DU 

FSV-DW 

FSV-EL 

FSV-EM 

FSV-ES 0.014 0.014 nq 0.023 

FSV-FG 

FSV-FH 

243 244 245 246 

0.40 0.064 0.022 0.105 

0.46 0.080 0.027 0.142 

0.48 0.071 0.037 0.123 

0.59 0.076 0.035 0.159 

0.37 0.048 0.026 0.111 

0.34 0.040 nd 0.095 

0.54 0.071 0.038 0.154 

0.59 0.071 0.034 0.108 

0.54 0.091 0.038 0.139 

0.43 0.066 0.023 0.125 

0.33 0.025 0.006 0.060 

0.05 0.070 0.033 0.136 

0.54 0.041 nq 0.114 

0.15 0.023 0.014 0.035 

0.40 0.180 nd 0.210 

0.11 0.022 0.009 0.034 

0.54 0.102 0.040 0.176 

0.40 0.079 0.044 0.092 

0.61 0.093 0.035 0.178 

0.43 0.067 0.027 0.122 

0.42 nq nq 0.099 

0.31 0.039 !0.067 !0.025 

0.48 0.087 0.030 0.155 

0.36 0.060 0.010 0.100 

0.56 0.081 0.032 0.161 

0.60 0.101 0.021 0.159 

0.17 0.030 0.012 0.045 

0.68 0.079 <0.015 <0.195 

0.37 0.062 0.028 0.092 

243 244 245 246 

0.312 0.047 0.014 0.080 

0.274 0.030 0.020 0.058 

0.300 0.035 0.017 0.073 

0.220 0.033 0.017 0.050 

0.348 0.049 0.020 0.091 

0.314 0.050 0.032 0.089 

0.292 0.035 0.017 0.067 

0.104 0.018 0.007 0.024 

0.222 0.026 0.011 0.048 

243 244 245 246 

0.074 0.029 0.068 0.031 

0.043 0.006 0.005 0.011 

0.038 0.009 0.004 0.016 

0.050 0.009 nq 0.014 

0.071 nq nq 0.025 

0.059 0.011 0.005 0.022 

0.062 nd nd nd 

0.065 0.016 0.010 0.027 

0.047 0.010 nq 0.019 

0.041 0.010 0.003 0.013 

0.069 0.014 0.005 0.025 

0.024 0.005 0.001 0.016 

0.042 0.005 0.002 0.011 

0.057 0.009 0.005 0.018 

0.042 0.006 0.002 0.013 

0.058 0.010 0.005 0.018 

0.058 0.009 0.006 0.019 

0.041 0.007 0.005 0.014 

0.059 0.005 nq 0.018 

0.064 0.009 !0.018 !0.001 

0.052 0.008 0.003 0.016 

0.040 <0.01 <0.01 0.010 

0.065 0.010 0.004 0.015 

0.060 nq nq 0.014 

0.057 0.012 0.006 0.022 

0.065 <0.015 <0.015 <0.015 

0.067 0.007 nq 0.017 

243 244 245 246 

0.033 0.010 0.008 0.013 

0.040 0.006 0.004 0.012 

0.030 0.005 0.003 0.009 

0.049 0.007 0.005 0.015 

0.038 0.003 nd 0.012 

0.024 0.008 nd 0.008 

n 1 1 0 1 29 28 23 27 9 9 9 9 27 22 17 24 6 6 4 6 

Min 0.05 0.022 0.006 0.034 0.104 0.018 0.007 0.024 0.024 0.005 0.001 0.010 0.024 0.003 0.003 0.008 

Median 0.014 0.014 0.023 0.43 0.071 0.028 0.122 0.292 0.035 0.017 0.067 0.058 0.009 0.005 0.016 0.035 0.007 0.005 0.012 

Max 0.68 0.180 0.044 0.210 0.348 0.050 0.032 0.091 0.074 0.029 0.068 0.031 0.049 0.010 0.008 0.015 

eSD 0.16 0.020 0.010 0.044 0.033 0.013 0.004 0.025 0.012 0.003 0.001 0.004 0.008 0.002 0.003 

eCV 39 28 34 36 11 37 26 38 20 29 30 26 22 33 25 

NISTa 0.043 0.017 nd 0.025
 

NISTb
 0.014 0.016 nq 0.032 0.52 nq nq 0.203 0.234 0.037 nq 0.075 0.047 0.007 nq 0.016
 

NAV
 0.014 0.016 0.032 0.47 0.071 0.028 0.163 0.263 0.036 0.017 0.071 0.052 0.011 0.005 0.018 0.035 0.007 0.012 

NAU 0.15 0.025 0.010 0.071 0.078 0.013 0.006 0.023 0.019 0.007 0.003 0.007 

All Lab Report G4 Page 3 / 6 
 

Round Robin XLIII Laboratory Results 

All Values in μg/mL 

Total Lutein Total Zeaxanthin Total Lutein&Zeaxanthin 

Lab 243 244 245 246 243 244 245 246 243 244 245 246 

FSV-BA 0.178 0.061 0.042 0.096 

FSV-BD 0.076 0.024 0.013 0.050 0.031 0.008 0.002 0.016 0.107 0.032 0.015 0.066 

FSV-BE 

FSV-BF 0.110 0.041 0.018 0.078 

FSV-BG 0.094 0.022 0.013 0.047 0.023 0.007 0.005 0.013 0.128 0.032 0.020 0.066 

FSV-BH 0.061 0.023 0.012 0.046 0.024 0.007 0.004 0.014 0.085 0.030 0.016 0.060 

FSV-BI 0.060 0.023 0.012 0.047 0.024 0.008 0.005 0.016 0.084 0.031 0.017 0.063 

FSV-BIa 

FSV-BJ 0.066 0.025 0.012 0.044 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.071 0.029 0.013 0.049 0.016 0.004 0.001 0.009 0.081 0.033 0.015 0.056 

FSV-BO 0.121 0.037 0.020 0.063 0.044 0.013 0.010 0.023 0.166 0.050 0.030 0.086 

FSV-BQ 

FSV-BR 

FSV-BS 0.105 0.036 0.011 0.054 

FSV-BT 0.089 0.029 0.026 0.050 0.031 0.008 0.008 0.015 0.120 0.038 0.035 0.066 

FSV-BU 0.117 0.031 0.022 0.068 

FSV-BV 0.094 0.030 0.014 0.058 

FSV-BW 

FSV-BX 0.082 0.028 0.013 0.057 0.039 0.009 0.003 0.020 0.121 0.037 0.016 0.078 

FSV-BZ 0.078 0.019 0.002 0.028 

FSV-CB 0.086 0.028 0.007 0.059 0.035 0.009 nd 0.019 0.121 0.037 0.007 0.077 

FSV-CC 

FSV-CD 0.086 0.030 0.016 0.051 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CI 

FSV-CK 0.138 0.047 0.025 0.073 

FSV-CL 0.085 0.030 0.015 0.060 

FSV-CM 

FSV-CN 0.102 0.052 0.042 0.077 0.044 0.033 0.034 0.038 0.146 0.085 0.076 0.116 

FSV-CP 0.139 0.039 !0.071 !0.029 

FSV-CQ 

FSV-CR 

FSV-CS 0.132 0.033 0.018 0.069 

FSV-CT 0.079 0.028 0.015 0.052 0.025 0.008 0.004 0.018 0.104 0.036 0.019 0.070 

FSV-CU 

FSV-CX 0.040 0.010 <0.01 0.020 <0.01 <0.01 <0.01 <0.01 

FSV-DA 0.086 0.027 0.013 0.059 0.048 0.012 0.005 0.025 0.134 0.039 0.018 0.084 

FSV-DB 0.097 0.030 0.016 0.061 

FSV-DF 

FSV-DJ 

FSV-DP 

FSV-DR 

FSV-DU 

FSV-DW 0.090 0.030 0.015 0.057 0.047 0.012 0.010 0.023 0.137 0.042 0.025 0.080 

FSV-EL 

FSV-EM 0.152 0.022 0.017 0.105 

FSV-ES 0.067 0.018 0.009 0.043 0.031 0.006 nq 0.014 0.098 0.024 nq 0.057 

FSV-FG 

FSV-FH 

n 16 16 15 16 14 14 12 14 27 27 25 26 

Min 0.040 0.010 0.002 0.020 0.016 0.004 0.001 0.009 0.066 0.022 0.007 0.044 

Median 0.081 0.028 0.013 0.050 0.031 0.008 0.005 0.017 0.117 0.033 0.017 0.067 

Max 0.121 0.052 0.042 0.077 0.048 0.033 0.034 0.038 0.178 0.085 0.076 0.116 

eSD 0.014 0.006 0.003 0.010 0.011 0.002 0.003 0.005 0.030 0.006 0.003 0.015 

eCV 17 22 23 21 35 20 68 28 25 18 17 22 

NISTa 

NISTb 

NAV 

NAU 

0.067 0.021 0.012 0.064 

0.090 0.026 0.013 0.054 

0.041 nd nd 0.024 

0.052 0.013 0.005 0.026 

0.107 

0.141 

>0.021 

0.039 

>0.012 

0.019 

0.088 

0.080 

0.079 0.026 0.013 0.055 

0.018 0.007 0.003 0.013 

0.039 0.010 0.005 0.021 

0.017 0.005 0.004 0.008 

0.121 

0.030 

0.032 

0.008 

0.016 

0.005 

0.075 

0.019 

All Lab Report G5 Page 4 / 6 
Round Robin XLIII Laboratory Results 

Analytes Reported By One Laboratory 

Values in μg/mL 

Term 

n 

Min 

Median
 

Max
 

eSD
 

eCV
 

NAV
 

NAU
 

nd 

nq 

<x 

>x 

! 

italics 

Analyte Code 243 244 245 246 

Coenzyme Q10 FSV-CH 0.416 0.099 0.085 0.260 

Phytoene FSV-CL 0.105 0.126 0.059 0.199 

Phytofluene FSV-CL 0.053 0.027 0.005 0.039 

Total Carotenoids FSV-EM 1.28 0.54 0.20 1.16 

Total cis-β-Cryptoxanthin FSV-BT 0.027 0.005 0.001 0.008 

trans-anhydro-Lutein FSV-BT 0.054 0.013 0.009 0.025 

Legend 

Definition

 Number of (non-NIST) quantitative values reported for this analyte

 Minimum (non-NIST) quantitative value reported

 Median (non-NIST) quantitative value reported

 Maximum (non-NIST) quantitative value reported

 Estimated standard deviation, calculated from the median absolute deviation

 from the median of the non-NIST results

 Coefficient of Variation for (non-NIST) results: 100*eSD/Median

 NIST Assigned Value, our estimate of the "true" analyte concentration

 NIST Assigned Uncertainty, our estimate of the total (serum hetergeniety and

 inter- and intra-laboratory) standard deviation

 For details on how we assign these quantities, see the "Analysis of Results."

 Not detected (i.e., no detectable peak for analyte)

 Detected but not quantitatively determined

 Concentration at or below the limit of quantification, x 

 Concentration at least as large as x

 Discrepant value: heterogeneous serum, damaged sample, malfunction, etc.

 Not explicitly reported but calculated by NIST from reported values

All Lab Report G6 Page 5 / 6 
 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Round Robin XLIII Laboratory Results 

Lab 

FSV-BA
 

FSV-BD
 

FSV-BE
 

FSV-BF
 

FSV-BG
 

FSV-BH
 

FSV-BI
 

FSV-BIa
 

FSV-BJ
 

FSV-BK
 

FSV-BL
 

FSV-BM
 

FSV-BN
 

FSV-BO
 

FSV-BQ
 

FSV-BR
 

FSV-BS
 

FSV-BT
 

FSV-BU
 

FSV-BV
 

FSV-BW 

FSV-BX 

FSV-BZ 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CI 

FSV-CK 

FSV-CL 

FSV-CM 

FSV-CN 

FSV-CP 

FSV-CQ 

FSV-CR 

FSV-CS 

FSV-CT 

FSV-CU 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DF 

FSV-DJ 

FSV-DP 

FSV-DR 

FSV-DU 

FSV-DW 

FSV-EL 

FSV-EM 

FSV-ES 

FSV-FG 

FSV-FH 

NISTa 

NISTb 

n 

% 1 

% 2 

% 3 

% 4 

R aT gT bC tbC 

1	 1 1 1 

1 

1	 2 1 1 

2 2 2 

2	 1 1 3 

1 2 1 

1	 1 1 2 

3	 1 1 1 1 

1	 2 2 2 1 

2	 2 1 3 

2	 1 1 4 

3 3 

1 

4	 4 

1	 3 2 2 

1	 1 

1 1 1 

1 1 1 

3	 2 3 3 

2	 2 1 2 

1	 1 2 1 

3 2 2 

2	 1 1 1 1 

2 2 

3 3 4 

4 3 1 

4	 2 1 2 2 

1 

3	 1 

1	 3 

3	 2 

2	 3 

2	 1 1 2 

1 1 2 

2	 1 4 1 

1	 2 1 2 1 

1 

3 

3	 2 1 1 

1 1 3 2 

2	 1 

1	 1 1 1 

1	 2 

1	 2 2 2 1 

2 2 4 

2 1 2 

2 2 3 

2	 2 

1 2 3 

3	 3 

1 1 2 

2 

2 2 2 2 

1 

1 1 1 1 1 

1 1 1 1 1 

50 48 23 32 11 

TR aT g/bT bC tbC 

42 44 65 34 55 

34 40 17 44 36 

18 15 13 16 0 

6 2 4 6 9 

All Lab Report 

Comparability Summary 

Definition 

Participant code 

"Standard Score" for Retinol 

"Standard Score" for α-Tocopherol 

"Standard Score" for γ-Tocopherol 

"Standard Score" for Total β-Carotene 

"Standard Score" for trans-β-Carotene 

number of laboratories providing data for this analyte for at least one serum 

"Standard Score" 

Given that our knowledge of the shapre, location, and width of the measurement 

distributions is approximate and that a limited number of laboratories are involved, we 

summarize comparability with the following 3-level "Standard Score" (StS)... 

Label 

Lab 

R 

aT 

gT 

bC 

tbC 

n 

StS 

A 

B 

C 

where: 

StV 

NAV 

NAU 

t (1-α,n-1) 

Definition 

All StV within ±t (1-0.683,n-1) (i.e., ±1 SD) 

All StV within ±t (1-0.954,n-1) (i.e., ±2 SD) 

At least one StV > ±t (1-0.954,n-1) (i.e., ≥2 SD) 

Standardized Value, the distance in standard deviation units your value is from 

the "true" concentration: StV = (your value - NAV) / NAU 

NIST Assigned Value, our estimate of the "true" analyte concentration 

NIST Assigned Uncertainty, our estimate of the total (serum heterogeneity and 

inter- and intra-laboratory measurement) standard deviation 

Two-tailed Student's t for coverage of ±1 and ±2 NAU about NAV assuming a 

normal population of size n 

Expected 

68.2 % These are the observed and normal-population-expected proportions 

27.3 % of each Standard Score (StS), based upon each laboratory's largest 

4.3 % StV for the four sera. 

0.3 % 

G7	 Page 6 / 6 
 

Appendix H. Representative “Individualized Report” for RR43 

Each participant in RR43 received an “Individualized Report” reflecting their reported 

results. Each report included a detailed analysis of the results they reported for the 

following analytes: 

• Total Retinol 

• α-Tocopherol 

• γ-Tocopherol 

• Total β-Carotene 

• trans-β-Carotene 

• Total α-Carotene 

• Total Lycopene 

• trans-Lycopene 

The following nine pages are the “Individualized Report” for the analytes evaluated by 

participant FSV-BA. 

Note 

The design file and program used to generate the original RR43 “Individualized 

Reports” are no longer available. The following pages were produced using the 

2013 version of the program (a linear descendant of that used in 1998) and a 

re-created design file. 

H1
 

 Set 1 of 54 

Individualized Round Robin XLIII Report: FSV-BA 

Summary 

Serum 243 Serum 244 Serum 245 Serum 2

Analyte You NAV n You NAV n You NAV n You NA

Retinol 0.591 0.462 50 0.484 0.370 50 0.247 0.192 49 0.809 0.7

Retinyl Palmitate 0.112 0.112 13 0.096 0.109 13 0.045 0.052 12 0.246 0.2

α-Tocopherol 7.22 7.01 47 7.1 7.2 48 3.4 3.5 47 14.44 14.3

γ-Tocopherol 2.18 2.26 23 1.31 1.27 23 0.71 0.68 22 2.44 2.5

Total β-Carotene 0.085 0.072 32 0.337 0.359 32 0.131 0.133 31 0.703 0.6

trans-β-Carotene 0.079 0.070 11 0.315 0.323 11 0.123 0.133 11 0.669 0.6

Total cis-β-Carotene 0.006 0.004 7 0.022 0.037 8 0.008 0.014 8 0.034 0.0

Total α-Carotene 0.013 0.014 24 0.013 0.020 24 0.008 0.010 20 0.041 0.0

trans-Lycopene 0.312 0.263 9 0.047 0.036 9 0.014 0.017 9 0.080 0.0

Total β-Cryptoxanthin 0.074 0.052 27 0.029 0.011 22 0.068 0.005 17 0.031 0.0

Total Lutein&Zeaxanthin 0.178 0.121 27 0.061 0.032 27 0.042 0.016 25 0.096 0.0

H2

You : Your reported values for the listed analytes (micrograms/milliliter)
 

NAV : NIST Assigned Values, here equal to this RR's median
 

n : Number of non-NIST laboratories reporting quantitative values for this analyte in this serum 

Please check our records against your records. Send corrections and/or updates to... 

Micronutrients Measurement Quality Assurance Program 

National Institute of Standards and Technology Tel: (301) 9

100 Bureau Drive Stop 8392 Fax: (301) 9

Gaithersburg, MD 20899-8392 USA Email: david.duewer@

Individualized Report 
 

 Set 1 of 54 

Individualized RR XLIII Report: FSV-BA 

Retinol, μg/mL 

Apparent Precision, SD 

Median [Analyte], μg/mL 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR 

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#243 Lyophilized, single-donor, augmented with retinyl palmitate RR28:#181, RR37:#222 

#246 Lyophilized, single donor, native RR31:#198, RR35:#212 

#242 Lyophilized, multi-donor, a 1:1 blend of the#241 pool and delipidized serum. RR31:#195, RR35:#214 

#239 Lyophilized, multi-donor, a 1:3 blend of the #241 pool and delipidized serum. RR31:#197, RR35:#211 Apparent Precision, SD [Analyte], μg/mL 181 222 243 198 212 246 195 214 244 197 211 245 Your [Analyte], μg/mL 

Individualized Report Page 2 / 8 

H3
 

 Set 1 of 54 

Individualized RR XLIII Report: FSV-BA 

α-Tocopherol, μg/mL 

Apparent Precision, SD 

Median [Analyte], μg/mL 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR 

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#243 Lyophilized, single-donor, augmented with retinyl palmitate RR28:#181, RR37:#222 

#246 Lyophilized, single donor, native RR31:#198, RR35:#212 

#242 Lyophilized, multi-donor, a 1:1 blend of the#241 pool and delipidized serum. RR31:#195, RR35:#214 

#239 Lyophilized, multi-donor, a 1:3 blend of the #241 pool and delipidized serum. RR31:#197, RR35:#211 Apparent Precision, SD [Analyte], μg/mL 181 222 243 198 212 246 195 214 244 197 211 245 Your [Analyte], μg/mL 

Individualized Report Page 3 / 8 

H4
 

 Set 1 of 54 

Individualized RR XLIII Report: FSV-BA 

γ-Tocopherol, μg/mL 

Apparent Precision, SD 

Median [Analyte], μg/mL 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR 

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#243 Lyophilized, single-donor, augmented with retinyl palmitate RR28:#181, RR37:#222 

#246 Lyophilized, single donor, native RR31:#198, RR35:#212 

#242 Lyophilized, multi-donor, a 1:1 blend of the#241 pool and delipidized serum. RR31:#195, RR35:#214 

#239 Lyophilized, multi-donor, a 1:3 blend of the #241 pool and delipidized serum. RR31:#197, RR35:#211 Apparent Precision, SD [Analyte], μg/mL 181 222 243 198 212 246 195 214 244 197 211 245 Your [Analyte], μg/mL 

Individualized Report Page 4 / 8 

H5
 

 Set 1 of 54 

Individualized RR XLIII Report: FSV-BA 

Total β-Carotene, μg/mL 

Apparent Precision, SD 

Median [Analyte], μg/mL 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR 

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#243 Lyophilized, single-donor, augmented with retinyl palmitate RR28:#181, RR37:#222 

#246 Lyophilized, single donor, native RR31:#198, RR35:#212 

#242 Lyophilized, multi-donor, a 1:1 blend of the#241 pool and delipidized serum. RR31:#195, RR35:#214 

#239 Lyophilized, multi-donor, a 1:3 blend of the #241 pool and delipidized serum. RR31:#197, RR35:#211 Apparent Precision, SD [Analyte], μg/mL 181 222 243 198 212 246 195 214 244 197 211 245 Your [Analyte], μg/mL 

Individualized Report Page 5 / 8 

H6
 

 Set 1 of 54 

Individualized RR XLIII Report: FSV-BA 

trans-β-Carotene, μg/mL 

Apparent Precision, SD 

Median [Analyte], μg/mL 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR 

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#243 Lyophilized, single-donor, augmented with retinyl palmitate RR28:#181, RR37:#222 

#246 Lyophilized, single donor, native RR31:#198, RR35:#212 

#242 Lyophilized, multi-donor, a 1:1 blend of the#241 pool and delipidized serum. RR31:#195, RR35:#214 

#239 Lyophilized, multi-donor, a 1:3 blend of the #241 pool and delipidized serum. RR31:#197, RR35:#211 Apparent Precision, SD [Analyte], μg/mL 181 222 243 198 212 246 195 214 244 197 211 245 Your [Analyte], μg/mL 

Individualized Report Page 6 / 8 

H7
 

 Set 1 of 54 

Individualized RR XLIII Report: FSV-BA 

Total α-Carotene, μg/mL Your [Analyte], μg/mL 

[Analyte], μg/mL

Median [Analyte], μg/mL 

181222243198212

246195214244197211245 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR 

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#243 Lyophilized, single-donor, augmented with retinyl palmitate RR28:#181, RR37:#222 

#246 Lyophilized, single donor, native RR31:#198, RR35:#212 

#242 Lyophilized, multi-donor, a 1:1 blend of the#241 pool and delipidized serum. RR31:#195, RR35:#214 

#239 Lyophilized, multi-donor, a 1:3 blend of the #241 pool and delipidized serum. RR31:#197, RR35:#211 

Individualized Report Page 7 / 8 

H8
	
 

 Set 1 of 54 

Individualized RR XLIII Report: FSV-BA 

trans-Lycopene, μg/mL 

Apparent Precision, SD 

Median [Analyte], μg/mL 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR 

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#243 Lyophilized, single-donor, augmented with retinyl palmitate RR28:#181, RR37:#222 

#246 Lyophilized, single donor, native RR31:#198, RR35:#212 

#242 Lyophilized, multi-donor, a 1:1 blend of the#241 pool and delipidized serum. RR31:#195, RR35:#214 

#239 Lyophilized, multi-donor, a 1:3 blend of the #241 pool and delipidized serum. RR31:#197, RR35:#211 [Analyte], μg/mL 181 222 243 198 212 246 195 214 244 197 211 245 Your [Analyte], μg/mL Apparent Precision, SD 

Individualized Report Page 8 / 8 

H9
Appendix I. Shipping Package Inserts for RR44 

The following two items were included in each package shipped to an RR44 participant: 

• Cover letter 

• Datasheet 

The cover letter and datasheet were enclosed in a sealed waterproof bag along with the 

samples themselves. 

I1
UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899-0001 

October 30, 1998 

Dear Colleague: 

Enclosed is the set of samples for the third quality assurance round robin exercise (Round Robin XLIV) 

for FY9 8. y OU will find one vial of each of four lyophilized serum samples for analysis along with a 

form for reporting your results. When reporting your results, please submit one value for each analyte 

for a given serum sample. If an obtained value is below your limit of quantitation, please indicate this 

result on the form by using NQ (Not Quantitated). For analytes not measured, please leave a blank. 

Results are due to NIST by October 9, 1998. Results received two weeks after the due date will not be 

included in the summary report for this round robin study. Written feedback concerning the study will 

be provided around November 13. 

Samples should be reconstituted with 1.0 mL ofHPLC-grade water or equivalent. We recommend that 

dissolution be facilitated with 3 to 5 min agitation in an ultrasonic bath or at least 30 min at room 

temperature with intermittent swirling. (CAUTION: Vigorous shaking will cause foaming and possibly 

interfere with accurate measurement. The rubber stopper contains phthalate esters that will leach into the 

sample upon intermittent contact of the liquid sample with the stopper. Tues~ esters absorb strongly in 

the UV region and elute very near retinal in most LC systems creating analytical problems.) Pipette a 

known volume of serum from the vial for analysis. (The final volume of the reconstituted sample is 

greater than 1.0 mL.). For consistency, we request that laboratories use the following absorptivities (E. 

1 % cm) in ethanol: retinal, 1843 at 325 run; retinyl palmitate, 975 at 325 nm; a-tocopherol, 75.8 at 292 

nm; y-tocopherol, 91.4 at 298 nm; a-carotene, 2800 at 444 run (in hexane); P-carotene, 2560 at 450 nm 

(in ethanol), 2592 at 452 nm (in hexane); lycopene, 3450 at 472 nm (in hexane). 

Please mail or fax your results for Round Robin XLIV to: 

Micronutrients Measurement Quality Assurance Program 

NIST 

Bldg.222,Rm.B208 

Gaithersburg, MD 20899 

Fax: (301) 977-0685 

If you have questions regarding this round robin exercise, please call me at (301) 975-3120; 

e-mail me at jeanice.brownthomas@nist.gov; or mail/fax queries to the above address. 

nice Brown Thomas 

esearch Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

Enclosures 

cc: S. Wise NISI 

Note: Actual date was sometime in August, 1998
­

I2
 

 

 

NIST 

Micronutrients Measurement Quality Assurance Program 

Round Robin XLIV Results from Laboratory #_____ 

Serum 

Analyte 247 248 249 250 Units* 

retinol 

retinyl palmitate 

α-tocopherol 

γ-tocopherol 

δ-tocopherol 

total β-carotene 

trans-β-carotene 

total cis-β-carotene 

total α-carotene 

trans-α-carotene 

total lycopene 

trans-lycopene 

β-cryptoxanthin 

α-cryptoxanthin 

“lutein” 

“zeaxanthin” 

“lutein&zeaxanthin” 

Other Analytes?
 

* We prefer mg/mL 

Today's Date: 

Comments? 

Mail: MMQAP, 222/B208 

NIST Please return results on-or-before Fax: 301-977-0685 

Gaithersburg, MD 20899 9-Oct-98 Email: David.Duewer@NIST.gov 

I3
 

 

Appendix J. Final Report for RR44 

The following four pages are the final report as provided to all participants: 

•	 Cover letter 

•	 An information sheet that: 

o	 describes the contents of the “All-Lab” report 

o	 describes the nature of the test samples and details any previous distributions 

o	 summarizes aspects of the study that we believe may be of interest to the 

participants 

J1
November 23, 1998 

Dear Colleague: 

UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899-0001 

Enclosed is the summary report of the results for Round Robin XLIV (RR44). Included in this report 

are: a summary of data for all laboratories; the measurement comparability summru-Y for evaluating 

laboratory performance; a summary of individual laboratory performance and interlaboratory accuracy 

and precision; and a summary of the NIST ,assigned value (NA V) vs. your laboratory value for the 

analytes measured. As in previous reports. the NIST assigned values are derived from the equally 

weighted results from the analyses performed by NIST and the laboratories that participated in this 

interlaboratory comparison exercise. 

In this round exercise. serum samples (Sera 248-249) were new distributions. Sera 248 and 249 are new 

serum pools to be used for candidate Standard Reference Material (SRM) 968c, Fat-Soluble Vitamins, 

Cholesterol. and Caroten01ds m Hum an Serum. Serum 24 7 is a blend (1: 1) of sera 248 and 249. Serum 

250 was distributed in three previous round robins (round robins 30, 32, and 36 as Sera 192, 199, and 

218, respectively). Per your request. a detailed (but brief) summary for this interlaboratory comparison 

exercise is provided in the anached report. 

Data for evaluating laboratory performance in RR44 are provided in the comparability summary (Score 

Card) on page 6 of the "All Lab Report." The criteria used to evaluate laboratory performance are as 

follows: results rated l (within l SD of the assigned value) indicate EXCEPTIONAL performance, 

results rated 2 (within 2 SD) indicate ACCEPTABLE performance, results rated 3 (within 3 SD of the 

assigned value) are MARGINAL. and those rated 4 (>3 SD from the assigned value) indicate POOR 

performance relative to the current state-of-the-practice for these measurements. 

If you have concerns regarding your laboratory performance, we suggest that you obtain a unit of SRM 

968b, Fat-Soluble Vitamins and Cholesterol in Human Serum, and analyze all three levels. If your 

measured values do not agree with the certified values, we suggest that you cont~ct us for consultation. 

Thank you for your responses regarding the continuance of the Micronutrients Measurement Quality 

Assurance (QA) Program. Due to the positive feedback, the QA program will continue through FY 99. 

The Intent-to-Participate form, which will provide us with formal notification of your intent to 

participate in the program for the upcoming year, has been mailed. Please contact us if you have not 

received your form. 

As mentioned in your participation letter, the program will consist of two round robin studies for the fatsoluble vitamins and carotenoids and one study for vitamin C. The participation fee for the fat-soluble 

vitamins and carotenoids will be $665 for U.S. laboratories and $1020 for laboratories outside of the U.S. 

To participate in the vitamin C study, there will be a fee of $370 for U.S. laboratories and $530 for 

laboratories outside of the U.S. 

Over the years, we have acquired a limited supply of well-characterized serum pools that were used in 

previous intercomparison exercises for the QA program. These materials can be used by laboratories as 

in-house control materials and will be made available to you at a nominal cost ($50 per vial). We will 

provide you with more details in a separate cover in January. 

J2

NISI 
The next QA workshop will be held as a pre-meeting on Friday, April 16 at Experimental Biology '99 in 

Washington, DC. Details regarding the workshop, housing information, and registration forms will be 

mailed to you at the beginning of next year. If you would like details regarding the conference, please 

contact the secretariat for the American Institute of Nutrition at (301)530-7050; fax: (301)571-1892; email: sec@asns.faseb.org. 

Enclosed please find a reprint on.the stability of vitamins in human serum and a draft of a manuscript, 

which has been submitted to Analytical Chemistry, on the use of interlaboratory comparison exercise 

results. If you have any questions regarding this report, please contact me at 301/975-3120; FAX: 

301/977-0685; e-mail: jeanice.brownthomas@nist.gov. 

Sincerely, 

J anice Brown Thomas 

Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

cc: S. Wise 

Enclosures 

J3
The NIST M2

QAP Round Robin XLIV (RR44) report includes: 

Page "All Lab" Report 

1-4 A listing of all results and statistics for analytes reported by at least two laboratories 

Sa A list ofresults for five analytes reported by only one laboratory 

Sb A legend for the above two lists 

6 A "Comparability Summary" or "Score Card" for retinal, a-tocopherol, y-tocopherol, total 

and trans-P-carotene, total a-carotene, P-cryptoxanthin, and total lycopene. 

Page "Individualized" Report 

l A summary of your data and the NIST assigned values 

2, 3 Summary box plots for retinal, a-tocopherol, y-tocopherol, total and trans-P-carotene, total 

a-carotene, P-cryptoxanthin. total and trans-lycopene, lutein, and zeaxanthin 

4, S Concordance/apparent precision plots for retinal, a-tocopherol, y-tocopherol, total and 

trans-P-carotene, total a-carotene. P-cryptoxanthin, total and trans-lycopene, lutein, and 

zeaxanthin 

6 Youden comparability plots for retinal, a-tocopherol,_y-tocopherol, and total and 

trans-P-carotene 

All elements of this report should be familiar to you, although the names of the various elements have 

changed somewhat from previous versions. The enclosed preprint "M2

QAP: Helping Participants Use 

Interlaboratory Comparison Exercise Results to Improve Their Long-term Measurement Performance" 

details the nomenclature, construction, and interpretation of the three plot types. 

Please note that we no longer report "percent bias" (IOO[you-NAV]/NAV) but rather use z-scores ([youNA V]/NAU) throughout, where NA V and NAU are our assignments of analyte value and total 

measurement uncertainty. 

Samples. Three new and one "old" sera were distributed in RR44. 

Sera 248 and 249 are new: they are the two components of candidate SRM® 968c. These two 

materials were prepared from well-characterized serum pools. All carotenoid levels are "native" but 

the sera were augmented with retinal, a-tocopherol, y-tocopherol, and/or 6-tocopherol. 

Serum 247 is new: it is a 1: l blend of the 248 and 249 serum pools, with an experimental liposomic 

augmentation of trans-P-carotene and P-cryptoxanthin. Since this material was prepared from the 

"tag-ends" of the pools after all 248 and 249 production was complete, it provides an independent 

check for analyte degradation in the 248 and 249 pools. 

Serum 250 was previously distributed as 192 in RR30, 199 in RR32, and 218 in RR36. This material 

was augmented with retinal and retinyl palmitate, but is natively high in most carotenoids. 

Qualitative Results. One participant noted an integration problem with their retinal peak due to a small 

leading peak. In retrospect, we often see some early-elution "junk" in many of our lyophilized sera; 

differential resolution/integration of these interferents (esters?) may contribute to the remaining 

inter laboratory retinal differences. Add this to the list of research topics! 

J4
Quantitative Results. To preserve resources and sanity, we no longer report our detailed dissection of 

the NIST measurements. We do include the most relevant statistics of this analysis in the "All 

Laboratory" report. The following summary conclusions draw from both the NIST and RR44 analyses. 

Sera 248 and 249: these materials are more-than-adequately homogenous, reconstitute well, and 

contain no "unusual" interferents. The measured levels of all analytes are adequately close to the 

design levels. Systematic zeaxanthin differences between the two sets of NIST analyses suggest that 

our assays are measuring different sets of carotenoid components for this analyte. Differences in 

lycopene levels between NIST3 and the RR44 expected values suggest that our trans-lycopene may 

include some cis-lycopene component(s). The C30 column measurements should help resolve these 

issues. 

Serum 247: the measured levels of all analytes are very close to the expected (248 + 249)/2. This 

confirms that the composition of the serum pools used for sera 248 and 249 did not change during 

the production process. The experimental P-carotene and P-cryptoxanthin augmentation either did 

not "take" and/or hexane does not appreciably extract analyte from the liposomes. 

Serum 250: The composition of this material is apparently unchanged by its five years' storage at 

-80 °C, using both the formal statistical tests of level and variance and "Mark I eyeball" of the 

summary box plots. Almost all participants who reported discordant values for sera 247-249 

reported a similarly discordant value for serum 250 (see the "target" plots in the Individualized 

Report). Since there is no compositional relationship between serum 250 and sera 247-249, these 

systematic differences are unlikely to be sample-related. 

Analyte nomenclature: total, trans-, and total cis-. There is considerable variation in the reportage of 

"speciated" carotenoids, particularly when cis-isomers are detected but not quantitatively determinable. 

This is (currently) mostly a problem with P-carotene. We propose the following rules: 

If your system does not routinely resolve the isomers, don't worry about it and just report "Total". 

If your system does routinely resolve the isomers but one or more cannot be quantitatively measured, 

report just these isomers as "not detected (nd)" or "not quantified (nq)". Report any composite 

analyte as ">" (or"~") the appropriate partial value. That is: a "total" normally calculated from 

trans+ cis peak areas (whether or not separately integrated) should be reported as ">"trans if the cis 

is "nq". Reporting "nq" for the total in this situation is confusing if you don't typically report 

explicit cis values! 

If you report any two of the "total= trans+ cis" trio, we will calculate the third. These calculated values 

(like "lutein & zeaxanthin" from "lutein" + "zeaxanthin") are listed in italics in the "All Laboratory 

Report". 

David L. Duewer 

J5
 

Appendix K. “All-Lab Report” for RR44 

The following six pages are the “All-Lab Report” as provided to all participants, with two 

exceptions: 

• the participant identifiers (Lab) have been altered. 

• the order in which the participant results are listed has been altered. 

The data summary in the “All-Lab Report” has been altered to ensure confidentiality of 

identification codes assigned to laboratories. The only attributed results are those 

reported by NIST. The NIST results are not used in the assessment of the consensus 

summary results of the study. 

K1
Round Robin XLIV Laboratory Results 

All Results in μg/mL 

Lab 247 

Retinol 

248 249 250 

Retinyl Palmitate α-Tocopherol γ-Tocopherol δ-Tocopherol 

FSV-BA 0.664 0.849 0.488 1.120 

FSV-BB 0.711 0.886 0.519 1.130 

FSV-BBa 

FSV-BD 0.650 0.854 0.482 1.075 

FSV-BE 0.660 0.860 0.480 1.060 

FSV-BF 0.743 0.871 0.499 1.017 

FSV-BG 0.658 0.855 0.473 1.122 

FSV-BH 0.651 0.790 0.474 1.004 

FSV-BI 0.694 0.823 0.504 1.108 

FSV-BJ 0.742 0.920 0.518 1.168 

FSV-BK 0.631 0.832 0.473 1.043 

FSV-BL 0.340 0.460 0.260 0.600 

FSV-BM 0.705 0.877 0.509 1.053 

FSV-BN 0.636 0.851 0.499 1.061 

FSV-BO 0.739 0.899 0.544 1.255 

FSV-BP 0.600 0.952 0.546 1.214 

FSV-BQ 0.748 0.917 0.544 1.163 

FSV-BR 0.720 0.920 0.520 1.130 

FSV-BS 0.672 0.944 0.566 1.098 

FSV-BT 0.681 0.797 0.420 1.003 

FSV-BU 0.642 0.882 0.494 1.092 

FSV-BV 0.799 1.090 0.563 1.270 

FSV-BW 0.700 0.903 0.490 1.008 

FSV-BX 0.649 0.838 0.457 1.062 

FSV-BZ 

FSV-CB 0.715 0.887 0.517 1.134 

FSV-CC 0.609 0.816 0.452 0.969 

FSV-CD 0.724 0.823 0.475 0.971 

FSV-CE 0.591 0.712 0.473 1.030 

FSV-CF 0.715 0.854 0.503 1.128 

FSV-CH 0.616 0.849 0.450 1.020 

FSV-CI 0.750 0.970 0.550 1.210 

FSV-CL 0.625 0.843 0.434 0.998 

FSV-CM 

FSV-CP 

FSV-CR 0.740 0.960 0.510 1.170 

FSV-CS 0.636 0.823 0.448 1.073 

FSV-CU 0.559 0.728 0.406 0.949 

FSV-CX 0.700 0.830 0.480 1.140 

FSV-DA 0.638 0.807 0.460 0.968 

FSV-DB 0.646 0.763 0.443 1.015 

FSV-DF 0.680 0.850 0.470 1.130 

FSV-DJ 0.660 0.860 0.480 1.020 

FSV-DK 0.550 0.690 0.410 0.840 

FSV-DP 0.681 0.871 0.478 1.122 

FSV-DR 0.640 0.840 0.630 1.700 

FSV-DU 0.710 0.900 0.520 1.090 

FSV-DW 0.706 0.800 0.434 1.137 

FSV-ES 0.656 0.859 0.504 1.117 

FSV-FG 0.660 0.840 0.450 1.000 

FSV-FH 

247 248 249 250 

0.081 0.061 0.107 0.075 

0.052 0.022 0.077 0.040 

0.051 0.029 0.070 0.060 

0.039 0.030 0.095 nq 

0.069 0.046 0.109 nd 

0.045 nq 0.076 nq 

0.041 0.028 0.077 0.023 

0.047 0.030 0.101 0.024 

0.060 0.033 0.103 nq 

0.122 0.084 0.151 0.119 

0.040 0.030 0.090 0.040 

0.073 0.057 0.083 0.065 

0.010 0.010 0.050 0.060 

nd nd 0.050 nd 

0.035 0.025 0.052 0.020 

247 248 249 250 

10.9 7.32 15.5 6.92 

10.9 6.90 15.7 6.55 

12.6 7.95 17.6 7.11 

10.9 8.10 15.8 7.20 

10.3 6.80 14.7 6.30 

12.7 7.73 17.6 7.14 

12.2 7.99 17.6 7.33 

11.6 7.37 17.0 6.97 

11.0 6.96 16.1 6.98 

12.6 8.22 17.3 7.61 

11.6 7.59 16.6 7.01 

7.3 5.17 10.3 4.74 

11.0 7.10 15.7 7.00 

11.9 7.44 18.1 7.17 

15.0 10.85 21.1 8.74 

11.8 7.99 17.8 7.67 

10.7 6.65 15.2 6.29 

8.9 5.62 14.2 6.42 

10.6 7.04 15.6 6.84 

11.4 7.58 17.0 6.92 

10.1 6.42 14.7 6.10 

11.8 7.70 16.4 6.91 

12.1 4.90 14.3 5.50 

11.4 6.64 15.4 6.53 

12.1 7.62 16.9 7.42 

13.2 7.88 17.5 7.43 

12.0 7.35 18.3 7.57 

12.9 7.90 18.0 7.40 

10.4 7.68 16.7 6.89 

10.2 6.10 15.4 5.90 

16.0 12.16 21.2 10.69 

10.1 6.20 16.9 7.33 

11.8 7.97 16.7 7.38 

12.5 8.10 17.7 7.30 

11.5 6.70 15.2 6.11 

9.7 6.65 13.3 6.76 

11.6 7.12 16.5 7.32 

11.4 7.20 16.3 6.75 

11.2 6.93 16.1 6.74 

12.4 9.00 16.8 9.13 

11.5 7.65 25.1 11.56 

13.2 8.02 18.1 7.80 

12.6 7.81 17.1 8.05 

12.9 8.15 18.8 8.06 

11.4 6.65 16.6 6.60 

11.4 6.80 16.4 6.90 

247 248 249 250 

2.42 3.65 1.48 2.34 

3.09 4.48 1.86 2.60 

2.59 3.96 1.49 2.28 

2.70 4.00 1.60 2.50 

2.74 3.80 1.61 2.26 

2.58 3.81 1.56 2.36 

2.67 3.90 1.61 2.35 

2.40 3.56 1.54 2.20 

2.95 4.13 1.63 2.54 

2.33 3.41 1.49 2.01 

2.85 3.78 1.96 2.51 

2.73 3.30 1.43 2.03 

2.88 4.54 1.72 2.60 

2.82 4.20 1.70 2.55 

2.65 3.87 1.63 2.36 

3.60 3.30 1.90 2.30 

2.77 3.80 1.47 2.30 

2.18 3.43 1.38 1.86 

3.02 4.80 1.60 2.72 

2.78 4.08 1.67 2.53 

3.06 4.17 1.65 2.46 

2.76 3.97 1.66 2.32 

5.89 7.36 4.16 5.57 

247 248 249 250 

0.389 0.164 0.581 0.163 

1.553 1.262 1.752 0.604 

0.400 <0.3 0.700 <0.3 

0.403 0.183 0.658 0.176 

N 46 46 46 46 14 13 15 10 46 46 46 46 23 23 23 23 4 3 4 3 

Min 0.340 0.460 0.260 0.600 0.010 0.010 0.050 0.020 7.3 4.90 10.3 4.74 2.18 3.30 1.38 1.86 0.389 0.164 0.581 0.163 

Median 0.662 0.853 0.481 1.083 0.049 0.030 0.083 0.050 11.5 7.40 16.6 7.01 2.76 3.90 1.61 2.36 0.402 0.183 0.679 0.176 

Max 0.799 1.090 0.630 1.700 0.122 0.084 0.151 0.119 16.0 12.16 25.1 11.56 5.89 7.36 4.16 5.57 1.553 1.262 1.752 0.604 

eSD 0.056 0.047 0.043 0.089 0.016 0.007 0.026 0.030 1.0 0.86 1.4 0.59 0.25 0.37 0.13 0.22 

eCV 9 5 9 8 32 25 32 59 9 12 9 8 9 10 8 9 

Npast 0 0 0 44 0 0 0 7 0 0 0 44 0 0 0 20 0 0 0 6 

Medianpast 1.078 0.054 7.18 2.47 0.110 

SDpast 0.112 0.038 0.57 0.29 0.020 

NISTa 0.691 0.821 0.481 1.012 12.4 7.83 17.4 7.16 2.65 3.97 1.49 2.25 0.296 0.133 0.465 nd 

NISTb 0.662 0.847 0.491 1.064 11.6 7.19 16.4 6.71 2.70 3.84 1.57 2.30 0.346 0.128 0.588 0.132 

NNIST 5 22 22 6 5 22 22 6 5 22 22 6 5 22 22 3 

Mean 0.677 0.834 0.486 1.038 12.0 7.51 16.9 6.94 2.68 3.90 1.53 2.27 0.321 0.131 0.526 0.132 

Srep 0.047 0.014 0.007 0.028 0.4 0.21 0.2 0.15 0.17 0.07 0.04 0.03 0.006 0.007 0.015 0.004 

Shet 0.018 0.013 0.008 0.029 0.3 0.11 0.2 0.06 0.06 0.03 0.02 0.04 0.002 0.004 0.016 0.004 

Sanl 0.021 0.018 0.007 0.037 0.6 0.46 0.7 0.31 0.04 0.09 0.06 0.04 0.035 0.004 0.087 

SNIST 0.055 0.026 0.013 0.055 0.8 0.51 0.8 0.35 0.18 0.12 0.07 0.06 0.036 0.009 0.090 0.006 

NAV 0.669 0.843 0.483 1.060 0.049 0.030 0.083 0.050 11.8 7.46 16.7 6.97 2.72 3.90 1.57 2.31
 

NAU
 0.056 0.073 0.043 0.098 0.016 0.007 0.026 0.030 1.1 0.85 1.5 0.61 0.29 0.37 0.20 0.26 

All Lab Report K2 Page 1 / 6 
Round Robin XLIV Laboratory Results 

All Results in μg/mL 

Lab 

Total β-Carotene trans-β-Carotene Total cis-β-Carotene 

247 248 249 250 

Total α-Carotene 

FSV-BA 0.346 0.191 0.446 0.604 

FSV-BB 0.355 0.203 0.478 0.605 

FSV-BBa 0.297 0.159 0.392 0.517 

FSV-BD 0.313 0.158 0.424 0.561 

FSV-BE 0.384 0.208 0.500 0.690 

FSV-BF 0.344 0.173 0.423 0.605 

FSV-BG 0.347 0.165 0.451 0.594 

FSV-BH 0.354 0.176 0.467 0.606 

FSV-BI 0.301 0.163 0.409 0.554 

FSV-BJ 0.317 0.162 0.411 0.588 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.326 0.181 0.462 0.544 

FSV-BO 0.317 0.198 0.406 0.542 

FSV-BP 0.179 0.101 0.250 0.366 

FSV-BQ 

FSV-BR 

FSV-BS 0.305 0.186 0.429 0.528 

FSV-BT 0.266 0.169 0.336 0.456 

FSV-BU 0.355 0.186 0.445 0.578 

FSV-BV 0.330 0.190 0.361 0.568 

FSV-BW 0.388 0.203 0.495 0.653 

FSV-BX >0.322 >0.158 >0.372 >0.538 

FSV-BZ >0.247 >0.132 >0.312 >0.432 

FSV-CB 0.206 0.113 0.268 0.400 

FSV-CC 

FSV-CD 0.278 0.171 0.377 0.506 

FSV-CE 0.430 0.206 0.629 0.799 

FSV-CF 

FSV-CH 0.295 0.180 0.355 0.543 

FSV-CI 

FSV-CL 0.291 0.155 0.398 0.533 

FSV-CM 

FSV-CP 0.394 0.210 0.495 0.677 

FSV-CR 

FSV-CS 0.356 0.181 0.402 0.537 

FSV-CU >0.265 >0.141 >0.373 >0.433 

FSV-CX >0.300 >0.150 >0.360 >0.490 

FSV-DA 0.245 0.117 0.414 0.599 

FSV-DB 0.305 0.170 0.382 0.544 

FSV-DF 

FSV-DJ 

FSV-DK 0.196 0.113 0.228 0.399 

FSV-DP 

FSV-DR 0.290 0.235 0.410 1.080 

FSV-DU 0.210 0.110 0.280 0.560 

FSV-DW 0.355 0.185 0.441 0.671 

FSV-ES >0.304 >0.166 >0.357 >0.493 

FSV-FG 

FSV-FH 

247 248 249 250 

0.324 0.175 0.419 0.571 

0.331 0.188 0.447 0.567 

0.279 0.149 0.367 0.487 

0.280 0.150 0.370 0.490 

0.296 0.163 0.413 0.504 

0.251 0.159 0.312 0.425 

0.322 0.158 0.372 0.538 

0.247 0.132 0.312 0.432 

0.320 0.163 0.359 0.487 

0.265 0.141 0.373 0.433 

0.300 0.150 0.360 0.490 

0.210 0.100 0.373 0.532 

0.324 0.170 0.399 0.614 

0.304 0.166 0.357 0.493 

247 248 249 250 

0.022 0.016 0.027 0.033 

0.024 0.015 0.031 0.038 

0.019 0.010 0.025 0.030 

0.024 0.010 0.035 0.041 

0.030 0.018 0.044 0.040 

0.015 0.010 0.024 0.031 

0.010 nd 0.020 0.030 

0.036 0.018 0.043 0.050 

0.035 0.017 0.042 0.067 

0.031 0.015 0.040 0.056 

247 248 249 250 

0.053 0.019 0.095 0.024 

0.047 0.010 0.083 0.013 

0.068 0.015 0.121 0.019 

0.054 0.016 0.100 0.019 

0.064 0.013 0.114 0.017 

0.050 0.016 0.090 0.014 

0.067 0.017 0.117 0.016 

0.048 0.014 0.091 0.012 

0.076 0.030 0.139 0.021 

0.053 0.014 0.077 0.021 

0.084 0.049 0.131 0.052 

0.047 0.018 0.079 0.015 

0.070 0.021 0.112 0.024 

0.070 0.020 0.110 0.016 

0.063 0.019 0.105 0.013 

0.052 0.018 0.080 0.029 

0.054 0.038 0.070 0.041 

0.040 0.010 0.069 0.013 

0.040 0.015 0.072 0.015 

0.039 0.013 0.072 0.015 

0.069 0.016 0.013 0.019 

0.054 0.014 0.093 0.015 

0.070 0.017 0.108 0.016 

0.050 0.010 0.080 0.020 

0.039 0.022 0.086 0.022 

0.032 0.007 0.049 0.013 

>0.046 >0.014 >0.086 >0.017 

>0.053 >0.027 >0.078 >0.025 

N 31 31 31 31 14 14 14 14 10 9 10 10 26 26 26 26 

Min 0.179 0.101 0.228 0.366 0.210 0.100 0.312 0.425 0.010 0.010 0.020 0.030 0.032 0.007 0.013 0.012 

Median 0.317 0.176 0.411 0.561 0.298 0.158 0.371 0.491 0.024 0.015 0.033 0.039 0.053 0.016 0.091 0.017 

Max 0.430 0.235 0.629 1.080 0.331 0.188 0.447 0.614 0.036 0.018 0.044 0.067 0.084 0.049 0.139 0.052 

eSD 0.055 0.022 0.052 0.064 0.037 0.013 0.019 0.065 0.010 0.004 0.013 0.013 0.018 0.004 0.027 0.005 

eCV 17 13 13 11 12 8 5 13 40 30 39 33 33 28 29 31 

Npast 0 0 0 33 0 0 0 10 0 0 0 8 0 0 0 21 

Medianpast 0.589 0.550 0.042 0.018 

SDpast 0.085 0.072 0.030 0.008 

NISTa 0.358 0.179 0.444 >0.475 0.348 0.170 0.431 0.475 0.010 0.009 0.013 nq 0.074 0.022 0.113 nd 

NISTb 0.327 >0.158 0.452 0.566 0.299 0.158 0.404 0.519 0.028 nq 0.048 0.047 >0.054 >0.017 0.111 0.029 

NNIST 5 5 22 3 5 22 22 6 5 5 22 3 2 4 22 3 

Mean 0.343 0.168 0.448 0.521 0.324 0.164 0.418 0.497 0.019 0.009 0.030 0.047 0.064 0.019 0.111 0.029 

Srep 0.010 0.004 0.012 0.007 0.009 0.005 0.013 0.013 0.009 0.005 0.014 0.009 0.003 0.002 0.004 0.005 

Shet 0.022 0.004 0.019 0.008 0.015 0.004 0.014 0.011 0.008 0.004 0.012 0.004 0.003 0.002 0.007 0.002 

Sanl 0.022 0.006 0.035 0.008 0.019 0.031 0.013 0.025 0.000 

SNIST 0.033 0.006 0.023 0.011 0.039 0.010 0.027 0.035 0.018 0.006 0.031 0.010 0.005 0.003 0.008 0.005 

NAV 0.330 0.172 0.429 0.541 0.311 0.161 0.394 0.494 0.022 0.012 0.032 0.043 0.059 0.018 0.101 0.023 

NAU 0.051 0.030 0.065 0.083 0.043 0.019 0.052 0.052 0.018 0.008 0.031 0.014 0.017 0.006 0.029 0.011 

All Lab Report K3 Page 2 / 6 
247 248 249 250 

0.357 0.315 0.42 0.59 

0.271 0.207 0.34 0.48 

0.407 0.364 0.46 0.72 

0.415 0.351 0.46 0.71 

0.372 0.323 0.43 0.63 

0.286 0.239 0.33 0.50 

0.285 0.246 0.32 0.47 

0.334 0.306 0.40 0.55 

0.564 0.507 0.62 0.97 

0.367 0.291 0.39 0.57 

0.396 0.340 0.49 0.65 

0.266 0.289 0.31 0.45 

0.374 0.314 0.43 0.67 

0.390 0.362 0.42 0.66 

0.373 0.330 0.42 0.59 

0.075 0.066 0.08 0.13 

0.397 0.359 0.46 0.62 

0.600 0.615 0.74 1.11 

0.376 0.330 0.46 0.65 

0.212 0.186 0.23 0.39 

0.369 0.304 0.37 0.52 

0.270 0.207 0.39 0.71 

0.361 0.328 0.39 0.65 

0.222 0.196 0.25 0.47 

0.272 0.224 0.31 0.50 

247 248 249 250 

0.195 0.167 0.215 0.364 

0.157 0.139 0.182 0.305 

0.223 0.184 0.244 0.417 

0.176 0.163 0.207 0.326 

0.135 0.124 0.172 0.292 

0.219 0.236 0.249 0.379 

0.177 0.150 0.173 0.338 

0.160 0.080 0.180 0.400 

0.350 0.290 0.380 0.560 

0.137 0.108 0.228 0.387 

0.141 0.126 0.155 0.319 

0.181 0.155 0.199 0.340 

247 248 249 250 

0.076 0.094 0.045 0.063 

0.070 0.089 0.048 0.064 

0.055 0.072 0.033 0.049 

0.046 0.062 0.021 0.040 

0.053 0.072 0.028 0.045 

0.059 0.078 0.032 0.048 

0.079 0.097 0.047 0.063 

0.062 0.084 0.030 0.052 

0.063 0.086 0.029 0.048 

0.061 0.082 0.037 0.051 

0.050 0.076 0.032 0.047 

0.066 0.085 0.042 0.073 

0.047 0.066 0.028 0.041 

0.070 0.083 0.044 0.058 

0.060 0.075 0.035 0.059 

0.031 0.047 0.014 0.024 

0.045 0.061 0.026 0.042 

0.050 0.054 0.024 0.033 

0.054 0.072 0.028 0.043 

0.054 0.073 0.035 0.057 

0.068 0.089 0.035 0.057 

0.058 0.074 0.031 0.044 

0.070 0.080 0.050 0.070 

0.049 0.043 0.051 0.063 

0.051 0.081 0.025 0.046 

0.059 0.081 0.032 0.059 

0.058 0.080 0.033 0.051 

247 248 249 250 

0.016 0.019 0.014 0.019 

0.018 0.023 0.020 0.024 

0.027 0.029 0.027 0.034 

0.019 0.020 0.018 0.029 

0.015 0.017 0.040 0.083 

0.018 0.006 0.016 0.019 

6 

42 

0 

K4

Round Robin XLIV Laboratory Results 

All Results in μg/mL 

Lab 

FSV-BA 

FSV-BB 

FSV-BBa 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 

FSV-BI 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 

FSV-BO 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BS 

FSV-BT 

FSV-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-BZ 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CI 

FSV-CL 

FSV-CM 

FSV-CP 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DF 

FSV-DJ 

FSV-DK 

FSV-DP 

FSV-DR 

FSV-DU 

FSV-DW 

FSV-ES 

FSV-FG 

FSV-FH 

N 

Min 

Median 

Max 

eSD 

eCV 

Npast 

Medianpast 

SDpast 

NISTa 

NISTb 

NNIST 

Mean 

Srep 

Shet 

Sanl 

SNIST 

NAV 

NAU 

trans-α-Carotene 

247 248 249 250 

nq nq nq nq 

0.046 0.014 0.086 0.017 

0.053 0.027 0.078 0.025 

2 2 2 2 

0.046 0.014 0.078 0.017 

0.049 0.020 0.082 0.021 

0.053 0.027 0.086 0.025 

0 0 0 0 

0.054 0.017 0.098 0.017 

3 17 17 3 

0.054 0.017 0.098 0.017 

0.004 0.002 0.004 0.002 

0.001 0.002 0.004 0.002 

0.005 0.002 0.005 0.002 

Total Lycopene trans-Lycopene Total β-Cryptoxanthin 

25 25 25 25 

0.075 0.066 0.08 0.13 

0.367 0.314 0.40 0.59 

0.600 0.615 0.74 1.11 

0.059 0.067 0.09 0.13 

16 21 23 21 

0 0 0 24 

0.57 

0.14 

0.400 0.342 0.48 0.68 

3 17 17 3 

0.400 0.342 0.48 0.68 

0.012 0.028 0.02 0.01 

0.006 0.014 0.02 0.00 

0.014 0.032 0.03 0.01 

0.384 0.328 0.44 0.63 

0.091 0.078 0.11 0.14 

12 12 12 12 

0.135 0.080 0.155 0.292 

0.177 0.152 0.203 0.352 

0.350 0.290 0.380 0.560 

0.041 0.040 0.040 0.050 

23 27 20 14 

0 0 0 9 

0.409 

0.107 

0.188 0.158 0.213 0.336 

3 17 17 3 

0.188 0.158 0.213 0.336 

0.002 0.007 0.005 0.015 

0.015 0.005 0.005 0.008 

0.015 0.008 0.007 0.017 

0.182 0.155 0.208 0.344 

0.037 0.034 0.042 0.073 

27 27 27 27 

0.031 0.043 0.014 0.024 

0.058 0.078 0.032 0.051 

0.079 0.097 0.051 0.073 

0.012 0.009 0.006 0.012 

20 11 19 23 

0 0 0 18 

0.065 

0.018 

0.049 0.067 0.029 0.032 

0.057 0.079 0.035 0.050 

5 22 22 6 

0.053 0.073 0.032 0.041 

0.003 0.004 0.002 0.001 

0.003 0.004 0.003 0.002 

0.006 0.009 0.004 0.013 

0.007 0.010 0.006 0.013 

0.056 0.075 0.032 0.046 

0.015 0.020 0.009 0.015 

Total α-Cryptoxanthin 

6 6 6 

0.015 0.006 0.014 0.019 

0.018 0.020 0.019 0.027 

0.027 0.029 0.040 0.083 

0.002 0.004 0.006 0.011 

12 23 31 

0 0 0 

All Lab Report Page 3 / 6 
Round Robin XLIV Laboratory Results 

All Results in μg/mL 

Total Lutein Total Zeaxanthin Total Lutein&Zeaxanthin 

Lab 247 248 249 250 

FSV-BA
 

FSV-BB
 0.111 0.085 0.137 0.124 

FSV-BBa 0.102 0.077 0.156 0.118 

FSV-BD 0.072 0.055 0.086 0.083 

FSV-BE 

FSV-BF 

FSV-BG 0.071 0.074 0.102 0.104 

FSV-BH 0.050 0.037 0.063 0.051 

FSV-BI 0.062 0.049 0.076 0.066 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM
 

FSV-BN
 0.078 0.060 0.087 0.075 

FSV-BO 0.111 0.094 0.135 0.118 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BS 0.063 0.065 0.085 0.092 

FSV-BT 0.100 0.088 0.085 0.093 

FSV-BU 

FSV-BV 

FSV-BW 

FSV-BX 0.006 0.041 0.072 0.062 

FSV-BZ 0.073 0.070 0.080 0.072 

FSV-CB 0.050 0.071 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CI 

FSV-CL
 

FSV-CM
 

FSV-CP
 

FSV-CR
 

FSV-CS
 

FSV-CU
 

FSV-CX
 0.060 0.040 0.070 0.070 

FSV-DA 0.071 0.051 0.091 0.070 

FSV-DB 

FSV-DF 

FSV-DJ 

FSV-DK 

FSV-DP 

FSV-DR 

FSV-DU 

FSV-DW 0.049 0.036 0.061 0.061 

FSV-ES 0.063 0.051 0.075 0.069 

FSV-FG 

FSV-FH 

247 248 249 250 

0.032 0.036 0.029 0.044 

0.028 0.032 0.010 0.040 

0.026 0.032 0.031 0.036 

0.024 0.018 0.022 0.025 

0.022 0.025 0.017 0.026 

0.025 0.025 0.020 0.028 

0.055 0.052 0.058 0.066 

0.044 0.047 0.034 0.048 

0.022 0.031 0.020 0.033 

0.038 0.040 0.030 0.029 

0.024 0.022 0.022 0.027 

0.030 0.033 

0.040 0.050 0.050 0.070 

0.035 0.040 0.037 0.048 

0.025 0.028 0.024 0.040 

0.024 0.034 0.021 0.027 

247 248 249 250 

0.175 0.167 0.179 0.182 

0.143 0.121 0.166 0.168 

0.130 0.109 0.166 0.158 

0.098 0.087 0.117 0.119 

0.096 0.086 0.109 0.093 

0.110 0.105 0.140 0.146 

0.072 0.062 0.080 0.077 

0.081 0.074 0.080 0.082 

0.140 0.117 0.151 0.148 

0.155 0.142 0.169 0.166 

0.086 0.097 0.105 0.125 

0.138 0.127 0.114 0.122 

0.160 0.124 0.159 0.169 

0.090 0.089 0.095 0.098 

0.030 0.063 0.094 0.089 

0.119 0.122 

0.089 0.081 0.097 0.080 

0.096 0.094 0.099 0.096 

0.112 0.104 0.118 0.130 

0.106 0.095 0.102 0.096 

0.106 0.091 0.128 0.118 

0.095 0.095 0.095 0.097 

0.074 0.064 0.085 0.101 

0.087 0.085 0.096 0.096 

N 16 17 16 17 15 16 15 16 24 23 24 23 

Min 0.006 0.036 0.061 0.051 0.022 0.018 0.010 0.025 0.030 0.062 0.080 0.077 

Median 0.071 0.055 0.085 0.072 0.026 0.032 0.024 0.035 0.102 0.095 0.112 0.118 

Max 0.111 0.094 0.156 0.124 0.055 0.052 0.058 0.070 0.175 0.167 0.179 0.182 

eSD 0.015 0.022 0.017 0.016 0.005 0.010 0.008 0.011 0.024 0.021 0.025 0.037 

eCV 21 40 20 23 21 32 35 32 24 22 22 31 

Npast 0 0 0 13 0 0 0 8 0 0 0 14 

Medianpast 0.087 0.034 0.116 

SDpast 0.026 0.011 0.027 

NISTa 0.077 0.059 0.090 0.084 0.020 0.020 0.013 0.041 0.097 0.079 0.102 0.125 

NISTb 0.071 0.063 0.101 0.091 0.039 0.044 0.040 0.053 0.111 0.108 0.141 0.145 

NNIST 5 22 22 6 5 22 22 6 5 22 22 6 

Mean 0.074 0.061 0.095 0.088 0.030 0.032 0.026 0.047 0.104 0.093 0.122 0.135 

Srep 0.002 0.003 0.003 0.001 0.002 0.002 0.002 0.001 0.003 0.004 0.005 0.002 

Shet 0.002 0.004 0.003 0.002 0.001 0.003 0.002 0.001 0.002 0.005 0.004 0.003 

Sanl 0.004 0.003 0.008 0.005 0.013 0.017 0.019 0.009 0.009 0.020 0.027 0.014 

SNIST 0.005 0.006 0.009 0.006 0.013 0.018 0.019 0.009 0.010 0.021 0.028 0.014 

NAV 0.073 0.058 0.090 0.080 0.028 0.032 0.025 0.041 0.103 0.094 0.117 0.126 

NAU 0.016 0.019 0.020 0.021 0.014 0.018 0.020 0.015 0.032 0.021 0.036 0.040 

All Lab Report K5 Page 4 / 6 
 

 

 

 

 

Round Robin XLIV Laboratory Results
 

Analytes Reported By One Laboratory
 

Values in μg/mL 

Term 

N 

Min 

Median 

Max 

eSD 

eCV 

Npast 

Medianpast 

SDpast 

NNIST 

Mean 

Srep
 

Shet
 

Sanl
 

SNIST
 

NAV 

NAU 

nd 

nq 

<x 

>x 

italics

Analyte Code 247 248 249 250 

Coenzyme Q10 FSV-CH 0.577 0.075 0.615 0.553 

Phytoene FSV-CL 0.074 0.066 0.088 0.084 

Phytofluene FSV-CL 0.074 0.047 0.066 0.071 

Total cis-β-Cryptoxanthin FSV-BT 0.019 0.024 0.016 0.029 

trans-anhydro-Lutein FSV-BT 0.040 0.035 0.045 0.046 

Legend 

Definition

 Number of (non-NIST) quantitative values reported for this analyte

 Minimum (non-NIST) quantitative value reported 

 Median (non-NIST) quantitative value reported

 Maximum (non-NIST) quantitative value reported

 Adjusted median absolute deviation from the median of the non-NIST results

 Coefficient of Variation for (non-NIST) results: 100*SD/Median

 Mean of N(s) from past RR(s)

 Mean of Median(s) from past RR(s)
 

 Pooled SD from past RR(s)

 Number of vials analyzed in duplicate by NIST analyst(s)

 Mean of the NIST-analyzed vial means

 W ithin-vial pooled standard deviation

 Among-vial pooled standard deviation

 Between NIST analyst standard deviation

2

)

0.5 Total standard deviation for NIST analyses: (Srep 2

 + Shet 2 + Sanl 

 NIST Assigned Value

 = (Median + Mean)/2 for analytes reported by NIST analyst(s)
 

= Median for analytes reported by ≥ 10 labs but not NIST

2

)

0.5 NIST Assigned Uncertainty: (S2

 + Sbtw 

 S is the maximum of (0.05*NAV, SD, SNIST, eSD) and Sbtw is the standard

 deviation between Median and Mean. The expected long-term SD, eSD,

 is defined in: Duewer, et al. Anal Chem 1997;69(7):1406-1413.

 Not detected (i.e., no detectable peak for analyte)

 Detected but not quantitatively determined

 Concentration below the limit of quantification, x

 Concentration greater than x 

 Not explicitly reported but calculated by NIST from reported values

All Lab Report 

K6

Page 5 / 6 
 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Lab 

FSV-BA 

FSV-BB 

FSV-BBa 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 

FSV-BI 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 

FSV-BO 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BS 

FSV-BT 

FSV-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-BZ 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CI 

FSV-CL 

FSV-CM 

FSV-CP 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DF 

FSV-DJ 

FSV-DK 

FSV-DP 

FSV-DR 

FSV-DU 

FSV-DW 

FSV-ES 

FSV-FG 

FSV-FH 

NISTa 

NISTb 

n 

% 1 

% 2 

% 3 

% 4 

Round Robin XLIV Laboratory Results 

Comparability Summary 

R aT gT bC tbC aC TLy TbX Label Definition 

1 1 2 1 2 1 2 1 Lab laboratory number 

1 1 2 2 2 1 1 1 R "Standard Score" for Retinol 

1 1 1 1 2 2 aT "Standard Score" for α-Tocopherol 

1 1 1 1 1 1 gT "Standard Score" for γ-Tocopherol 

1 2 1 2 bC "Standard Score" for Total β-Carotene 

2 1 1 1 1 2 tbC "Standard Score" for trans-β-Carotene 

1 1 1 1 2 1 2 aC "Standard Score" for Total α-Carotene 

1 1 1 1 1 1 Ly "Standard Score" for Total Lycopene 

1 1 2 1 1 1 2 bX "Standard Score" for β-Cryptoxanthin 

2 2 1 1 1 1 n number of laboratories providing data for this analyte 

1 1 3 

4 4 "Standard Score" 

Given that our knowledge of the shape, location, and width of the measurement
 

1 1 2 1 1 1 2 1
 

1 1 

distributions is approximate and that a limited number of labs are involved, we
 

2 4 1
 summarize comparability with the following four-level "Standard Score" (StS)...
 

2 2 3
 

2 2 1 2 1
 StS Definition
 

2 2 4
 1 All StV within ±t (1-0.683,n-1) { ±1 SD}
 

2 1 3 1 1
 2 All StV within ±t (1-0.954,n-1) { ±2 SD}
 

2 3 2 2 2 2 2
 3 All StV within ±t (1-0.997,n-1) { ±3 SD}
 

1 2 2 1 2 4 2
 4 At least one StV > ±t (1-0.997,n-1) { >3 SD}
 

4 1 2 2 1 1 2
 

1 2 1 2 1 1 1
 where:
 

1 1 1 1 4 1 1
 StV Standardized Value, the distance in standard deviation units your 

3 3 2 2 3 1 value is from the "true" concentration: StV = (your value - NAV) / NAU 

1 1 3 1 2 2 

2 1 NAV NIST Assigned Value, our estimate of the "true" analyte concentration 

1 2 1 1 

2 2 3 NAU NIST Assigned Uncertainty, our estimate of the total measurement
 

1 2
 standard deviation (serum heterogeniety, analytical repeatibility,
 

1 2 2 2
 and among-laboratory reproducibility)
 

2 2 2 1 1
 

2 4 3 1 2
 t (1-α,n-1) Two-tailed Student's t for coverage of ±1, ±2, and ±3 NAU about 

2 1 1 NAV, assuming a normal population of size n 

1 1 2 1 1 1
 

2 1 2 2 3
 

1 2 2 1 1
 

2 3 2 1 1 2
 

1 1 1
 

1 1 1 2 3 1 1
 

2 1 1
 

1 1 1 1
 

1
 

3 4 4 3
 

1
 

4 4 4
 

1 2 3
 

2 2 2 3 2 1
 

1 2 1
 

1 1 2 1
 

1
 

1 1 1 1 1 1 1
 

1 1 1 1 1 1 1 1
 

47 47 24 32 15 27 25 28 

TR aT g/bT bC tbC aC TLy TbX Expected 

55 47 46 50 47 56 56 61 68.2 % These are the observed and normal-population-expected proportions 

34 34 38 28 33 30 32 32 27.3 % of each Standard Score (StS), based upon each laboratory's largest
 

2 6 8 16 13 7 4 4
 4.3 % StV for the four sera.
 

6 11 4 3 0 4 8 0
 0.3 % 

All Lab Report K7 Page 6 / 6 
 

 

Appendix L. Representative “Individualized Report” for RR44 

Each participant in RR44 received an “Individualized Report” reflecting their reported 

results. Each report included a detailed analysis of the results they reported for the 

following analytes: 

• Retinol 

• α-Tocopherol 

• γ-Tocopherol 

• Total β-Carotene 

• trans-β-Carotene 

• Total α-Carotene 

• Total Lycopene 

• trans-Lycopene 

• Total β-Cryptoxanthin 

• Total Lutein 

• Total Zeaxanthin 

The following nine pages are the “Individualized Report” for the analytes evaluated by 

participant FSV-BA. 

Note 

The design file and program used to generate the original RR44 “Individualized 

Reports” are no longer available. The following pages were produced using the 

2013 version of the program (a linear descendant of that used in 1998) and a 

re-created design file. 

L1
 

 Set 1 of 52 

Individualized Round Robin XLIV Report: FSV-BA 

Summary 

Serum 247 Serum 248 Serum 249 Serum 

Analyte You NAV n You NAV n You NAV n You N

Retinol 0.664 0.669 46 0.849 0.843 46 0.488 0.483 46 1.120 1

Retinyl Palmitate 0.081 0.049 14 0.061 0.030 13 0.107 0.083 15 0.075 0

α-Tocopherol 10.92 11.77 46 7.3 7.5 46 15.5 16.7 46 6.92 6

γ-Tocopherol 2.42 2.72 23 3.65 3.90 23 1.48 1.57 23 2.34 2

Total β-Carotene 0.346 0.330 31 0.191 0.172 31 0.446 0.429 31 0.604 0

trans-β-Carotene 0.324 0.311 14 0.175 0.161 14 0.419 0.394 14 0.571 0

Total cis-β-Carotene 0.022 0.022 10 0.016 0.012 9 0.027 0.032 10 0.033 0

Total α-Carotene 0.053 0.059 26 0.019 0.018 26 0.095 0.101 26 0.024 0

trans-Lycopene 0.195 0.182 12 0.167 0.155 12 0.215 0.208 12 0.364 0

Total β-Cryptoxanthin 0.076 0.056 27 0.094 0.075 27 0.045 0.032 27 0.063 0

Total Lutein&Zeaxanthin 0.175 0.103 24 0.167 0.094 23 0.179 0.117 24 0.182 0

L2

You : Your reported values for the listed analytes (micrograms/milliliter)
 

NAV : NIST Assigned Values, here equal to this RR's median
 

n : Number of non-NIST laboratories reporting quantitative values for this analyte in this serum 

Please check our records against your records. Send corrections and/or updates to... 

Micronutrients Measurement Quality Assurance Program 

National Institute of Standards and Technology Tel: (301) 

100 Bureau Drive Stop 8392 Fax: (301) 

Gaithersburg, MD 20899-8392 USA Email: david.duewer@

Individualized Report 
 

 Set 1 of 52 

Individualized RR XLIV Report: FSV-BA 

Retinol, μg/mL 

[Analyte], μg/mL

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

Apparent Precision, SD 

248247249

192199218250 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#248 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 1 

#247 Lyophilized, multi-donor, a 1:1 blend of the #248 and #249 pools. New 

#249 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 2 

RR30:#192, RR32:#199, #250 Lyophilized, single-donor, augmented with retinol and retinyl palmitate RR36:#218 

Individualized Report Page 2 / 9 

L3
 

 Set 1 of 52 

Individualized RR XLIV Report: FSV-BA 

α-Tocopherol, μg/mL 

[Analyte], μg/mL

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

Apparent Precision, SD 

248247249

192199218250 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#248 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 1 

#247 Lyophilized, multi-donor, a 1:1 blend of the #248 and #249 pools. New 

#249 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 2 

RR30:#192, RR32:#199, #250 Lyophilized, single-donor, augmented with retinol and retinyl palmitate RR36:#218 

Individualized Report Page 3 / 9 

L4
 

 Set 1 of 52 

Individualized RR XLIV Report: FSV-BA 

γ-Tocopherol, μg/mL 

[Analyte], μg/mL

Your [Analyte], μg/mL 

Apparent Precision, SD

248247249

192199218250

Median [Analyte], μg/mL Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#248 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 1 

#247 Lyophilized, multi-donor, a 1:1 blend of the #248 and #249 pools. New 

#249 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 2 

RR30:#192, RR32:#199, #250 Lyophilized, single-donor, augmented with retinol and retinyl palmitate RR36:#218 

Individualized Report Page 4 / 9 

L5
 

 Set 1 of 52 

Individualized RR XLIV Report: FSV-BA 

Total β-Carotene, μg/mL 

[Analyte], μg/mL

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

Apparent Precision, SD 

248247249

192199218250 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR

You, ≥x, past RRs Others, this RR Apparent Precision, SD 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#248 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 1 

#247 Lyophilized, multi-donor, a 1:1 blend of the #248 and #249 pools. New 

#249 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 2 

RR30:#192, RR32:#199, #250 Lyophilized, single-donor, augmented with retinol and retinyl palmitate RR36:#218 

Individualized Report Page 5 / 9 

L6
 

 Set 1 of 52 

Individualized RR XLIV Report: FSV-BA 

trans-β-Carotene, μg/mL 

[Analyte], μg/mL

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

Apparent Precision, SD 

248247249

192199218250 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#248 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 1 

#247 Lyophilized, multi-donor, a 1:1 blend of the #248 and #249 pools. New 

#249 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 2 

RR30:#192, RR32:#199, #250 Lyophilized, single-donor, augmented with retinol and retinyl palmitate RR36:#218 

Individualized Report Page 6 / 9 

L7
 

 Set 1 of 52 

Individualized RR XLIV Report: FSV-BA 

Total α-Carotene, μg/mL 

[Analyte], μg/mL

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

Apparent Precision, SD 

248247249

192199218250 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#248 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 1 

#247 Lyophilized, multi-donor, a 1:1 blend of the #248 and #249 pools. New 

#249 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 2 

RR30:#192, RR32:#199, #250 Lyophilized, single-donor, augmented with retinol and retinyl palmitate RR36:#218 

Individualized Report Page 7 / 9 

L8
 

 Set 1 of 52 

Individualized RR XLIV Report: FSV-BA 

Total β-Cryptoxanthin, μg/mL 

[Analyte], μg/mL

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

Apparent Precision, SD

248247249

192199218250 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#248 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 1 

#247 Lyophilized, multi-donor, a 1:1 blend of the #248 and #249 pools. New 

#249 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 2 

RR30:#192, RR32:#199, #250 Lyophilized, single-donor, augmented with retinol and retinyl palmitate RR36:#218 

Individualized Report Page 8 / 9 

L9
 

 Set 1 of 52 

Individualized RR XLIV Report: FSV-BA 

trans-Lycopene, μg/mL 

[Analyte], μg/mL

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

Apparent Precision, SD 

248247249

192199218250 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) You, this RR 

You, past RRs 

Expectation 

You, ≥x, this RR

You, ≥x, past RRs Others, this RR 

For the construction and interpretation of these plots, see the Final Report for 

"Round Robin" XL, August 1997 

Serum Comments History 

#248 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 1 

#247 Lyophilized, multi-donor, a 1:1 blend of the #248 and #249 pools. New 

#249 Lyophilized, multi-donor, augmented with retinol, α- and γ-tocopherol New: SRM 968c Lv 2 

RR30:#192, RR32:#199, #250 Lyophilized, single-donor, augmented with retinol and retinyl palmitate RR36:#218 

Individualized Report Page 9 / 9 

L10
Appendix M. Shipping Package Inserts for RR11 

The following three items were included in each package shipped to each RR11 

participant: 

• Cover letter 

• Preparation of Stock Solution and Diluted Solution Datasheet 

• Results Datasheet 

The cover letter and datasheet were enclosed in a sealed waterproof bag along with the 

samples themselves. 

M1
 

 

September 10, 1998 

Dr. Margolis printed a separate cover letter for «Name» each participant. The words within the “«»” 

«Company» are parameters for a mail-merge macro 

«Address» routine. 

Dear «Name»: 

Thank you for agreeing to measure the ascorbic acid in the accompanying samples. Enclosed are 

two sets of samples, one set consisting of four ampules referred to as Test Samples (candidate 

SRM 970) and the second set consisting of a vial of solid ascorbic acid is the Control Sample. 

The Control sample consists of a sample of solid ascorbic acid in an amber vial and should be 

used in the following manner (please record your weights on the attached report form): 

1. Prepare 250 mL of 5% metaphosphoric acid (MPA) in distilled water. 

2. Weigh out 180-220 mg of the solid ascorbic acid sample to 0.1 mg (if possible) and 

dissolve it in 100mLof5% MPA using a 100 mL volumetric flask. Weigh the amount 

of MPA solution that was added. This will be referred to as the Stock Solution. 

3. Dilute the Stock Solution by weighing 0.5 mL of the stock solution into a 100 mL 

volumetric flask. Then add 5% MPA solution to 100 mL and weigh the amount of 

MPA solution that was added. 

4. Record the ultraviolet spectrum of the diluted solution against 5% MPA solution as 

the blank using paired cuvettes. 

5. Record the absorbance of the sample at 243 and 244 nm . 

6 Measure the concentration of the ascorbic acid in the dilute solution in duplicate 

along with the ampuled Test Samples. 

The Test Samples are in sealed ampules and were prepared by adding equal volumes of spiked 

human serum to 10% metaphosphoric acid. We have checked them for stability and homogeneity 

and the ascorbic acid appears to be sufficiently stable. 

Each ampule should contain between 20 and 120 μmol of ascorbic acid/L of diluted serum and 

each ampule should be analyzed in duplicate by the method(s) used in your laboratory 

(preferably one measuring total ascorbic acid). 

The Test Samples should be defrosted by warming at 20 °C for not more than 10 min otherwise 

some oxidation of ascorbic acid may occur. 

M2
 

 

 

A report form is attached and we would appreciate it if you would make your measurements and 

return the report to me by October 20, 1998. We also request that you send us a representative 

chromatogram from each lot and indicate whether you used the peak height or the peak area for 

calculating the concentration of ascorbic acid in your samples. Your results will be kept 

confidential. We will use these results in a study to demonstrate the comparative accuracy and 

the precision of the laboratories currently measuring ascorbic acid. However values will not be 

assigned to individual laboratories. If you wish to FAX your results to me, the Fax number is 

(301) 977- 0685. If you have any questions I can be reached at (301) 975-3137. Please let us 

know if the samples arrive defrosted and we will send you a duplicate set. 

Thank you for your assistance. 

Sincerely, 

Sam A. Margolis, Ph.D. 

Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

Attachment 

M3
 

 

 

 

 

 

 

 

 

 

 

REPORT OF ANALYSIS
 

NAME: 

ADDRESS: 

Telephone no.: 

Fax no.: 

Method of Analysis: 

Please attach representative chromatograms.
 

Method used for calculating ascorbic acid concentration.
 

Peak height Peak area
 

Manufacturer of ascorbic acid used to make in-house standards
 

Date of Analysis:
 

PREPARATION OF STOCK SOLUTION AND DILUTED SOLUTIONS 

STOCK SOLUTION 

Weight of ascorbic acid in the Stock Solution 

Weight of 5% MPA added to the 100 mL volumetric flask

mg 

g 

DILUTE SOLUTION 

Weight of added stock solution (0.5 mL)

Weight of 5% MPA added to the 100 mL volumetric flask

 mg 

g 

Absorbance of Dilute Solution 1 at 243 nm 

Absorbance of Dilute Solution 1 at 244 nm 

M4
 

 

 

 

CONTROL SAMPLE 1 

REPLICATE 1

REPLICATE 2

TEST SAMPLE HIGH VIAL # 

REPORT OF ANALYSIS
 

RESULTS (μmol/L)
 

 μmol/L 

 μmol/L 

REPLICATE 1 μmol/L
 

REPLICATE 2 μmol/L
 

TEST SAMPLE HIGH VIAL # 

REPLICATE 1 μmol/L 

REPLICATE 2 μmol/L 

TEST SAMPLE LOW VIAL # 

REPLICATE 1 μmol/L 

REPLICATE 2 μmol/L 

TEST SAMPLE LOW VIAL # 

REPLICATE 1 μmol/L 

REPLICATE 2 μmol/L 

M5