NISTIR 7880-24 

NIST Micronutrients Measurement 

Quality Assurance Program 

Winter and Summer 2000 

Comparability Studies 

Results for Round Robins XLVII and XLVIII 

Fat-Soluble Vitamins and Carotenoids in Human Serum 

and Round Robin 13 Ascorbic Acid in Human Serum 

David L. Duewer 

Margaret C. Kline 

Sam A. Margolis (Retired) 

Katherine E. Sharpless 

Jeanice B. Thomas 

 

 

 

 

NISTIR 7880-24 

NIST Micronutrients Measurement 

Quality Assurance Program 

Winter and Summer 2000 

Comparability Studies 

Results for Round Robins XLVII and XLVIII 

Fat-Soluble Vitamins and Carotenoids in Human Serum 

and Round Robin 13 Ascorbic Acid in Human Serum 

David L. Duewer 

Sam A. Margolis (Retired) 

Katherine E. Sharpless 

Jeanice B. Thomas 

Chemical Sciences Division 

Material 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) 

ii
 
 

 

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 and Summer 2000 MMQAP measurement comparability improvement studies: 1) Round 

Robin XLVII Fat-Soluble Vitamins and Carotenoids in Human Serum, 2) Round Robin XLVIII FatSoluble Vitamins and Carotenoids in Human Serum and 3) Round Robin 13 Total Ascorbic Acid in 

Human Serum. The materials for Round Robin XLVII were shipped to participants in February 

2000; participants were requested to provide their measurement results by May 12, 2000. The 

materials for Round Robin XLIII and Round Robin 13 were shipped to participants in June 2000; 

participants were requested to provide their measurement results by September 15, 2000. 

Keywords 

Human Serum
 

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

Total Ascorbic Acid
 

iii 
 

 

 

 

 

 

 

 

 

 

 

Table of Contents 

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

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

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

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

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

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

Round Robin 13: Vitamin C in Human Serum............................................................................... 2
 

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

Appendix A. Shipping Package Inserts for RR47........................................................................ A1
 

Appendix B. Final Report for RR47 ..............................................................................................B1
 

Appendix C. “All-Lab Report” for RR47 ......................................................................................C1
 

Appendix D. Representative “Individualized Report” for RR47 ............................................... D1
 

Appendix E. Shipping Package Inserts for RR48 ......................................................................... E1
 

Appendix F. Final Report for RR48............................................................................................... F1
 

Appendix G. “All-Lab Report” for RR48..................................................................................... G1
 

Appendix H. Representative “Individualized Report” for RR48............................................... H1
 

Appendix I. Shipping Package Inserts for RR13 ........................................................................... I1
 

Appendix J. Final Report for RR13 ................................................................................................ J1
 

Appendix K. “All-Lab Report” for RR13..................................................................................... K1
 

Appendix L. Representative “Individualized Report” for RR13 ................................................ L1
 

iv 
 

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 XLVII: Fat-Soluble Vitamins and Carotenoids in Human Serum 

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

XLVII comparability study (hereafter referred to as RR47) received three lyophilized and two 

liquid-frozen 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 2000. 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 RR47 consists of three documents: 

•	 A cover letter for the current study, a brief description of the other two documents, 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. 

1
 
 

 

 

 

•	 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 XLVIII: Fat-Soluble Vitamins and Carotenoids in Human Serum 

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

XLVIII comparability study (hereafter referred to as RR48) received three lyophilized and two 

liquid-frozen 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 June 2000. 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 RR48 consists of three documents: 

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

discussion of our analysis of the 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 13: Vitamin C in Human Serum 

Participants in the MMQAP Vitamin C in Human Serum Round Robin 13 comparability study 

(hereafter referred to as RR13) received four frozen serum test samples and a solid ascorbic acid 

control material 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 

2000. The communication materials included in the sample shipment are provided in Appendix I. 

The test and control serum materials were prepared by adding equal volumes of 10 % 

metaphosphoric acid (MPA) to human serum that had been spiked with ascorbic acid. While these 

samples contain some dehydroascorbic acid, its content is variable. Therefore, the participants 

report only total ascorbic acid (TAA, ascorbic acid plus dehydroascorbic acid). Participants are also 

2
 
 

encouraged to prepare calibration solutions from the supplied solid control to enable calibrating their 

serum measurements to the same reference standard. 

The final report delivered to every participant in RR13 consists of three documents: 

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

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

reproduced as Appendix J. 

•	 The “All-Lab Report” that summarizes all of the reported measurement results and provides 

several consensus statistics. This report is reproduced as Appendix K. 

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

including 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 L. 

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. 

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. 

3
 
 

Appendix A. Shipping Package Inserts for RR47 

The following two items were included in each package shipped to an RR47 participant: 

• Cover letter 

• Datasheet 

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

samples themselves. 

A1
A2
 

 

 

Participant #: ________ Date: _____________ 

Round Robin XLVII 

NIST Micronutrients Measurement Quality Assurance Program 

Analyte 259 260 261 262 263 Units* 

total retinol 

trans-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 

total β-cryptoxanthin 

total α-cryptoxanthin 

total lutein 

total zeaxanthin 

total lutein&zeaxanthin 

ubiquinone-10 (Q10) 

phylloquinone (K1) 

25-hydroxyvitamin D 

Other analytes? 

* We prefer μg/mL 

Were sera 259 & 260 frozen when received? Yes | No 

Mail: M2QAP 

NIST, Stop 8392 Please return results on-or-before Fax: 301-977-0685 

Gaithersburg, MD 20899-8392 12-May-2000 Email: David.Duewer@NIST.gov 

A3
 

 

Appendix B. Final Report for RR47 

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 content of the “Individualized” 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 

B1
June 16, 2000 

Dear Colleague: 

UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899-

Enclosed is the summary report of the results for Round Robin XL VII (RR 47). 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 and 

inter laboratory accuracy and precision; and a summary of the NIST assigned value (NA V) vs. your 

laboratory value for the analytes you measured. As in previous reports, the NIST assigned values 

are derived from the equally weighted means of the medians from this interlaboratory comparison 

exercise and the means from the analyses performed by NIST. 

Data for evaluating laboratory performance in RR 47 are provided in the comparability summary 

(Score Card) on page 6 of the "All Lab Report." Laboratory comparability is summarized as 

follows: results rated 1 to 3 are within 1 to 3 standard deviation(s) of the assigned value, 

respectively; those rated 4 are >3 standard deviations from the assigned value. 

If you have concerns regarding your laboratory's performance, we suggest that you obtain and 

analyze a unit of SRM 968c, Fat-Soluble Vitamins, Carotenoids, and Cholesterol in Human Serum. 

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

consultation. 

The following are newly released or forthcoming publications. Reprints will be provided upon 

request. 

"NIST Micronutrients Measurement Quality Assurance Program: Characterizing Individual 

Participant Measurement Performance Over Time," Duewer et al., Anal. Chem. 1999, 71, 1870-

1878. http://dx.doi.org/10. l 02 l/ac991481 b 

"Liquid Chromatographic Methods for the Determination of Vitamins in Food-Matrix Standard 

Reference Materials," Sharpless et al., J. Chromatogr. A, 2000, 881(1-2), 171-181. 

www .elsevier.nl/oasis 

"Analysis of Anthocyanins in Foods by Liquid Chromatography, Liquid Chromatography Mass 

Spectrometry and Capillary Electrophoresis," da Costa et al., J. Chromatogr. A, 2000, 881(1-2), 

403-41 O.www.elsevier.nl/oasis 

"NIST Micronutrients Measurement Quality Assurance Program: Characterizing the Measurement 

Community's Performance Over Time," Duewer et al., Anal. Chem., in press. 

"Preparation and Value Assignment of Standard Reference Material 968c: Fat-Soluble Vitamins, 

Carotenoids, and Cholesterol in Human Serum, Brown Thomas et al., submitted to Clin. Chim. 

Acta. 

As you are aware, the participation fees for the QA program will increase in 2001. The participation 

fees for the fat-soluble vitamins and carotenoids in serum studies (two exercises per year) will be 

$1600 for U.S. laboratories and $2000 for laboratories outside of the U.S. The fees for the vitamin C 

in serum study (one exercise per year) will be $800 for U.S. laboratories and $1000 for non-U.S. 

laboratories. Please complete and return the Intent-to-Participate form no later than August 4, 2000. 

B2

NISI 
Invoicing for the 2001 program will take place after shipment of the first set of samples which will 

be in January 2001. 

If you have any questions regarding this report, please contact David Duewer at 301/975-3935; email: david.duewer@nist.gov, or me at 301/975-3120; e-mail: jbthomas@nist.gov; fax: 301 /977-

0685. 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

cc: L. C. Sander 

Enclosures 

B3
 

1 

The NIST M2QAP Round Robin XLVII (RR47) report includes the usual 

Page “Individualized” Report
 

Your values, the number of labs reporting values, and our assigned values.
 

2+
 “Four Plot” summaries of your current and past measurement performance, one page for 

each analyte you report that is also reported by at least 10 other participants. 

Page “All Lab” Report 

1-5 A listing of all results and statistics for analytes reported by at least two laboratories 

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

A legend for the above two lists
 

7 The “Comparability Summary” (or “Score Card”) 

We have modified the definition of the “Comparability Summary” scores. Previously, the scores 

reflected your “worst” value for the given measurand. The scores are now calculated from the 

concordance and apparent precision characteristic of all your values for the measurand, as displayed in
 

the “target” plots in your Individualized Report and defined in Anal Chem 1999; 71:1074-9. We have 

also included, on an experimental basis, a graphical version of the “Comparability Summary” that
 

displays the full target plots for 14 measurands all on one page. If you like it – or hate it – please let us 

know. 

Samples. Five sera were distributed in RR47: two pairs of newly prepared {liquid frozen, lyophilized}
 

sera and a redistribution of SRM 968c Level I. The {liquid frozen, lyophilized} pairs were designed to 

enable investigation of potential measurement differences between “fresh” and lyophilized sera. SRM
 

968c Level I was distributed as a known reference for the matrix studies and to further assess measurand
 

stability in the SRM.
 

Sera {#259, #261} are {liquid frozen, lyophilized} material prepared from a freshly drawn male-donor
 

native serum pool. These samples were prepared and aliquoted into vials as a single batch.
 

Sera {#260, #262} are {liquid frozen, lyophilized} material prepared from a freshly drawn female-donor
 

native serum pool. These samples were prepared and aliquoted into vials as a single batch. 

Serum #263 is Level I of SRM 968c, previously distributed as #249 (RR44, 10/98) and #258 

(RR46,10/99). This material is a blended serum that was augmented with retinol and γ-tocopherol, and 

contains native carotenoid levels.
 

Qualitative Results. 

1)	 A number of participants “reconstituted” the liquid frozen samples with 1 mL water. All such results 

have been mathematically corrected (2x measured). We will be distributing some liquid frozen 

samples in the next several Round Robins. 

2)	 A number of participants did not receive their samples in frozen form. We have instituted a more 

aggressive sample delivery and storage tracking program to help resolve these issues. We ask that 

you examine carefully all future RR samples upon delivery and quickly provide us with the 

information requested in the shipment’s manifest. 

Quantitative Results 

1)	 With the possible exception of total lutien, total zeaxanthin, and total lutein&zeaxanthin, there have 

been no changes in median level or measurement variability in SRM 968c Level 1. We believe that 

the small changes in the lutein and zeaxanthin measurands may be more a reflection of measurement 

systems changes rather than a result of SRM degradation. We will continue to monitor this material 

and will revise the SRM 968c Certificate if/when necessary. 

B4
2) Since the lyophilized materials are reconstituted with 1.0 mL water rather than TO a total volume of 

1.0 mL, we expect that the measurand concentrations in the lyophilized member of each {liquid 

frozen, lyophilized} pair will be about 0.95x that of the liquid frozen. In general, this is true for the 

retinol and tocopherol measurands. It appears less true for the carotenoids. We will be exploring 

this issue in greater detail in future round robins. 

B5
 

 

Appendix C. “All-Lab Report” for RR47 

The following seven 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 XLVII Laboratory Results 

All Results are in μg/mL 

Lab 259 

Total Retinol 

260 261 262 

trans-Retinol Retinyl Palmitate 

263 

α-Tocopherol

FSV-BA 0.598 0.705 0.560 0.646 0.878 

FSV-BB 0.520 0.615 0.505 0.608 0.865 

FSV-BD 0.585 0.690 0.564 0.643 0.880 

FSV-BE 0.710 0.760 0.620 0.710 0.920 

FSV-BF 0.545 0.640 0.555 0.625 0.865 

FSV-BG 0.615 0.718 0.547 0.655 0.872 

FSV-BH 0.546 0.649 0.509 0.604 0.774 

FSV-BI 0.603 0.726 0.565 0.684 0.881 

FSV-BJ 0.579 0.668 0.556 0.629 0.866 

FSV-BK 0.548 0.649 0.529 0.627 0.845 

FSV-BL 0.659 0.716 0.602 0.659 0.802 

FSV-BM 0.594 0.736 0.603 0.717 0.901 

FSV-BN 0.514 0.598 0.534 0.636 0.856 

FSV-BO >0.521 >0.593 >0.518 >0.536 >0.722 

FSV-BP 0.564 0.664 0.549 0.643 0.817 

FSV-BQ 0.609 0.711 0.558 0.657 0.873 

FSV-BR >0.600 >0.700 >0.510 >0.650 >0.840 

FSV-BU 0.581 0.691 0.520 0.629 0.833 

FSV-BV 0.480 0.560 0.440 0.517 0.720 

FSV-BW 0.530 0.660 0.510 0.580 0.790 

FSV-BX >0.599 >0.699 >0.568 >0.641 >0.857 

FSV-BZ
 

FSV-CB
 0.521 0.603 0.526 0.593 0.866 

FSV-CC 0.550 0.670 0.590 0.670 0.910 

FSV-CD >0.567 >0.624 >0.500 >0.598 >0.786 

FSV-CE 0.540 0.630 0.520 0.610 0.840 

FSV-CF 0.602 0.710 0.568 0.673 0.877 

FSV-CG 0.623 0.761 0.744 0.853 1.232 

FSV-CH 0.483 0.567 0.468 0.538 0.706 

FSV-CI 0.670 0.760 0.760 0.730 1.000 

FSV-CL 0.579 0.769 0.594 0.646 0.857 

FSV-CN 0.586 0.705 0.566 0.658 0.886 

FSV-CR 0.650 0.370 0.700 0.730 0.900 

FSV-CS >0.577 >0.695 >0.529 >0.646 >0.886 

FSV-CU >0.613 >0.695 >0.541 >0.608 >0.782 

FSV-CV 0.529 0.487 0.585 0.564 0.961 

FSV-CW >0.473 >0.543 >0.459 >0.597 >1.019 

FSV-CX >0.643 >0.769 >0.600 >0.715 >0.921 

FSV-DA >0.619 >0.745 >0.563 >0.667 >0.855 

FSV-DB 0.490 0.580 0.486 0.616 0.842 

FSV-DF 0.505 0.625 0.485 0.564 0.768 

FSV-DI >0.582 >0.690 >0.547 >0.643 >0.841 

FSV-DK 0.533 0.627 0.506 0.593 0.803 

FSV-DP >0.609 >0.723 >0.586 >0.683 >0.853 

FSV-DQ 

FSV-DR 0.615 0.687 0.548 0.636 0.822 

FSV-DU 0.770 0.750 0.560 0.690 0.930 

FSV-EM 0.520 0.570 0.490 0.640 0.790 

FSV-EQ 0.698 0.810 0.647 0.757 0.989 

FSV-ES >0.626 >0.742 >0.522 >0.677 >0.870 

FSV-FH 0.668 0.799 0.655 0.769 1.051 

FSV-FT 0.740 0.890 0.730 0.870 1.350 

FSV-FW 0.558 0.705 0.582 0.604 0.797 

259 260 261 262 263 

0.521 0.593 0.518 0.536 0.722 

0.600 0.700 0.510 0.650 0.840 

0.599 0.699 0.568 0.641 0.857 

0.550 0.660 0.540 0.630 0.820 

0.567 0.624 0.500 0.598 0.786 

0.577 0.695 0.529 0.646 0.886 

0.613 0.695 0.541 0.608 0.782 

0.473 0.543 0.459 0.597 1.019 

0.643 0.769 0.600 0.715 0.921 

0.619 0.745 0.563 0.667 0.855 

0.582 0.690 0.547 0.643 0.841 

0.609 0.723 0.586 0.683 0.853 

0.626 0.742 0.522 0.677 0.870 

259 260 261 262 263 

0.111 0.101 0.097 0.092 0.049 

0.105 0.100 0.099 0.091 0.030 

0.127 0.147 0.125 0.132 0.072 

0.117 0.115 0.126 0.105 0.043 

0.157 0.151 0.143 0.138 0.042 

0.140 0.148 0.121 0.135 0.034 

0.109 0.092 0.089 0.102 0.039 

0.154 0.150 0.160 0.150 0.041 

0.091 0.090 0.083 0.090 0.048 

0.130 0.070 0.160 0.130 0.060 

0.127 0.132 0.124 0.115 0.074 

0.122 0.139 0.127 0.123 0.022 

0.102 0.114 0.100 0.115 0.026 

0.181 0.145 0.163 0.108 0.039 

0.118 0.110 0.095 0.092 0.027 

0.065 0.062 0.067 0.045 0.023 

259 260 261 262 263 

12.1 19.3 10.9 17.4 7.42 

12.0 19.2 11.5 18.3 7.89 

12.5 18.5 10.8 16.9 8.10 

13.3 20.0 11.8 18.5 7.50 

11.9 19.0 11.6 18.2 7.75 

13.0 20.8 11.4 18.8 7.44 

11.8 18.6 10.9 17.0 7.36 

12.0 18.4 11.2 17.8 7.64 

12.7 20.0 12.5 18.5 7.31 

11.9 18.5 11.1 17.6 7.60 

9.5 13.4 9.5 12.1 8.18 

12.2 19.8 11.5 17.6 7.80 

12.2 18.2 11.6 18.8 8.47 

9.8 15.2 9.0 13.9 6.37 

11.4 15.9 10.1 15.3 7.91 

13.0 20.4 11.7 18.4 8.15 

11.5 19.7 11.0 18.7 7.03 

12.3 20.2 11.0 17.7 6.83 

10.4 17.2 9.8 15.4 6.51 

12.8 20.4 12.2 18.8 8.00 

9.6 16.2 8.9 14.3 7.00 

11.7 18.0 11.4 17.7 7.74 

11.7 19.3 11.4 18.2 7.70 

10.9 16.0 9.1 14.3 6.21 

12.7 19.6 11.8 18.7 6.52 

12.8 19.8 11.9 18.9 8.10 

10.2 16.3 9.4 15.2 6.22 

10.7 16.3 10.0 14.9 6.36 

11.4 17.9 12.9 17.2 7.70 

14.4 26.7 14.9 22.4 9.24 

12.5 20.1 12.1 18.7 8.02 

12.3 9.3 12.5 19.8 7.30 

10.4 18.1 10.3 17.4 6.74 

11.1 18.1 9.9 16.0 6.91 

12.3 18.0 13.2 15.6 7.14 

11.9 18.2 12.3 19.7 6.75 

11.8 20.0 11.6 17.2 7.32 

11.0 17.5 10.9 17.6 8.23 

12.7 20.1 11.8 18.8 7.91 

11.2 18.4 10.7 16.2 6.13 

10.1 16.0 8.1 13.6 6.89 

12.0 19.2 11.0 18.3 6.89 

16.8 24.1 13.4 21.7 10.86 

10.0 16.6 10.7 18.0 7.37 

13.9 21.2 12.4 19.5 8.48 

12.6 19.3 10.6 17.8 7.90 

11.1 17.1 10.4 16.0 7.10 

10.9 17.6 11.0 15.3 8.29 

N 39 39 39 39 39 13 13 13 13 13 16 16 16 16 16 48 48 48 48 48 

Min 0.480 0.370 0.440 0.517 0.706 0.473 0.543 0.459 0.536 0.722 0.065 0.062 0.067 0.045 0.022 9.5 9.3 8.1 12.1 6.13 

Median 0.579 0.687 0.558 0.643 0.866 0.599 0.695 0.540 0.643 0.853 0.120 0.115 0.123 0.112 0.040 11.9 18.5 11.2 17.7 7.47 

Max 0.770 0.890 0.760 0.870 1.350 0.643 0.769 0.600 0.715 1.019 0.181 0.151 0.163 0.150 0.074 16.8 26.7 14.9 22.4 10.86 

eSD 0.065 0.085 0.056 0.052 0.065 0.032 0.052 0.034 0.050 0.049 0.019 0.036 0.036 0.029 0.014 1.1 1.9 1.0 1.5 0.80 

eCV 11 12 10 8 8 5 7 6 8 6 16 32 30 26 35 10 11 9 9 11 

Npast 0 0 0 0 47 0 0 0 0 7 0 0 0 0 14 0 0 0 0 48 

Medianpast 0.849 0.830 0.036 7.45 

SDpast 0.057 0.050 0.012 0.73 

NISTa >0.592 >0.703 >0.569 >0.677 0.877 0.592 0.703 0.569 0.677 0.848 11.4 19.3 11.5 18.3 7.44 

NISTb >0.596 >0.712 >0.526 >0.643 >0.799 0.596 0.712 0.526 0.643 0.799 12.6 19.4 11.6 19.3 7.74 

NNIST 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 

MeanNIST 0.594 0.708 0.547 0.660 0.838 0.594 0.708 0.547 0.660 0.824 12.0 19.4 11.5 18.8 7.59 

Srep 0.027 0.019 0.021 0.023 0.021 0.027 0.019 0.021 0.023 0.016 0.4 0.3 0.3 0.4 0.12 

Shet 0.021 0.024 0.030 0.006 0.004 0.021 0.024 0.030 0.006 0.005 0.5 0.4 0.3 0.5 0.10 

Sanl 0.003 0.007 0.030 0.024 0.055 0.003 0.007 0.030 0.024 0.034 0.9 0.1 0.0 0.7 0.22 

SNIST 0.035 0.032 0.048 0.034 0.059 0.035 0.032 0.048 0.034 0.038 1.0 0.5 0.4 0.9 0.27 

NAV 0.587 0.699 0.553 0.651 0.852 0.597 0.701 0.544 0.651 0.838 0.118 0.114 0.121 0.108 0.041 11.9 19.0 11.3 18.3 7.57 

NAU 0.056 0.072 0.055 0.056 0.070 0.048 0.056 0.048 0.052 0.070 0.032 0.037 0.033 0.030 0.019 1.1 1.9 1.0 2.1 0.80 

All Lab R eport C2 P age 1 / 7 
 

 

Round Robin XLVII Laboratory Results 

All Results are in μg/mL 

Lab 

γ-Tocopherol

259 260 261 262 263 

δ-Tocopherol Total β-Carotene trans-β-Carotene

FSV-BA 2.35 1.14 2.12 1.01 3.80 

FSV-BB 1.99 0.94 1.93 0.90 3.57 

FSV-BD 

FSV-BE 2.70 1.20 2.40 1.10 4.00 

FSV-BF 2.15 0.99 2.10 0.94 3.95 

FSV-BG 2.34 1.04 2.02 1.00 3.63 

FSV-BH 2.34 1.12 2.16 1.02 4.00 

FSV-BI 2.21 1.06 2.02 1.04 3.79 

FSV-BJ 2.63 1.14 2.45 1.04 3.83 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 1.84 0.74 1.75 0.86 3.11 

FSV-BO 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BU 2.64 1.19 2.80 1.11 4.15 

FSV-BV 2.40 1.12 2.22 1.02 4.17 

FSV-BW 2.45 1.18 2.39 1.14 4.21 

FSV-BX 2.41 1.06 2.26 0.99 4.14 

FSV-BZ 1.90 0.80 2.20 0.90 3.90 

FSV-CB 

FSV-CC 

FSV-CD 2.24 1.17 1.90 1.08 3.23 

FSV-CE 

FSV-CF 

FSV-CG 2.43 1.29 2.29 1.21 3.88 

FSV-CH 1.90 0.90 1.82 0.82 3.05 

FSV-CI 2.70 1.90 3.10 1.80 4.30 

FSV-CL 2.54 1.68 2.62 1.41 4.52 

FSV-CN 2.28 1.09 2.21 1.01 4.16 

FSV-CR 

FSV-CS 2.02 1.02 1.93 0.97 3.62 

FSV-CU 

FSV-CV 2.52 1.27 2.62 0.91 3.20 

FSV-CW 2.46 1.14 2.48 1.22 4.02 

FSV-CX 

FSV-DA 2.41 1.23 2.34 1.11 4.04 

FSV-DB 

FSV-DF 

FSV-DI 2.20 1.01 2.04 0.93 3.80 

FSV-DK 2.11 0.92 1.91 0.79 3.17 

FSV-DP 

FSV-DQ 2.10 1.40 1.74 0.99 2.99 

FSV-DR 

FSV-DU 

FSV-EM 

FSV-EQ 

FSV-ES 

FSV-FH 

FSV-FT 

FSV-FW 

259 260 261 262 263 

0.380 0.362 0.389 0.377 0.348 

0.198 0.198 0.147 0.179 0.156 

0.080 0.040 0.110 0.070 0.120 

0.115 0.077 0.150 0.052 0.105 

0.112 0.070 0.102 0.063 0.141 

259 260 261 262 263 

0.231 0.306 0.213 0.289 0.182 

0.211 0.297 0.196 0.286 0.158 

0.266 0.356 0.247 0.347 0.193 

0.246 0.312 0.237 0.311 0.176 

0.267 0.334 0.238 0.305 0.177 

0.232 0.333 0.240 0.317 0.175 

0.252 0.316 0.223 0.308 0.168 

0.281 0.354 0.245 0.334 0.184 

0.265 0.315 0.228 0.334 0.208 

0.186 0.258 0.192 0.248 0.148 

0.233 0.328 0.241 0.329 0.193 

0.237 0.294 0.231 0.293 0.162 

0.228 0.297 0.196 0.276 0.160 

0.210 0.280 0.220 0.280 0.170 

>0.237 >0.324 >0.220 >0.274 >0.150 

>0.190 >0.327 >0.235 >0.290 >0.162 

0.241 0.284 0.231 0.296 0.189 

0.192 0.291 0.190 0.285 0.142 

0.270 0.350 0.250 0.340 0.120 

0.282 0.387 0.268 0.360 0.196 

0.261 0.334 0.256 0.311 0.174 

0.292 0.343 0.296 0.387 0.229 

>0.239 >0.321 >0.234 >0.302 >0.175 

0.215 0.317 0.217 0.310 0.177 

0.208 0.329 0.275 0.270 0.215 

0.216 0.286 0.216 0.298 0.144 

>0.202 >0.279 >0.206 >0.260 >0.150 

0.304 0.379 0.268 0.299 0.146 

0.180 0.261 0.194 0.281 0.164 

>0.262 >0.346 >0.216 >0.286 >0.167 

0.331 0.426 0.271 0.406 0.216 

0.132 0.190 0.095 0.182 0.110 

0.275 0.358 0.249 0.339 0.127 

>0.090 >0.160 >0.110 >0.170 >0.090 

0.320 0.410 0.280 0.410 0.210 

>0.267 >0.300 >0.256 >0.338 >0.186 

>0.254 >0.344 >0.200 >0.298 >0.174 

259 260 261 262 263 

0.212 0.284 0.195 0.267 0.164 

0.202 0.284 0.187 0.272 0.150 

0.222 0.319 0.228 0.303 0.167 

0.236 0.286 0.208 0.304 0.184 

0.171 0.237 0.179 0.238 0.137 

0.237 0.324 0.220 0.274 0.150 

0.190 0.327 0.235 0.290 0.162 

0.261 0.359 0.248 0.334 0.180 

0.239 0.321 0.234 0.302 0.175 

0.200 0.292 0.198 0.280 0.153 

0.202 0.267 0.200 0.279 0.132 

0.202 0.279 0.206 0.260 0.150 

0.265 0.350 0.241 0.256 0.122 

0.262 0.346 0.216 0.286 0.167 

0.090 0.160 0.110 0.170 0.090 

0.267 0.300 0.256 0.338 0.186 

0.254 0.344 0.200 0.298 0.174 

N 27 27 27 27 27 5 5 5 5 5 29 29 29 29 29 17 17 17 17 17 

Min 1.84 0.74 1.74 0.79 2.99 0.080 0.040 0.102 0.052 0.105 0.132 0.190 0.095 0.182 0.110 0.090 0.160 0.110 0.170 0.090 

Median 2.34 1.12 2.20 1.01 3.88 0.115 0.077 0.147 0.070 0.141 0.241 0.317 0.237 0.308 0.175 0.222 0.300 0.208 0.280 0.162 

Max 2.70 1.90 3.10 1.80 4.52 0.380 0.362 0.389 0.377 0.348 0.331 0.426 0.296 0.410 0.229 0.267 0.359 0.256 0.338 0.186 

eSD 0.27 0.15 0.30 0.13 0.39 0.052 0.055 0.055 0.027 0.031 0.043 0.039 0.030 0.039 0.027 0.033 0.035 0.030 0.029 0.018 

eCV 11 13 13 13 10 45 71 37 38 22 18 12 13 13 15 15 12 14 10 11 

Npast 0 0 0 0 26 0 0 0 0 8 0 0 0 0 33 0 0 0 0 15 

Medianpast 3.83 0.130 0.173 0.165 

SDpast 0.34 0.067 0.022 0.017 

NISTa 2.31 1.19 2.12 1.00 4.00 nq nq nq nq 0.138 0.211 0.336 0.265 0.353 0.172 

NISTb 2.36 1.21 2.13 1.10 4.05 0.142 nq 0.101 nq 0.143 0.217 0.278 0.230 0.322 0.159 0.204 0.257 0.192 0.271 0.134 

NNIST 5 5 5 5 5 2 2 5 5 5 5 5 5 2 2 2 2 2 

MeanNIST 2.34 1.20 2.13 1.05 4.03 0.146 0.101 0.140 0.217 0.307 0.248 0.338 0.165 0.204 0.257 0.192 0.271 0.134 

Srep 0.10 0.09 0.06 0.04 0.16 0.001 0.000 0.027 0.007 0.020 0.024 0.018 0.018 0.019 0.013 0.003 0.010 0.016 

Shet 0.09 0.06 0.13 0.07 0.11 0.020 0.016 0.035 0.015 0.006 0.013 0.010 0.009 0.022 0.012 0.016 0.013 0.004 

Sanl 0.04 0.02 0.00 0.07 0.03 0.003 0.007 0.041 0.025 0.022 0.010 

SNIST 0.14 0.11 0.14 0.10 0.19 0.020 0.016 0.044 0.018 0.046 0.037 0.031 0.022 0.029 0.018 0.017 0.016 0.016 

NAV 2.34 1.16 2.15 1.03 3.96 0.131 0.077 0.124 0.070 0.141 0.229 0.311 0.239 0.323 0.170 0.213 0.279 0.200 0.276 0.148 

NAU 0.24 0.14 0.32 0.12 0.38 0.068 0.055 0.044 0.027 0.044 0.043 0.046 0.039 0.049 0.028 0.041 0.044 0.029 0.031 0.027 

All Lab R eport C3 P age 2 / 7 
 

 

Round Robin XLVII Laboratory Results 

All Results are in μg/mL 

Lab 

Total cis-β-Carotene

259 260 261 262 263 

Total α-Carotene trans-α-Carotene Total Lycopene 

FSV-BA 0.018 0.022 0.017 0.022 0.017 

FSV-BB 0.009 0.013 0.009 0.014 0.008 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 0.010 0.014 0.012 0.015 0.008 

FSV-BI 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.029 0.029 0.020 0.030 0.024 

FSV-BO 0.015 0.020 0.013 0.010 0.011 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-BZ 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CG 0.021 0.028 0.020 0.026 0.016 

FSV-CH 

FSV-CI 

FSV-CL 

FSV-CN 

FSV-CR 

FSV-CS 0.015 0.025 0.019 0.030 0.024 

FSV-CU
 

FSV-CV
 

FSV-CW
 0.014 0.019 0.016 0.019 0.012 

FSV-CX 

FSV-DA 0.039 0.029 0.027 0.043 0.024 

FSV-DB 

FSV-DF 

FSV-DI 

FSV-DK 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-DU 

FSV-EM 

FSV-EQ 

FSV-ES 

FSV-FH 

FSV-FT 

FSV-FW 

259 260 261 262 263 

0.039 0.068 0.036 0.065 0.018 

0.032 0.062 0.033 0.063 0.011 

0.042 0.075 0.043 0.072 0.019 

0.046 0.069 0.038 0.060 0.031 

0.040 0.075 0.039 0.071 0.012 

0.039 0.072 0.039 0.067 0.016 

0.052 0.092 0.042 0.086 nq 

0.040 0.068 0.037 0.067 0.020 

0.053 0.082 0.049 0.088 0.028 

0.046 0.090 0.049 0.087 0.021 

0.042 0.070 0.042 0.065 0.017 

0.037 0.069 0.031 0.063 0.009 

0.038 0.068 0.038 0.068 0.014 

0.051 0.087 0.049 0.071 0.019 

0.040 0.086 0.057 0.089 0.020 

0.032 0.052 0.033 0.058 0.011 

0.045 0.091 0.048 0.087 0.016 

0.050 0.092 0.048 0.083 0.018 

0.039 0.064 0.038 0.053 0.013 

0.057 0.093 0.058 0.094 0.021 

0.050 0.080 0.049 0.076 0.027 

0.048 0.095 0.044 0.090 0.017 

0.039 0.069 0.048 0.058 nq 

>0.032 >0.056 >0.033 >0.058 >0.012 

0.036 0.071 0.038 0.066 0.014 

0.044 0.079 0.042 0.057 0.013 

0.045 0.074 0.042 0.074 0.019 

nq 0.048 0.022 0.042 0.018 

0.030 0.050 0.030 0.050 0.010 

0.046 0.070 0.043 0.080 0.015 

>0.047 >0.084 >0.037 >0.074 >0.017 

259 260 261 262 263 

0.032 0.056 0.033 0.058 0.012 

0.047 0.084 0.037 0.074 0.017 

259 260 261 262 263 

0.419 0.47 0.488 0.58 0.406 

0.422 0.43 0.425 0.43 0.384 

0.366 0.36 0.332 0.34 0.290 

0.375 0.41 0.385 0.40 0.325 

0.340 0.33 0.297 0.32 0.240 

0.450 0.44 0.408 0.43 0.354 

0.388 0.36 0.351 0.41 0.337 

0.357 0.38 0.370 0.38 0.298 

0.366 0.50 0.398 0.47 0.338 

0.406 0.40 0.380 0.37 0.280 

0.405 0.41 0.368 0.38 0.305 

0.330 0.35 0.340 0.34 0.270 

0.342 0.30 0.332 0.32 0.290 

0.344 0.38 0.309 0.39 0.269 

0.435 0.46 0.412 0.43 0.326 

0.363 0.37 0.364 0.34 0.273 

0.637 0.65 0.656 0.64 0.553 

0.444 0.46 0.441 0.42 0.359 

0.337 0.34 0.474 0.28 0.312 

0.402 0.42 0.405 0.42 0.309 

0.448 0.48 0.438 0.36 0.237 

0.381 0.42 0.416 0.41 0.353 

0.420 0.43 0.300 0.31 0.327 

0.340 0.35 0.310 0.37 0.260 

0.463 0.40 0.437 0.46 0.309 

0.390 0.40 0.310 0.39 0.302 

N 

Min 

Median 

Max 

eSD 

eCV 

9 

0.009 

0.015 

0.039 

0.008 

50 

9 

0.013 

0.022 

0.029 

0.009 

40 

9 

0.009 

0.017 

0.027 

0.004 

22 

9 

0.010 

0.022 

0.043 

0.012 

54 

9 

0.008 

0.016 

0.024 

0.011 

70 

28 

0.030 

0.042 

0.057 

0.006 

14 

29 

0.048 

0.072 

0.095 

0.011 

16 

29 

0.022 

0.042 

0.058 

0.009 

21 

29 

0.042 

0.068 

0.094 

0.015 

22 

27 

0.009 

0.017 

0.031 

0.004 

26 

2 2 2 2 2 

0.032 0.056 0.033 0.058 0.012 

0.039 0.070 0.035 0.066 0.015 

0.047 0.084 0.037 0.074 0.017 

0.011 0.021 0.003 0.012 0.004 

28 29 7 18 26 

26 26 26 26 26 

0.330 0.30 0.297 0.28 0.237 

0.389 0.41 0.383 0.39 0.309 

0.637 0.65 0.656 0.64 0.553 

0.048 0.06 0.069 0.06 0.043 

12 14 18 15 14 

Npast 

Medianpast 

SDpast 

0 0 0 0 9 

0.014 

0.004 

0 0 0 0 28 

0.016 

0.004 

0 0 0 0 0 0 0 0 0 27 

0.313 

0.061 

NISTa 

NISTb 

NNIST 

MeanNIST 

Srep 

Shet 

Sanl 

SNIST 

0.013 0.021 0.038 0.051 0.024 

nq 

0.038 

2 

0.039 

0.003 

0.004 

0.005 

>0.081 

0.064 

5 

0.072 

0.004 

0.004 

0.012 

0.013 

>0.042 

0.046 

5 

0.044 

0.008 

0.004 

0.003 

0.009 

>0.090 

0.070 

5 

0.080 

0.010 

0.009 

0.015 

0.020 

nq 

0.013 

2 

0.013 

0.000 

0.003 

0.003 

nq 0.081 0.042 0.090 nq 

0.029 0.048 0.033 0.054 0.012 

2 5 5 5 2 

0.031 0.065 0.037 0.073 0.011 

0.004 0.005 0.004 0.007 0.005 

0.008 0.009 0.002 0.008 0.002 

0.023 0.006 0.025 

0.009 0.025 0.007 0.027 0.005 

0.452 0.54 0.458 0.55 0.418 

2 2 2 2 2 

0.452 0.54 0.458 0.55 0.404 

0.032 0.08 0.054 0.05 0.030 

0.045 0.05 0.025 0.01 0.057 

0.055 0.09 0.059 0.05 0.065 

NAV 

NAU 

0.014 

0.008 

0.022 

0.009 

0.028 

0.004 

0.036 

0.012 

0.018 

0.009 

0.041 

0.014 

0.073 

0.022 

0.043 

0.013 

0.076 

0.022 

0.015 

0.007 

0.424 0.47 0.420 0.47 0.357 

0.094 0.13 0.099 0.14 0.097 

All Lab R eport C4 P age 3 / 7 
 

 

Round Robin XLVII Laboratory Results 

All Results are in μg/mL 

Lab 259 

trans-Lycopene 

260 261 262 263 

Total β-Cryptoxanthin Total α-Cryptoxanthin Total Lutein 

FSV-BA 0.239 0.292 0.219 0.271 0.228 

FSV-BB 0.177 0.236 0.169 0.216 0.161 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 0.183 0.205 0.168 0.185 0.159 

FSV-BH
 

FSV-BI
 

FSV-BJ
 

FSV-BK
 

FSV-BL 

FSV-BM 

FSV-BN 0.170 0.179 0.156 0.192 0.162 

FSV-BO 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BU 

FSV-BV 

FSV-BW 

FSV-BX 0.150 0.195 0.140 0.172 0.119 

FSV-BZ 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CG 0.195 0.250 0.185 0.229 0.166 

FSV-CH 

FSV-CI 

FSV-CL 

FSV-CN 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CV 

FSV-CW 0.162 0.195 0.161 0.203 0.139 

FSV-CX 0.160 0.214 0.158 0.193 0.144 

FSV-DA 0.210 0.270 0.196 0.191 0.123 

FSV-DB 

FSV-DF 

FSV-DI 0.214 0.228 0.179 0.192 0.152 

FSV-DK 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-DU 

FSV-EM 

FSV-EQ 

FSV-ES 0.236 0.305 0.186 0.263 0.205 

FSV-FH 

FSV-FT 

FSV-FW 

259 260 261 262 263 

0.099 0.087 0.092 0.083 0.107 

0.099 0.089 0.092 0.085 0.089 

0.080 0.069 0.083 0.065 0.077 

0.082 0.082 0.078 0.079 0.077 

0.139 0.115 0.138 0.111 0.105 

0.101 0.085 0.088 0.082 0.089 

0.089 0.078 0.083 0.073 0.082 

0.095 0.082 0.091 0.089 0.089 

0.067 0.059 0.063 0.050 0.061 

0.059 0.058 0.059 0.058 0.053 

0.071 0.056 0.066 0.055 0.063 

0.060 0.050 0.055 0.046 0.055 

0.066 0.060 0.059 0.048 0.051 

0.049 0.045 0.049 0.044 0.049 

0.144 0.137 0.137 0.135 0.125 

0.086 0.075 0.079 0.070 0.064 

0.083 0.079 0.085 0.070 0.082 

0.074 0.064 0.070 0.061 0.067 

0.081 0.073 0.073 0.065 0.046 

0.090 0.077 0.087 0.078 0.077 

0.085 0.079 0.082 0.073 0.081 

0.091 0.079 0.085 0.056 0.060 

0.078 0.075 0.088 0.073 0.075 

0.080 0.082 0.053 0.046 0.076 

0.070 0.070 0.070 0.060 0.070 

0.151 0.121 0.140 0.131 0.104 

0.085 0.079 0.074 0.071 0.074 

259 260 261 262 263 

0.036 0.046 0.042 0.035 0.024 

0.038 0.038 0.038 0.041 0.028 

0.035 0.038 0.034 0.032 0.022 

0.036 0.035 0.036 0.035 0.022 

0.032 0.032 0.034 0.027 0.018 

259 260 261 262 263 

0.107 0.205 0.094 0.197 0.053 

0.135 0.233 0.124 0.212 0.053 

0.082 0.163 0.078 0.151 0.038 

0.103 0.229 0.100 0.210 0.055 

0.129 0.200 0.121 0.179 0.059 

0.086 0.169 0.098 0.179 0.058 

0.136 0.245 0.114 0.219 0.049 

0.120 0.216 0.109 0.183 0.050 

0.073 0.089 0.073 0.090 0.061 

- - - - 0.045 

0.134 0.228 0.128 0.216 0.085 

>0.085 >0.156 >0.081 >0.169 >0.059 

0.075 0.173 0.069 0.159 0.038 

0.127 0.210 0.112 0.184 0.058 

0.096 0.194 0.091 0.181 0.050 

0.106 0.221 0.086 0.186 0.052 

0.139 0.266 0.106 0.242 0.057 

N 

Min 

Median 

Max 

eSD 

eCV 

11 11 11 11 11 

0.150 0.179 0.140 0.172 0.119 

0.183 0.228 0.169 0.193 0.159 

0.239 0.305 0.219 0.271 0.228 

0.034 0.048 0.019 0.015 0.022 

19 21 11 8 14 

27 27 27 27 27 

0.049 0.045 0.049 0.044 0.046 

0.083 0.078 0.082 0.070 0.076 

0.151 0.137 0.140 0.135 0.125 

0.018 0.012 0.015 0.018 0.019 

21 15 18 25 25 

5 5 5 5 5 

0.032 0.032 0.034 0.027 0.018 

0.036 0.038 0.036 0.035 0.022 

0.038 0.046 0.042 0.041 0.028 

0.001 0.004 0.003 0.004 0.002 

4 12 8 12 10 

15 

0.073 

0.107 

0.139 

0.032 

30 

15 

0.089 

0.210 

0.266 

0.028 

13 

15 

0.069 

0.100 

0.128 

0.020 

20 

15 

0.090 

0.184 

0.242 

0.037 

20 

16 

0.038 

0.053 

0.085 

0.007 

13 

Npast 

Medianpast 

SDpast 

0 0 0 0 13 

0.157 

0.031 

0 0 0 0 28 

0.074 

0.011 

0 0 0 0 6 

0.022 

0.007 

0 0 0 0 17 

0.056 

0.017 

NISTa 

NISTb 

NNIST 

MeanNIST 

Srep 

Shet 

Sanl 

SNIST 

0.054 0.094 0.074 0.078 0.070 

0.085 0.087 0.091 0.087 0.089 

5 5 5 5 5 

0.070 0.090 0.082 0.082 0.079 

0.009 0.012 0.009 0.004 0.003 

0.008 0.002 0.014 0.007 0.005 

0.021 0.005 0.012 0.007 0.013 

0.024 0.013 0.020 0.010 0.014 

0.056 0.055 0.052 0.056 0.039 

2 2 2 2 2 

0.057 0.055 0.052 0.056 0.039 

0.003 0.012 0.005 0.009 0.001 

0.005 0.014 0.010 0.002 0.001 

0.006 0.019 0.011 0.009 0.001 

0.101 

>0.089 

3 

0.101 

0.006 

0.004 

0.007 

0.251 

>0.179 

3 

0.251 

0.011 

0.012 

0.016 

0.114 

>0.083 

3 

0.114 

0.000 

0.006 

0.006 

0.248 

>0.169 

3 

0.252 

0.016 

0.014 

0.022 

0.055 

>0.047 

3 

0.055 

0.002 

0.001 

0.002 

NAV 

NAU 

0.183 0.228 0.169 0.193 0.159 

0.034 0.044 0.030 0.034 0.028 

0.077 0.084 0.082 0.076 0.078 

0.026 0.020 0.020 0.020 0.019 

0.047 0.046 0.044 0.045 0.030 

0.016 0.022 0.016 0.017 0.012 

0.104 

0.030 

0.231 

0.047 

0.107 

0.022 

0.218 

0.058 

0.054 

0.011 

All Lab R eport C5 P age 4 / 7 
 

 

Round Robin XLVII Laboratory Results 

All Results are in μg/mL 

Lab 

trans-Lutein 

259 260 261 262 263 

Total Zeaxanthin Total Lutein&Zeaxanthin Coenzyme Q10 

FSV-BA 

FSV-BB 

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-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-BZ 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CG 

FSV-CH 

FSV-CI 

FSV-CL 

FSV-CN 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CV 

FSV-CW 0.085 0.156 0.081 0.169 0.059 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DF 

FSV-DI 

FSV-DK 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-DU 

FSV-EM 

FSV-EQ 

FSV-ES 

FSV-FH 

FSV-FT 

FSV-FW 

259 260 261 262 263 

0.052 0.053 0.048 0.051 0.042 

0.037 0.052 0.028 0.048 0.011 

0.039 0.037 0.021 0.035 0.028 

0.031 0.049 0.031 0.045 0.036 

0.028 0.043 0.030 0.045 0.046 

0.026 0.037 0.021 0.037 0.021 

0.022 0.033 0.020 0.026 0.019 

- - - - 0.028 

0.027 0.045 0.025 0.042 0.022 

0.024 0.035 0.023 0.039 0.041 

0.022 0.043 0.023 0.038 0.023 

0.039 0.058 0.032 0.049 0.027 

0.018 0.028 0.011 0.022 0.026 

0.041 0.053 0.028 0.047 0.035 

259 

0.169 

0.159 

0.165 

0.184 

0.121 

0.134 

0.106 

0.162 

0.178 

0.150 

0.144 

0.142 

0.148 

0.197 

0.162 

0.149 

0.136 

0.175 

0.134 

>0.109 

0.097 

0.166 

0.118 

0.124 

0.090 

0.176 

0.180 

260 

0.290 

0.258 

0.266 

0.303 

0.200 

0.278 

0.199 

0.282 

0.364 

0.254 

0.255 

0.248 

0.266 

0.262 

0.273 

0.286 

0.223 

0.308 

0.239 

>0.191 

0.216 

0.268 

0.193 

0.249 

0.200 

0.312 

0.319 

261 

0.158 

0.142 

0.165 

0.161 

0.099 

0.131 

0.118 

0.134 

0.167 

0.144 

0.145 

0.129 

0.127 

0.155 

0.153 

0.150 

0.128 

0.145 

0.159 

>0.104 

0.092 

0.144 

0.119 

0.097 

0.090 

0.159 

0.134 

262 

0.27 

0.25 

0.26 

0.28 

0.19 

0.26 

0.21 

0.26 

0.34 

0.24 

0.24 

0.21 

0.24 

0.25 

0.26 

0.24 

0.21 

0.27 

0.24 

>0.208 

0.20 

0.23 

0.21 

0.21 

0.19 

0.33 

0.29 

263 

0.149 

0.095 

0.093 

0.067 

0.066 

0.091 

0.090 

0.070 

0.105 

0.086 

0.105 

0.069 

0.073 

0.126 

0.107 

0.093 

0.085 

0.097 

0.079 

>0.100 

0.061 

0.085 

0.104 

0.078 

0.040 

0.101 

0.092 

259 260 261 262 263 

0.614 0.826 0.571 0.610 0.464 

0.341 0.510 0.371 0.576 0.507 

0.560 0.800 0.550 0.740 0.520 

0.606 0.816 0.484 0.677 0.535 

N 1 1 1 1 1 13 13 13 13 14 26 26 26 26 26 4 4 4 4 4 

Min 0.018 0.028 0.011 0.022 0.011 0.090 0.193 0.090 0.19 0.040 0.341 0.510 0.371 0.576 0.464 

Median 0.085 0.156 0.081 0.169 0.059 0.028 0.043 0.025 0.042 0.027 0.150 0.264 0.143 0.24 0.091 0.583 0.808 0.517 0.644 0.514 

Max 0.052 0.058 0.048 0.051 0.046 0.197 0.364 0.167 0.34 0.149 0.614 0.826 0.571 0.740 0.535 

eSD 0.010 0.012 0.007 0.007 0.011 0.027 0.035 0.022 0.04 0.019 0.040 0.019 0.064 0.075 0.021 

eCV 34 28 27 18 39 18 13 16 18 21 7 2 12 12 4 

Npast 0 0 0 0 0 0 0 0 0 15 0 0 0 0 26 0 0 0 0 0 

Medianpast 0.034 0.095 

SDpast 0.008 0.017 

NISTa 0.025 0.030 0.021 0.029 0.026 0.126 0.281 0.136 0.28 0.081 

NISTb 0.089 0.179 0.083 0.169 0.047 0.029 0.036 0.027 0.035 0.033 >0.119 >0.215 >0.110 >0.204 >0.080 

NNIST 2 2 2 2 2 5 5 5 5 5 5 5 5 5 5 

MeanNIST 0.089 0.179 0.083 0.169 0.047 0.027 0.033 0.024 0.032 0.030 0.123 0.248 0.123 0.20 0.080
 

Srep 0.008 0.006 0.003 0.009 0.004 0.003 0.004 0.004 0.004 0.007 0.009 0.009 0.005 0.12 0.009
 

Shet 0.008 0.005 0.000 0.003 0.001 0.002 0.002 0.003 0.003 0.002 0.007 0.009 0.005 0.05 0.001
 

Sanl 0.004 0.004 0.004 0.005 0.005 0.006 0.047 0.018 0.01 0.002
 

SNIST 0.011 0.007 0.003 0.010 0.004 0.006 0.006 0.006 0.006 0.009 0.013 0.048 0.019 0.13 0.009 

NAV 0.027 0.038 0.025 0.037 0.029 0.139 0.257 0.133 0.22 0.086
 

NAU
 0.011 0.014 0.007 0.014 0.010 0.039 0.058 0.033 0.14 0.021 

All Lab R eport C6 P age 5 / 7 
 

 

 

 

 

Round Robin XLVII Laboratory Results
 

All Results are in μg/mL
 

Analytes Reported By One Laboratory 

Analyte Code 259 260 261 262 263 

trans-β-Cryptoxanthin NISTb 0.07 0.06 0.07 0.06 0.06 

25-hydroxyvitamin D FSV-BF 0.027 0.030 0.030 0.031 0.021 

25-hydroxyvitamin D2 FSV-BN 0.0134 0.0083 0.0059 0.0163 nd 

Phylloquinone (K1) x1000 FSV-DI 0.78 0.38 0.73 0.30 0.57 

Phytofluene FSV-CL 0.032 0.026 0.032 0.023 0.037 

Phytoene FSV-CL 0.120 0.140 0.133 0.130 0.075 

Term 

N 

Min 

Medianpart 

Max 

eSD 

eCV 

Npast 

Medianpast 

SDpast 

NNIST 

MeanNIST 

Srep 

Shet 

Sanl 

SNIST 

NAV 

NAU 

nq 

>x 

italics

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

 Robust estimate of standard deviation for (non-NIST) results

 Coefficient of Variation for (non-NIST) results: 100*eSD/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 total vials analyzed in duplicate by NIST analysts

 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

 = (Medianpart + MeanNIST)/2 for analytes reported by NIST analyst(s)

 = Medianpart 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 Medianpart and MeanNIST. The expected long-term SD, eSD,

 is defined in: Duewer, et al. Anal Chem 1997;69(7):1406-1413.

 Detected but not quantitatively determined

 Concentration larger than x

 Not explicitly reported but calculated by NIST from reported values

All Lab Report 

C7

Page 6 / 7 
 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Round Robin XLVII Laboratory Results
 

Comparability Summary
 

Lab 

FSV-BA 

FSV-BB 

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-BU 

FSV-BV 

FSV-BW
 

FSV-BX
 

FSV-BZ
 

FSV-CB
 

FSV-CC
 

FSV-CD
 

FSV-CE
 

FSV-CF
 

FSV-CG
 

FSV-CH
 

FSV-CI
 

FSV-CL
 

FSV-CN
 

TR aT gT bC tbC aC TLy TbX TLu TZ L&Z 

1 1 1 1 1 1 1 1 1 1 

1 1 2 1 1 1 1 1 1 1 1 

1 1 

2 1 1 1 1 

1 1 1 1 1 1 1 

1 1 1 1 1 1 1 2 

1 1 1 1 1 1 1 3 1 2 1 

1 1 1 1 1 1 1 1 1 2 

1 1 1 1 1 1 1 1 1 1 

1 1 2 

1 3 

1 1 1 

1 1 2 1 1 1 1 1 

2 2 2 2 1 1 1 1 

1 2 1 1 1 1 

1 1 

1 1 

1 1 2 1 1 1 1 2 1 2 

3 1 1 1 1 1 2 1 

1 2 1 1 1 1 2 

1 1 1 1 1 1 2 1 1 1 

2 2 1 1 1 1 1 1 

1 1 1 1 1 2 

1 1 

1 2 2 1 1 1 3 2 1 1 

1 1 2 

1 1 

4 2 1 2 2 1 1 1 2 

2 2 2 1 1 1 

3 1 4 1 

1 4 3 2 2 3 1 1 

1 1 1 1 1 1 1 1 1 1 1 

Label 

Lab 

TR 

aT

gT 

bC 

tbC 

aC 

TLy 

TbX 

TLu 

TZ 

L&Z 

n 

% 1 

% 2 

% 3 

% 4 

Definition 

Participant code 

Total Retinol 

α-Tocopherol 

γ/β-Tocopherol 

Total β-Carotene 

trans-β-Carotene 

Total α-Carotene 

Total Lycopene 

 Total β-Cryptoxanthin 

Total Lutein 

Total Zeaxanthin 

Total Lutein & Zeaxanthin 

number of participants providing quantitative data 

Percent of CS = 1 (within 1 SD of medians) 

Percent of CS = 2 (within 2 SD of medians) 

Percent of CS = 3 (within 3 SD of medians) 

Percent of CS = 4 (3 or more SD from medians) 

“Comparability Score” 

The Comparability Score (CS) summarizes your measurement 

performance for a given analyte relative to the consensus 

medians in this study. CS is the average distance (in units of 

standard deviation) of your measurement performance 

characteristics from the consensus performance. CS is 

calculated when the number of quantitative values you reported 

Nyou, is at least two and at least six participants reported 

quantitative values for the analyte. 

We define CS as follows: 





 MINIMUM 4,INTEGER 1 



 





 

2 2 CS = + + C AP 



 

i Median i

you You − N 

NAU i

Nyou 

C = Concordance = i 1 

∑ 

= 

you 



 



 ∑ 

= 

N Youi 

NAU 

Me

i 

− 

i 1 

i 

 





2

dian 

N 1 

FSV-CW 2 1 1 1 1 1 1 1 

FSV-CU 1 1 1 

FSV-CR 3 3 

AP = Apparent Precision = 

you −

FSV-CS 1 1 1 1 1 1 1 1 

FSV-CV 2 2 2 2 1 1 

FSV-CX 2 1 1 1 1 

FSV-DA 1 1 1 2 2 1 1 1 1 

FSV-DB 2 1 2 1 1 

FSV-DI 1 1 1 1 1 1 2 1 NAU = NIST Assigned Uncertainty 

FSV-DK 1 1 2 2 1 2 

FSV-DP 1 For further details, please see 

FSV-DF 2 

FSV-DQ
 

FSV-DR
 

FSV-DU
 

FSV-EM
 

FSV-EQ
 

FSV-ES
 

FSV-FH
 

FSV-FT
 

FSV-FW 

NISTa 

NISTb 

n 

% 1 

% 2 

% 3 

% 4 

2 2 3 2 1 1 

1 1 2 1 1 1 

2 4 4 4 

2 1 2 1 1 1 

2 2 1 2 1 1 3 1 

1 1 1 1 1 1 1 1 

3 1 

4 1 

1 1 1 1 

1 1 1 1 1 1 1 1 1 

1 1 1 1 1 1 1 1 1 1 1 

53 50 29 39 18 33 27 29 18 15 29 

TR aT g/bT bC tbC aC TLy TbX TLu TZ L&Z 

68 72 62 69 72 94 96 79 83 87 79 

21 20 31 26 22 6 0 10 17 13 21 

8 4 3 3 0 0 4 10 0 0 0 

4 4 3 3 6 0 0 0 0 0 0 

Duewer DL, Kline MC, Sharpless KE, Brown Thomas J, Gar 

KT. Micronutrients Measurement Quality Assurance 

Program: Helping participants use interlaboratory compariso 

exercise results to improve their long-term measurement 

performance. Anal Chem 1999;71(9):1870-8. 

All Lab Report C8 Page 7 / 7 
Appendix D. Representative “Individualized Report” for RR47 

Each participant in RR47 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 

• trans-Retinol 

• Retinyl Palmitate 

• α-Tocopherol 

• γ-Tocopherol 

• δ-Tocopherol 

• Total β-Carotene 

• trans-β-Carotene 

• Total cis-β-Carotene 

• Total α-Carotene 

• Total Lycopene 

• trans-Lycopene 

• Total β-Cryptoxanthin 

• Total α-Cryptoxanthin 

• Total Lutein 

• Total Zeaxanthin 

• Total Lutein & Zeaxanthin 

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

participant FSV-BA. 

D1
 

 Set 1 of 55

Individualized Round Robin XLVII Report: FSV-BA 

Summary 

Serum 259 Serum 260 Serum 261 Serum 262 

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

Total Retinol 0.598 0.587 39 0.705 0.699 39 0.560 0.553 39 0.646 0.651 

Retinyl Palmitate 0.11 0.12 16 0.1 0.1 16 0.1 0.1 16 0.09 0.11 

α-Tocopherol 12.06 11.93 48 19.35 18.96 48 10.92 11.35 48 17.35 18.25 

γ-Tocopherol 2.354 2.338 27 1.143 1.160 27 2.123 2.153 27 1.006 1.032 

Total β-Carotene 0.231 0.229 29 0.306 0.311 29 0.213 0.239 29 0.289 0.323 

trans-β-Carotene 0.212 0.213 17 0.284 0.279 17 0.195 0.200 17 0.267 0.276 

Total cis-β-Carotene 0.018 9 0.022 9 0.017 9 0.022 

Total α-Carotene 0.039 0.041 28 0.068 0.073 29 0.036 0.043 29 0.065 0.076 

trans-Lycopene 0.239 0.183 11 0.292 0.228 11 0.219 0.169 11 0.271 0.193 

Total β-Cryptoxanthin 0.099 0.077 27 0.087 0.084 27 0.092 0.082 27 0.083 0.076 

Total Lutein&Zeaxanthin 0.169 0.139 26 0.290 0.257 26 0.158 0.133 26 0.273 0.221 

D2

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

NAV : NIST Assigned Values, equal to (NIST's average-of-averages + this RR's median) / 2 

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 

100 Bureau Drive Stop 8392 

Gaithersburg, MD 20899-8392 USA Ema

 Individualized Report 
 

 

 Set 1 of 55

Individualized RR XLVII Report: FSV-BA 

Total Retinol 

259 261 260 262 248 258 263 

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see:
 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem May 1, 1999.
 

Serum History Comments 

#259 Fresh frozen 

#260 Fresh frozen 

#261 Lyophilized, same pool as #259 

#262 Lyophilized, same pool as #260 

#263 #248 in RR44 (9/98), #258 in RR46 (9/99) SRM 968c, Level I 

 Individualized Report Page 2 / 12 

D3
 

 

 Set 1 of 55

Individualized RR XLVII Report: FSV-BA 

Retinyl Palmitate 

259 261 260 262 248 258 263 

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see:
 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem May 1, 1999.
 

Serum History Comments 

#259 Fresh frozen 

#260 Fresh frozen 

#261 Lyophilized, same pool as #259 

#262 Lyophilized, same pool as #260 

#263 #248 in RR44 (9/98), #258 in RR46 (9/99) SRM 968c, Level I 

 Individualized Report Page 3 / 12 

D4
 

 

 Set 1 of 55

Individualized RR XLVII Report: FSV-BA 

α-Tocopherol 

259 261 260 262 248 258 263 

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see:
 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem May 1, 1999.
 

Serum History Comments 

#259 Fresh frozen 

#260 Fresh frozen 

#261 Lyophilized, same pool as #259 

#262 Lyophilized, same pool as #260 

#263 #248 in RR44 (9/98), #258 in RR46 (9/99) SRM 968c, Level I 

 Individualized Report Page 4 / 12 

D5
 

 

 Set 1 of 55

Individualized RR XLVII Report: FSV-BA 

γ-Tocopherol 

259 261 260 262 248 258 263 

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see:
 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem May 1, 1999.
 

Serum History Comments 

#259 Fresh frozen 

#260 Fresh frozen 

#261 Lyophilized, same pool as #259 

#262 Lyophilized, same pool as #260 

#263 #248 in RR44 (9/98), #258 in RR46 (9/99) SRM 968c, Level I 

 Individualized Report Page 5 / 12 

D6
 

 

 Set 1 of 55

Individualized RR XLVII Report: FSV-BA 

Total β-Carotene 

259 261 260 262 248 258 263 

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see:
 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem May 1, 1999.
 

Serum History Comments 

#259 Fresh frozen 

#260 Fresh frozen 

#261 Lyophilized, same pool as #259 

#262 Lyophilized, same pool as #260 

#263 #248 in RR44 (9/98), #258 in RR46 (9/99) SRM 968c, Level I 

 Individualized Report Page 6 / 12 

D7
 

 

 Set 1 of 55

Individualized RR XLVII Report: FSV-BA 

trans-β-Carotene 

259 261 260 262 248 258 263 

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see:
 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem May 1, 1999.
 

Serum History Comments 

#259 Fresh frozen 

#260 Fresh frozen 

#261 Lyophilized, same pool as #259 

#262 Lyophilized, same pool as #260 

#263 #248 in RR44 (9/98), #258 in RR46 (9/99) SRM 968c, Level I 

 Individualized Report Page 7 / 12 

D8
 

 

 Set 1 of 55

Individualized RR XLVII Report: FSV-BA 

Total α-Carotene 

259 261 260 262 248 258 263 

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see:
 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem May 1, 1999.
 

Serum History Comments 

#259 Fresh frozen 

#260 Fresh frozen 

#261 Lyophilized, same pool as #259 

#262 Lyophilized, same pool as #260 

#263 #248 in RR44 (9/98), #258 in RR46 (9/99) SRM 968c, Level I 

 Individualized Report Page 8 / 12 

D9
 

 

 Set 1 of 55

Individualized RR XLVII Report: FSV-BA 

trans-Lycopene 

259 261 260 262 248 258 263 

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see:
 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem May 1, 1999.
 

Serum History Comments 

#259 Fresh frozen 

#260 Fresh frozen 

#261 Lyophilized, same pool as #259 

#262 Lyophilized, same pool as #260 

#263 #248 in RR44 (9/98), #258 in RR46 (9/99) SRM 968c, Level I 

 Individualized Report Page 9 / 12 

D10
 

 

 Set 1 of 55

Individualized RR XLVII Report: FSV-BA 

Total β-Cryptoxanthin 

259 261 260 262 248 258 263 

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see:
 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem May 1, 1999.
 

Serum History Comments 

#259 Fresh frozen 

#260 Fresh frozen 

#261 Lyophilized, same pool as #259 

#262 Lyophilized, same pool as #260 

#263 #248 in RR44 (9/98), #258 in RR46 (9/99) SRM 968c, Level I 

 Individualized Report Page 10 / 12 

D11
 

 

 Set 1 of 55

Individualized RR XLVII Report: FSV-BA 

Total Lutein&Zeaxanthin 

259 261 260 262 248 258 263 

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see:
 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem May 1, 1999.
 

Serum History Comments 

#259 Fresh frozen 

#260 Fresh frozen 

#261 Lyophilized, same pool as #259 

#262 Lyophilized, same pool as #260 

#263 #248 in RR44 (9/98), #258 in RR46 (9/99) SRM 968c, Level I 

 Individualized Report Page 11 / 12 

D12
Set 1 of 55 

Individualized Round Robin XLVII Report: FSV-BA 

Graphical Comparability Summary 

Total Retinol α-Tocopherol Total α-Carotene 

D13

trans-Retinol γ-Tocopherol Total Lycopene To

Retinyl Palmitate Total β-Carotene trans-Lycopene Total L

trans-β-Carotene Total β-Cryptoxanthin 

Individualized Report 
Appendix E. Shipping Package Inserts for RR48 

The following three items were included in each package shipped to an RR48 participant: 

• Cover letter 

• Datasheet 

• Packing List and Shipment Receipt Confirmation Form 

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

samples themselves. The packing list was placed at the top of the shipping box, between 

the cardboard covering and the foam insulation. 

E1
UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899-

June 13, 2000 

Dear Colleague: 

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

XVIII) for 2000. You will find one vial of each of three lyophilized and two liquid-frozen 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 September 15, 2000. Results received two 

weeks after the due date will not be included in the summary report for this round robin study. The 

feedback report concerning the study will be provided around mid-October. 

Lyophilized 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. These esters 

absorb strongly in the UV region and elute 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). Liquid-frozen samples 267 and 268 should not be 

reconstituted. 

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; a-tocopherol, 75.8 at 292 nm; y-tocopherol, 

91.4 at 298 nm; a-carotene, 2800 at 444 nm (in hexane); ~-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 XL VIII to: 

Micronutrients Measurement Quality Assurance Program 

NIST 

100 Bureau Drive, Stop 8392 

Gaithersburg, MD 20899-8392 

Fax: (301) 977-0685 

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

e:::7: at jb omas l/t.gov; or mail/fax queries to the above address. 

v~Jf HJJ 

ice Brown Thomas 

earch Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

Enclosures 

cc: L. C. Sander 

E2

NISI 
 

 

 

Participant #: ________ Date: _____________ 

Round Robin XLVIII 

NIST Micronutrients Measurement Quality Assurance Program 

Analyte 264 265 266 267 268 Units* 

total retinol 

trans-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 

total β-cryptoxanthin 

total α-cryptoxanthin 

total lutein 

total zeaxanthin 

total lutein&zeaxanthin 

ubiquinone-10 (Q10) 

phylloquinone (K1) 

25-hydroxyvitamin D 

cholesterol 

Other analytes? 

* we prefer μg/mL 

Were sera 267 & 268 frozen when received? Yes | No 

Mail: M2QAP 

NIST, Stop 8392 Please return results on-or-before Fax: 301-977-0685 

Gaithersburg, MD 20899-8392 15-Sep-2000 Email: David.Duewer@NIST.gov 

E3
 

 

 

 

Participant #: ________ Date: _____________ 

Round Robin XLVIII
 

NIST Micronutrients Measurement Quality Assurance Program
 

Packing List and Shipment Receipt Confirmation Form
 

The enclosed bubble-pack (should) contain one vial each of the following five sera: 

Serum Form Reconstitute? 

#264 Lyophilized Yes (1 ml H2O) 

#265 Lyophilized Yes (1 ml H2O) 

#266 Lyophilized Yes (1 ml H2O) 

#267 Liquid frozen No 

#268 Liquid frozen No 

Please 1) Open the pack immediately 

2) Check that it contains one vial each of the above samples 

3) Check if sera #267 and #268 arrived frozen 

4) Store the RR XLVIII samples upright at -20  ̊C or below until analysis 

5) Complete the following information 

6) Fax the completed form to us at 301-977-0685 

(or email requested information to david.duewer@nist.gov) 

1) Date this shipment arrived: ___________________________ 

2) Are all five vials intact? Yes | No 

If "No", which one(s) were damaged? 

3) Was there any dry-ice left in cooler? Yes | No 

4) Did sera #267 and #268 arrive frozen? Yes | No 

5) At what temperature are you storing the samples? _______  ̊C 

6) When do you expect to analyse these samples? ________________________ 

Thank you in advance for your prompt response. 

The M2QAP Gang 

Mail: M2QAP 

NIST, Stop 8392 Fax: 301-977-0685 

Gaithersburg, MD 20899-8392 Email: David.Duewer@NIST.gov 

E4
 

 

Appendix F. Final Report for RR48 

The following three 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 content of the “Individualized” 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
UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899-0001 

October 23, 2000 

Dear Colleague: 

Enclosed is the summary report of the results for Round Robin XL VIII (RR 48). 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 and interlaboratory accuracy 

and precision; and a summary of the NIST assigned value (NAV) vs. your laboratory value for the 

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

weighted means of the medians from this interlaboratory comparison exercise and the means from the 

analyses performed by NIST. 

Data for evaluating laboratory performance in RR 48 are provided in the comparability summary (Score 

Card) on page 8 of the "All Lab Report." Laboratory comparability is summarized as follows: results 

rated 1 to 3 are within 1 to 3 standard deviation(s) of the assigned value, respectively; those rated 4 are 

>3 standard deviations from the assigned value. 

If you hav~ concerns regarding your laboratory's performance, we suggest that you obtain and analyze a 

unit of SRM 968c, Fat-Soluble Vitamins, Carotenoids, and Cholesterol in Human Serum. If your 

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

The following are newly released publications. Reprints will be provided upon request. 

"NIST Micronutrients Measurement Quality Assurance Program: Characterizing the 

Measurement Community's Performance Over Time," Du ewer et al., Anal. Chem., 72, .lL 

4163- 4170 (2000). 

"C30 Stationary Phases for the Analysis of Food by Liquid Chromatography," Sander, L.C., 

Sharpless, K.E., and Pursch M., J. Chromatogr. A. 880, 189-202 (2000). 

The next NIST Micronutrients Measurement Quality Assurance Workshop will be held on April 4, 2001 

as a symposium at the Experimental Biology meeting in Orlando, Florida. This workshop will be held to 

allow participants to discuss analytical methods, results of intercomparison exercises from the past year, 

and other related topics. Details about the meeting will be sent under a separate cover as soon as meeting 

plans are finalized. A tentative workshop agenda is enclosed. There is no registration fee for the 

workshop. However, if you plan on attending the Experimental Biology conference on March 31-April 

4, a registration fee is required. Please contact the secretariat for the American Institute of Nutrition at 

301-530-7050; fax: 301-571-1892; e-mail:sec@asns.faseb.org for details regarding the conference. 

If you have any questions regardin this report, please contact David Duewer at 3011975-3935; e-mail: 

david.duewer@nist. 01/975-3120; e-mail: jbthomas@nist.gov; fax: 301/977-0685. 

n ytical Chemistry Division 

mical Science and Technology Laboratory 

cc: L. C. Sander 

Enclosures NlSI 

F2
1 

The NIST M2QAP Round Robin XLVIII (RR48) report consists of 

Page “Individualized” Report 

Your values, the number of labs reporting values, and our assigned values. 

2 to “Four Plot” summaries of your current and past measurement performance, one page for 

n each analyte you report that is also reported by at least 10 other participants. 

n+1 The “target” plot version of your “Comparability Summary” scores. 

Page “All Lab” Report 

1-5 A listing of all results and statistics for analytes reported by at least two laboratories 

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

A legend for the above two lists
 

7 The “Comparability Summary” (or “Score Card”) 

Samples. Five sera were distributed in RR48: the third distribution of SRM 968c Level II, a newly
 

prepared {liquid-frozen, lyophilized} pair, a single new lyophilized serum, and a single new liquid-frozen 

serum. The new {liquid-frozen, lyophilized} pair furthers our investigation of measurement differences
 

between “fresh” and lyophilized sera. SRM 968c Level II was distributed as a known reference for the 

new sera and to further assess measurand stability in the SRM.
 

Serum #264 is Level II of SRM 968c, previously distributed as #248 (RR44, 10/98) and #256 

(RR46,10/99). This material is a blended serum with native carotenoid levels, but it was augmented with
 

α- and δ-tocopherol. 

Sera {#268, #265} are {liquid-frozen, lyophilized} material prepared from a native serum pool. These
 

samples were prepared and aliquoted into vials as a single batch.
 

Serum #266 is a lyophilized material prepared from a native serum pool. 

Serum #267 is a liquid-frozen material prepared from a native serum pool.
 

Qualitative Results. 

1)	 Three participants noted (and, we think, all of you had) a small amount of precipitated material in 

Serum #266. We failed to re-filter the final blend of the serum pool used for this sample after a 

relatively small volume of a (filtered) stock serum was added to bring the pool to adequate volume. 

The resulting solids do not appear to affect anything other than aesthetics, but add it to the list of 

things we won’t do again... 

2)	 Two participants again diluted the liquid-frozen samples with 1 mL water. In addition to providing 

reconstitution instructions in the sample manifest and study cover letter, in the future we will label 

the vials themselves. 

3)	 Nearly all participants did receive their samples still frozen. We thank all of you who promptly 

confirmed receipt of the samples. We will request similar confirmation in all future studies. 

Quantitative Results 

1)	 There have been no changes in median level or measurement variability in SRM 968c Level II. We 

will continue to monitor this material. 

F3
 

2)	 Since the lyophilized materials are reconstituted WITH 1.0 mL water rather than TO a total volume 

of 1.0 mL, we expect that the measurand concentrations in serum #265 (lyophilized) should be about 

0.95x those of serum #268 (liquid-frozen). The observed medians of the participant ratios ranged 

from 0.97 for total a-carotene to 0.92 for retinyl palmitate, all with a fairly constant SD of ±0.05. 

The ratios for individual participants ranged from quite constant across all reported measurands to 

quite different for different measurands. All very confusing... we will try to sort some of it out for 

the Workshop coming up this Spring (see enclosed workshop agenda). If your average #265/#268 

ratio was not in the 0.90 to 1.00 range, you should re-evaluate how you reconstitute lyophilized 

materials. 

F4
 

Appendix G. “All-Lab Report” for RR48 

The following seven 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 XLVIII Laboratory Results 

All Results in μg/mL 

Lab 264 

Total Retinol 

265 266 267 268 

trans-Retinol Retinyl Palmitate α-Tocopherol γ-Tocopherol

FSV-BA 0.504 0.628 0.457 0.687 0.673 

FSV-BB 0.497 0.578 0.456 0.675 0.632 

FSV-BD 0.479 0.571 0.440 0.658 0.615 

FSV-BE 0.450 0.570 0.420 0.640 0.650 

FSV-BF 0.465 0.575 0.390 0.645 0.615 

FSV-BG 0.467 0.597 0.439 0.695 0.680 

FSV-BH 0.443 0.540 0.395 0.607 0.571 

FSV-BI 0.489 0.595 0.457 0.687 0.644 

FSV-BJ 0.481 0.580 0.431 0.647 0.603 

FSV-BK 0.494 0.556 0.450 0.668 0.624 

FSV-BL 0.490 0.600 0.460 0.720 0.690 

FSV-BM 0.467 0.574 0.421 0.651 0.593 

FSV-BN 0.446 0.503 0.440 0.595 0.570 

FSV-BO 0.426 0.536 0.402 0.622 0.595 

FSV-BP 0.525 0.605 0.490 0.708 0.658 

FSV-BQ 0.492 0.581 0.411 0.631 0.595 

FSV-BR >0.510 >0.620 >0.480 >0.685 >0.630 

FSV-BT 0.471 0.660 0.474 0.791 0.753 

FSV-BU 0.386 0.524 0.370 0.584 0.573 

FSV-BV 0.451 0.536 0.406 0.579 0.542 

FSV-BW 0.510 0.630 0.460 0.710 0.660 

FSV-BX >0.489 >0.588 >0.435 >0.682 >0.649 

FSV-CB 0.409 0.520 0.385 0.604 0.554 

FSV-CC 0.540 0.580 0.460 0.650 0.600 

FSV-CD >0.501 >0.605 >0.447 >0.668 >0.620 

FSV-CE 0.490 0.550 0.400 0.620 0.340 

FSV-CF 0.527 0.679 0.477 0.718 0.661 

FSV-CG 0.672 0.707 0.529 0.705 0.690 

FSV-CH 0.452 0.553 0.384 0.588 0.601 

FSV-CI 0.500 0.610 0.460 0.720 0.690 

FSV-CK 0.370 0.440 0.340 0.510 0.500 

FSV-CL 0.485 0.579 0.462 0.688 0.632 

FSV-CN 0.501 0.636 0.452 0.755 0.682 

FSV-CR 0.560 0.690 0.490 0.750 0.720 

FSV-CS >0.484 >0.595 >0.442 >0.719 >0.623 

FSV-CU >0.431 >0.559 >0.402 >0.623 >0.621 

FSV-CV 0.523 0.432 0.205 0.325 0.400 

FSV-CW >0.441 >0.511 >0.388 >0.687 >0.558 

FSV-CX >0.420 >0.533 >0.386 >0.562 >0.535 

FSV-DA 0.466 0.579 0.442 0.656 0.615 

FSV-DB 0.533 0.613 0.468 0.673 0.668 

FSV-DF 0.414 0.516 0.393 0.568 0.540 

FSV-DI >0.496 >0.610 >0.442 >0.687 >0.646 

FSV-DK 0.497 0.605 0.434 0.751 0.662 

FSV-DP >0.507 >0.606 >0.442 >0.667 >0.622 

FSV-DQ 

FSV-DR 0.490 0.575 0.459 0.700 0.580 

FSV-DU 0.650 0.580 0.370 0.610 0.660 

FSV-EM 0.410 0.490 0.370 0.550 0.490 

FSV-EQ 0.484 0.592 0.461 0.804 0.640 

FSV-ES >0.471 >0.587 >0.402 >0.667 >0.625 

FSV-FH 0.606 0.715 0.516 0.806 0.747 

FSV-FJ 0.690 0.950 0.700 1.060 0.980 

FSV-FT 0.530 0.700 0.520 0.750 0.660 

FSV-FW 0.504 0.645 0.492 0.742 0.726 

264 265 266 267 268 

0.510 0.620 0.480 0.685 0.630 

0.489 0.588 0.435 0.682 0.649 

0.490 0.560 0.440 0.640 0.600 

0.501 0.605 0.447 0.668 0.620 

0.484 0.595 0.442 0.719 0.623 

0.431 0.559 0.402 0.623 0.621 

0.441 0.511 0.388 0.687 0.558 

0.420 0.533 0.386 0.562 0.535 

0.496 0.610 0.442 0.687 0.646 

0.507 0.606 0.442 0.667 0.622 

0.471 0.587 0.402 0.667 0.625 

264 265 266 267 268 

0.102 0.214 0.061 nd 0.232 

0.071 0.186 0.046 nd 0.216 

0.082 0.203 0.077 0.069 0.236 

0.112 0.248 0.053 0.048 0.284 

0.084 0.234 0.058 0.022 0.270 

0.063 0.189 0.032 nq 0.208 

0.084 0.217 0.064 0.027 0.233 

0.082 0.340 0.056 0.022 0.340 

0.093 0.181 0.056 0.035 0.220 

0.080 0.210 0.050 0.030 0.210 

0.126 0.202 0.098 0.081 0.231 

0.066 0.207 0.040 0.013 0.216 

0.068 0.263 0.041 0.028 0.294 

0.060 0.185 0.035 0.010 0.203 

0.023 0.114 0.022 nq 0.123 

264 265 266 267 268 

16.4 15.4 6.92 6.37 16.4 

17.9 15.7 7.13 6.61 16.8 

15.1 13.8 6.40 6.20 14.8 

15.4 13.8 6.30 5.80 15.6 

15.6 15.0 5.90 6.05 16.2 

16.8 15.6 6.95 6.57 17.4 

16.5 14.3 6.60 6.25 15.2 

16.8 14.2 6.99 6.46 15.3 

17.4 16.8 6.92 5.94 17.2 

16.4 13.4 6.35 5.53 14.6 

16.8 15.1 9.04 6.89 13.8 

15.3 13.9 6.40 5.70 14.6 

16.1 12.5 6.82 5.80 14.2 

16.4 14.0 7.00 6.90 15.7 

17.0 12.7 7.89 9.80 12.7 

15.2 12.9 6.14 5.98 13.0 

20.0 17.1 7.82 7.62 17.5 

14.6 13.1 6.55 5.65 13.4 

14.2 9.0 5.68 5.21 14.9 

19.1 16.7 7.84 6.72 15.9 

18.0 15.5 7.32 6.45 15.4 

16.3 14.6 6.71 6.30 16.1 

16.4 14.3 6.82 6.48 15.4 

17.2 13.5 6.73 6.16 14.4 

16.4 14.8 6.40 6.00 14.4 

26.4 25.2 11.10 9.98 11.9 

18.5 17.4 7.60 7.20 17.1 

14.1 12.8 5.59 5.56 14.1 

18.6 15.5 6.85 7.08 16.9 

16.2 12.6 6.20 5.80 12.6 

13.3 12.2 5.06 4.80 12.6 

18.8 18.1 8.88 7.79 20.3 

16.3 14.8 6.44 6.37 15.6 

18.7 16.1 7.80 7.30 16.9 

17.2 14.7 6.80 6.02 14.4 

15.4 12.7 6.69 6.55 14.9 

18.0 14.9 6.17 6.07 15.4 

18.9 15.8 7.26 6.65 17.7 

15.2 13.3 6.04 5.34 13.4 

15.9 14.6 6.85 6.28 15.8 

16.9 15.5 7.65 6.35 17.0 

17.1 14.6 6.81 6.23 15.4 

16.3 12.4 5.36 5.35 11.0 

14.9 12.5 4.05 4.29 10.5 

18.2 14.6 7.39 7.19 14.6 

27.9 18.9 7.10 6.40 20.8 

14.1 11.8 5.60 4.80 12.2 

16.7 15.1 6.90 8.40 15.6 

16.0 14.6 6.37 6.50 15.0 

16.9 13.2 6.70 6.50 13.7 

18.6 17.4 8.10 7.30 18.4 

20.0 14.2 8.70 7.20 13.9 

264 265 266 267 268 

1.48 1.92 1.88 2.40 2.05 

1.51 1.66 1.77 2.23 1.79 

1.60 1.90 1.90 2.40 2.20 

1.45 1.66 1.85 2.34 1.82 

1.57 1.72 1.93 2.40 1.91 

1.77 1.95 1.97 2.58 2.01 

1.47 1.67 1.91 2.31 1.83 

1.58 1.80 1.80 2.22 1.91 

1.21 1.20 1.46 1.67 1.42 

1.74 1.84 1.78 2.02 1.54 

1.28 1.55 1.73 2.12 1.67 

1.65 1.89 1.99 2.45 1.89 

1.90 2.08 2.28 2.67 2.20 

1.64 1.79 1.91 2.52 1.97 

1.62 1.95 1.94 2.38 1.86 

1.55 1.80 1.77 2.52 1.97 

1.13 1.34 1.26 1.78 1.44 

1.40 1.70 1.70 2.10 1.70 

1.24 2.10 1.44 1.91 2.24 

2.02 2.62 2.98 4.08 6.59 

1.56 1.74 1.79 2.55 1.90 

1.64 1.84 1.97 2.40 1.86 

1.65 1.71 1.74 2.33 1.88 

1.78 1.99 2.08 2.64 2.11 

1.47 1.61 1.67 2.09 1.68 

1.61 1.79 1.94 2.45 1.90 

1.48 1.53 1.49 2.08 1.46 

1.49 1.39 1.30 1.45 1.72 

1.90 2.30 2.40 3.00 2.40 

N 44 44 44 44 44 11 11 11 11 11 15 15 15 11 15 52 52 52 52 52 29 29 29 29 29 

Min 0.370 0.432 0.205 0.325 0.340 0.420 0.511 0.386 0.562 0.535 0.023 0.114 0.022 0.010 0.123 13.3 9.0 4.05 4.29 10.5 1.13 1.20 1.26 1.45 1.42 

Median 0.490 0.580 0.446 0.671 0.632 0.489 0.588 0.440 0.668 0.622 0.082 0.207 0.053 0.028 0.231 16.6 14.6 6.81 6.36 15.3 1.57 1.79 1.85 2.38 1.89 

Max 0.690 0.950 0.700 1.060 0.980 0.510 0.620 0.480 0.719 0.649 0.126 0.340 0.098 0.081 0.340 27.9 25.2 11.10 9.98 20.8 2.02 2.62 2.98 4.08 6.59 

eSD 0.043 0.047 0.044 0.073 0.059 0.027 0.033 0.010 0.028 0.012 0.021 0.031 0.016 0.010 0.031 1.8 1.6 0.67 0.70 1.7 0.13 0.19 0.17 0.25 0.23 

eCV 9 8 10 11 9 5 6 2 4 2 25 15 31 37 13 11 11 10 11 11 8 11 9 10 12 

Npas t 47 0 0 0 0 7 0 0 0 0 16 0 0 0 0 48 0 0 0 0 26 0 0 0 0 

Medianpas t 0.479 0.485 0.081 16.6 1.58 

SDpas t 0.038 0.050 0.022 1.3 0.14 

NISTa >0.491 >0.633 >0.460 >0.717 >0.671 0.491 0.633 0.460 0.717 0.671 16.8 15.5 7.18 6.29 15.4 1.55 1.98 1.98 2.53 1.98 

NISTb >0.475 >0.602 >0.439 >0.673 >0.644 0.475 0.602 0.439 0.673 0.644 17.2 15.2 6.92 6.26 15.5 1.60 1.82 1.91 2.40 1.88 

NNIST 6 5 6 6 6 6 5 6 6 6 6 5 6 6 6 6 5 6 6 6 

MeanNIST 0.483 0.618 0.449 0.695 0.657 0.483 0.618 0.449 0.695 0.657 17.0 15.4 7.05 6.28 15.4 1.58 1.90 1.94 2.46 1.93 

Sr ep 0.015 0.005 0.012 0.011 0.012 0.015 0.005 0.012 0.011 0.012 0.3 0.2 0.18 0.11 0.1 0.06 0.06 0.09 0.08 0.08 

Shet 0.019 0.016 0.009 0.011 0.022 0.019 0.016 0.009 0.011 0.022 0.5 0.4 0.17 0.22 0.4 0.03 0.12 0.04 0.06 0.10 

Sanl 0.011 0.022 0.017 0.031 0.019 0.011 0.022 0.017 0.031 0.019 0.3 0.2 0.19 0.02 0.1 0.04 0.11 0.05 0.09 0.07 

SNIST 0.026 0.028 0.022 0.035 0.031 0.026 0.028 0.022 0.035 0.031 0.7 0.5 0.31 0.25 0.4 0.08 0.17 0.11 0.14 0.15 

NAV 0.486 0.599 0.449 0.682 0.645 0.486 0.603 0.444 0.682 0.640 0.082 0.207 0.053 0.028 0.231 16.8 15.0 6.93 6.30 15.3 1.57 1.85 1.90 2.40 1.91 

NAU 0.040 0.056 0.043 0.080 0.065 0.040 0.051 0.036 0.056 0.055 0.026 0.050 0.021 0.018 0.055 1.6 1.7 0.70 0.64 1.7 0.17 0.21 0.21 0.28 0.22 

All Lab R epor t G2 P age 1 / 7 
Round Robin XLVIII Laboratory Results 

All Results in μg/mL 

Lab 

δ-Tocopherol

264 265 266 267 268 

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

FSV-BA 

FSV-BB 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 0.23 nd nd nd nd 

FSV-BI 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.96 0.45 0.46 0.47 0.46 

FSV-BO 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BT 1.65 0.80 0.82 0.54 0.50 

FSV-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CG 0.83 0.17 0.16 0.12 0.20 

FSV-CH 

FSV-CI 

FSV-CK 

FSV-CL 

FSV-CN 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CV 

FSV-CW 0.47 0.08 0.08 0.07 0.09 

FSV-CX 

FSV-DA 0.56 0.15 0.14 0.11 0.12 

FSV-DB 

FSV-DF 

FSV-DI 0.67 0.14 0.14 0.12 0.14 

FSV-DK 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-DU 

FSV-EM 

FSV-EQ 

FSV-ES 

FSV-FH 

FSV-FJ
 

FSV-FT
 

FSV-FW
 

264 265 266 267 268 

0.419 0.276 0.326 0.515 0.302 

0.386 0.254 0.296 0.475 0.271 

0.189 0.109 0.143 0.224 0.117 

0.405 0.183 0.307 0.530 0.252 

0.452 0.301 0.338 0.614 0.319 

0.461 0.290 0.337 0.533 0.311 

0.460 0.290 0.353 0.582 0.313 

0.391 0.205 0.271 0.394 0.197 

0.455 0.265 0.368 0.508 0.298 

0.396 0.248 0.190 0.247 0.272 

0.415 0.245 0.290 0.465 0.243 

0.346 0.236 0.272 0.442 0.242 

0.483 0.335 0.373 0.590 0.356 

0.404 0.269 0.333 0.527 0.288 

0.420 0.270 0.330 0.520 0.270 

>0.413 >0.271 >0.315 >0.525 >0.294 

0.530 0.316 0.399 0.535 0.320 

0.426 0.258 0.299 0.494 0.263 

0.420 0.340 0.380 0.550 0.140 

0.400 0.271 0.304 0.498 0.287 

0.441 0.284 0.307 0.528 0.304 

0.258 0.170 0.213 0.329 0.172 

0.506 0.323 0.397 0.558 0.350 

>0.405 >0.260 >0.307 >0.523 >0.263 

0.452 0.302 0.356 0.567 0.310 

0.490 0.165 0.400 0.587 0.174 

0.391 0.248 0.310 0.472 0.271 

>0.332 >0.223 >0.259 >0.418 >0.208 

0.280 0.275 0.227 0.362 0.288 

0.350 0.252 0.295 0.457 0.245 

>0.356 >0.216 >0.287 >0.452 >0.247 

0.340 0.232 0.283 0.461 0.246 

0.305 0.149 0.197 0.433 0.268 

0.450 0.326 0.440 0.705 0.324 

>0.280 >0.130 >0.200 >0.470 >0.090 

0.429 0.290 0.135 0.515 0.268 

0.477 0.310 0.455 0.634 0.790 

>0.349 >0.227 >0.263 >0.468 >0.246 

0.306 0.193 0.247 0.424 0.199 

264 265 266 267 268 

0.385 0.255 0.300 0.491 0.281 

0.367 0.244 0.284 0.461 0.261 

0.430 0.273 0.314 0.511 0.292 

0.409 0.243 0.341 0.478 0.277 

0.388 0.237 0.179 0.238 0.267 

0.316 0.219 0.254 0.418 0.222 

0.413 0.271 0.315 0.525 0.294 

0.369 0.249 0.280 0.470 0.265 

0.405 0.260 0.307 0.523 0.263 

0.407 0.276 0.327 0.528 0.285 

0.363 0.233 0.290 0.448 0.252 

0.332 0.223 0.259 0.418 0.208 

0.250 0.244 0.208 0.331 0.255 

0.356 0.216 0.287 0.452 0.247 

0.280 0.130 0.200 0.470 0.090 

0.463 0.301 0.444 0.622 0.630 

0.349 0.227 0.263 0.468 0.246 

264 265 266 267 268 

0.034 0.021 0.025 0.024 0.021 

0.019 0.011 0.013 0.014 0.010 

0.031 0.018 0.023 0.022 0.019 

0.046 0.022 0.027 0.030 0.021 

0.008 0.011 0.011 0.009 0.005 

0.034 0.017 0.018 0.024 0.021 

0.031 0.022 0.023 0.028 0.022 

0.044 0.026 0.030 0.039 0.025 

0.028 0.015 0.020 0.024 0.019 

0.030 0.031 0.019 0.031 0.033 

0.014 0.009 0.011 0.012 0.160 

N 7 6 6 6 6 33 33 33 33 33 17 17 17 17 17 11 11 11 11 11 

Min 0.23 0.08 0.08 0.07 0.09 0.189 0.109 0.135 0.224 0.117 0.250 0.130 0.179 0.238 0.090 0.008 0.009 0.011 0.009 0.005 

Median 0.67 0.16 0.15 0.12 0.17 0.419 0.269 0.307 0.515 0.271 0.369 0.244 0.287 0.470 0.263 0.031 0.018 0.020 0.024 0.021 

Max 1.65 0.80 0.82 0.54 0.50 0.530 0.340 0.455 0.705 0.790 0.463 0.301 0.444 0.622 0.630 0.046 0.031 0.030 0.039 0.160 

eSD 0.30 0.07 0.06 0.05 0.10 0.049 0.047 0.068 0.077 0.046 0.055 0.026 0.042 0.061 0.025 0.004 0.006 0.007 0.009 0.003 

eCV 45 47 41 40 57 12 18 22 15 17 15 11 14 13 9 14 33 37 37 14 

Npas t 10 0 0 0 0 33 0 0 0 0 15 0 0 0 0 10 0 0 0 0 

Medianpas t 0.80 0.424 0.389 0.031 

SDpas t 0.41 0.048 0.029 0.010 

NISTa 0.53 nd nd nd nd 0.424 0.249 0.326 0.506 0.241 0.378 0.215 <0.326 0.438 0.200 0.047 0.033 nd 0.068 0.041 

NISTb 0.54 0.11 0.10 0.09 0.11 0.425 0.275 0.329 0.526 0.289 0.379 0.243 0.300 0.486 0.259 0.046 0.032 0.029 0.040 0.030 

NNIST 6 2 3 3 3 6 5 6 6 6 6 5 3 6 6 

MeanNIST 0.54 0.11 0.10 0.09 0.11 0.425 0.264 0.328 0.516 0.264 0.385 0.229 0.300 0.462 0.230 

Sr ep 0.02 0.01 0.02 0.01 0.01 0.009 0.007 0.020 0.017 0.012 0.009 0.005 0.005 0.026 0.010 

Shet 0.03 0.02 0.01 0.01 0.01 0.023 0.012 0.024 0.031 0.011 0.032 0.010 0.003 0.024 0.006 

Sanl 0.00 0.007 0.022 0.002 0.014 0.033 0.004 0.020 0.033 0.042 

SNIST 0.03 0.02 0.02 0.02 0.02 0.025 0.026 0.031 0.038 0.036 0.034 0.022 0.006 0.049 0.043 

NAV 0.61 0.14 0.12 0.11 0.14 0.422 0.266 0.317 0.512 0.268 0.377 0.237 0.293 0.466 0.246 0.031 0.018 0.020 0.024 0.021 

NAU 0.30 0.18 0.18 0.20 0.21 0.059 0.040 0.064 0.071 0.046 0.044 0.029 0.042 0.050 0.049 0.011 0.007 0.007 0.008 0.007 

All Lab R epor t G3 P age 2 / 7 
Round Robin XLVIII Laboratory Results 

All Results in μg/mL 

Lab 264 

Total α-Carotene

265 266 267 

trans-α-Carotene Total Lycopene 

268 

trans-Lycopene 

FSV-BA 0.096 0.102 0.030 0.020 0.112 

FSV-BB 0.077 0.093 0.020 0.015 0.099 

FSV-BD 

FSV-BE 

FSV-BF 0.093 0.101 0.039 0.030 0.099 

FSV-BG 0.098 0.106 0.036 0.036 0.102 

FSV-BH 0.112 0.116 0.026 0.019 0.124 

FSV-BI 0.100 0.101 0.029 0.025 0.115 

FSV-BJ 0.104 0.095 0.026 0.017 0.098 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.090 0.088 0.031 0.016 0.108 

FSV-BO 0.192 0.175 0.064 0.076 0.207 

FSV-BP 0.121 0.117 0.036 0.027 0.109 

FSV-BQ 

FSV-BR 

FSV-BT 0.074 0.083 0.026 0.020 0.086 

FSV-BU 0.111 0.141 0.040 0.031 0.148 

FSV-BV 0.098 0.111 0.030 0.019 0.105 

FSV-BW 0.104 0.112 0.038 0.026 0.110 

FSV-BX 0.110 0.121 0.036 0.026 0.126 

FSV-CB 0.085 0.084 0.022 0.013 0.085 

FSV-CC 

FSV-CD 0.106 0.092 0.028 0.016 0.105 

FSV-CE 

FSV-CF 

FSV-CG 0.098 0.110 0.032 0.024 0.118 

FSV-CH 0.094 0.104 0.028 0.021 0.111 

FSV-CI 

FSV-CK 0.053 0.098 0.033 0.019 0.098 

FSV-CL 0.112 0.115 0.029 0.022 0.116 

FSV-CN 0.105 0.104 0.038 0.030 0.103 

FSV-CR 

FSV-CS 0.137 0.151 0.035 0.027 0.158 

FSV-CU 

FSV-CV 

FSV-CW >0.076 >0.081 >0.025 >0.018 >0.087 

FSV-CX >0.097 >0.100 >0.026 >0.017 >0.091 

FSV-DA 0.069 0.102 0.026 0.019 0.112 

FSV-DB 

FSV-DF 

FSV-DI 

FSV-DK 0.096 0.113 0.032 0.021 0.117 

FSV-DP 

FSV-DQ 0.073 0.087 0.027 0.026 0.052 

FSV-DR 

FSV-DU 

FSV-EM 0.102 0.102 0.027 0.016 0.097 

FSV-EQ 0.117 0.118 0.046 0.114 0.120 

FSV-ES >0.088 >0.099 >0.023 >0.018 >0.100 

FSV-FH 

FSV-FJ 0.070 0.075 0.021 nq 0.075 

FSV-FT 

FSV-FW 

264 265 266 267 268 

0.076 0.081 0.025 0.018 0.087 

0.097 0.100 0.026 0.017 0.091 

0.088 0.099 0.023 0.018 0.100 

264 265 266 267 268 

!0.544 !0.39 !0.465 !0.313 !0.426 

0.410 0.310 0.334 0.233 0.330 

0.428 0.318 0.306 0.214 0.308 

0.447 0.305 0.313 0.232 0.313 

0.434 0.311 0.330 0.229 0.325 

0.349 0.241 0.269 0.192 0.281 

0.340 0.234 0.244 0.148 0.217 

0.485 0.330 0.417 0.270 0.370 

0.351 0.241 0.310 0.228 0.295 

0.546 0.355 0.469 0.346 0.337 

0.425 0.325 0.334 0.248 0.336 

0.338 0.265 0.265 0.132 0.278 

0.427 0.324 0.354 0.246 0.337 

0.410 0.310 0.330 0.250 0.310 

0.355 0.227 0.282 0.150 0.220 

0.407 0.289 0.308 0.226 0.318 

0.424 0.324 0.332 0.246 0.344 

0.367 0.267 0.260 0.215 0.319 

0.283 0.230 0.252 0.158 0.197 

0.519 0.392 0.435 0.274 0.408 

0.428 0.323 0.343 0.262 0.347 

0.473 0.369 0.388 0.271 0.378 

0.480 0.326 0.332 0.278 0.343 

0.423 0.314 0.346 0.228 0.329 

0.332 0.318 0.269 0.183 0.365 

0.493 0.357 0.402 0.302 0.344 

0.305 0.209 0.258 0.200 0.243 

0.381 0.268 0.268 0.193 0.247 

0.397 0.295 0.399 0.724 0.756 

0.315 0.231 0.256 0.205 0.267 

264 265 266 267 268 

0.229 0.159 0.187 0.155 0.176 

0.169 0.122 0.145 0.119 0.130 

0.237 0.155 0.178 0.150 0.159 

0.259 0.160 0.220 0.159 0.182 

0.174 0.132 0.139 0.102 0.132 

0.196 0.137 0.163 0.136 0.144 

0.212 0.156 0.173 0.146 0.166 

0.189 0.131 0.163 0.124 0.142 

0.204 0.143 0.167 0.134 0.132 

0.161 0.154 0.135 0.111 0.172 

0.212 0.140 0.175 0.126 0.163 

0.188 0.135 0.158 0.139 0.151 

N 29 29 29 28 29 3 3 3 3 3 29 29 29 29 29 12 12 12 12 12 

Min 0.053 0.075 0.020 0.013 0.052 0.076 0.081 0.023 0.017 0.087 0.283 0.209 0.244 0.132 0.197 0.161 0.122 0.135 0.102 0.130 

Median 0.098 0.104 0.030 0.022 0.109 0.088 0.099 0.025 0.018 0.091 0.410 0.310 0.330 0.229 0.325 0.200 0.142 0.165 0.135 0.155 

Max 0.192 0.175 0.064 0.114 0.207 0.097 0.100 0.026 0.018 0.100 0.546 0.392 0.469 0.724 0.756 0.259 0.160 0.220 0.159 0.182 

eSD 0.017 0.016 0.006 0.007 0.015 0.081 0.031 0.086 0.049 0.033 0.028 0.017 0.017 0.019 0.022 

eCV 17 15 20 33 14 20 10 26 21 10 14 12 10 14 14 

Npas t 28 0 0 0 0 0 0 0 0 0 27 0 0 0 0 13 0 0 0 0 

Medianpas t 0.095 0.404 0.206 

SDpas t 0.023 0.076 0.041 

NISTa 0.106 0.109 0.040 nd 0.109 

NISTb 0.092 0.091 0.029 0.020 0.097 0.080 0.082 0.024 0.015 0.089 0.439 0.291 0.334 0.241 0.319 

NNIST 6 5 5 3 6 3 2 3 3 3 3 2 3 3 3 

MeanNIST 0.100 0.100 0.034 0.020 0.103 0.082 0.082 0.024 0.015 0.089 0.449 0.291 0.334 0.241 0.319 

Sr ep 0.008 0.004 0.004 0.005 0.004 0.009 0.002 0.003 0.004 0.005 0.047 0.015 0.028 0.013 0.030 

Shet 0.009 0.004 0.005 0.006 0.004 0.009 0.003 0.001 0.001 0.004 0.047 0.013 0.026 0.023 0.025 

Sanl 0.009 0.012 0.008 0.008 

SNIST 0.015 0.013 0.010 0.008 0.010 0.013 0.004 0.003 0.004 0.006 0.066 0.019 0.038 0.026 0.039 

NAV 0.099 0.102 0.032 0.020 0.106 0.429 0.300 0.332 0.235 0.319 0.200 0.142 0.165 0.135 0.155 

NAU 0.028 0.030 0.011 0.008 0.031 0.092 0.071 0.074 0.055 0.072 0.036 0.025 0.029 0.024 0.027 

All Lab R epor t G4 P age 3 / 7 
Round Robin XLVIII Laboratory Results 

All Results in μg/mL 

Lab 

Total β-Cryptoxanthin

264 265 266 267 268 

Total α-Cryptoxanthin Total Lutein trans-Lutein 

264 265 266 267 268 

0.014 0.042 0.024 0.026 0.043 

0.016 0.040 0.026 0.033 0.049 

0.031 0.052 0.035 0.039 0.053 

0.034 0.034 0.021 0.032 0.038 

0.018 0.054 0.035 0.030 0.060 

0.022 0.043 0.028 0.029 0.046 

0.015 0.040 0.020 0.024 0.044 

264 265 266 267 268 

0.098 0.172 0.089 0.102 0.189 

0.089 0.180 0.089 0.065 0.209 

0.071 0.142 0.073 0.078 0.153 

0.078 0.172 0.091 0.089 0.189 

0.080 0.189 0.075 0.080 0.189 

0.064 0.123 0.074 0.073 0.141 

0.142 0.276 0.179 0.184 0.307 

0.090 0.181 0.100 0.138 0.211 

0.082 0.167 0.082 0.103 0.181 

- 0.159 0.086 0.083 0.166 

0.078 0.140 0.074 0.099 0.155 

0.063 0.128 0.064 0.061 0.129 

0.090 0.158 0.084 0.094 0.170 

0.074 0.156 0.076 0.084 0.165 

nd 0.041 0.060 0.190 0.262 

0.108 0.210 0.098 0.095 0.233 

29 29 29 29 29 

0.017 0.023 0.025 0.026 0.025 

0.034 0.062 0.054 0.052 0.067 

0.059 0.113 0.083 0.078 0.105 

0.010 0.012 0.013 0.010 0.013 

31 19 25 20 19 

28 

0.031 

0.008 

0 0 0 0 

0.041 0.065 0.067 0.073 0.067 

0.026 0.049 0.048 0.050 0.054 

5 5 6 6 6 

0.034 0.057 0.057 0.062 0.061 

0.001 0.004 0.002 0.004 0.005 

0.002 0.005 0.001 0.006 0.002 

0.011 0.011 0.014 0.016 0.009 

0.011 0.013 0.014 0.017 0.010 

0.034 0.059 0.056 0.056 0.063 

0.011 0.015 0.014 0.019 0.016 

0.020 0.041 0.027 0.029 0.043 

0.008 0.006 0.007 0.006 0.005 

0.081 0.166 0.085 0.089 0.181 

0.016 0.030 0.018 0.018 0.035 

7 7 7 7 7 

0.014 0.034 0.020 0.024 0.038 

0.018 0.042 0.026 0.030 0.046 

0.034 0.054 0.035 0.039 0.060 

0.006 0.003 0.007 0.004 0.004 

33 7 29 15 10 

6 

0.018 

0.007 

0 0 0 0 

0.021 0.039 0.028 0.029 0.042 

3 2 3 3 3 

0.021 0.039 0.028 0.029 0.042 

0.003 0.004 0.003 0.001 0.005 

0.003 0.004 0.003 0.002 0.002 

0.004 0.006 0.004 0.002 0.005 

14 16 16 16 16 

0.063 0.041 0.060 0.061 0.129 

0.081 0.163 0.083 0.092 0.185 

0.142 0.276 0.179 0.190 0.307 

0.013 0.029 0.013 0.017 0.037 

16 18 15 19 20 

16 

0.084 

0.016 

0 0 0 0 

0.088 0.187 0.100 0.096 0.195 

0.075 0.153 0.076 0.078 0.158 

6 5 6 6 6 

0.081 0.170 0.088 0.087 0.177 

0.006 0.002 0.006 0.005 0.010 

0.002 0.003 0.003 0.003 0.004 

0.009 0.024 0.017 0.013 0.027 

0.011 0.024 0.018 0.014 0.029 

264 265 266 267 268 

0.069 0.159 0.075 0.076 0.167 

0.074 0.133 0.070 0.094 0.146 

2 2 2 2 2 

0.069 0.133 0.070 0.076 0.146 

0.072 0.146 0.073 0.085 0.157 

0.074 0.159 0.075 0.094 0.167 

0 0 0 0 0 

FSV-BA
 

FSV-BB
 

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-BT 

FSV-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CG 

FSV-CH 

FSV-CI 

FSV-CK 

FSV-CL 

FSV-CN 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CV 

FSV-CW 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DF 

FSV-DI 

FSV-DK 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-DU 

FSV-EM 

FSV-EQ 

FSV-ES 

FSV-FH 

FSV-FJ
 

FSV-FT
 

FSV-FW
 

N 

Min 

Median 

Max 

eSD 

eCV 

Npas t 

Medianpas t 

SDpas t 

NISTa 

NISTb 

NNIST 

MeanNIST 

Sr ep 

Shet 

Sanl 

SNIST 

NAV 

NAU 

0.059 0.070 0.083 0.078 0.078 

0.034 0.062 0.054 0.054 0.066 

0.027 0.053 0.039 0.043 0.058 

0.032 0.052 0.048 0.047 0.066 

0.043 0.079 0.061 0.062 0.081 

0.036 0.071 0.064 0.064 0.077 

0.025 0.047 0.042 0.041 0.049 

0.037 0.061 0.063 0.065 0.074 

0.047 0.053 0.042 0.046 0.059 

0.055 0.061 0.065 0.056 0.064 

0.038 0.066 0.061 0.060 0.070 

0.017 0.113 0.079 0.076 0.105 

0.020 0.039 0.037 0.036 0.042 

0.035 0.056 0.051 0.054 0.062 

0.019 0.032 0.031 0.032 0.035 

0.026 0.054 0.054 0.045 0.072 

0.041 0.064 0.049 0.048 0.070 

0.037 0.086 0.054 0.059 0.086 

0.036 0.072 0.063 0.066 0.088 

0.035 0.066 0.055 0.046 0.067 

0.031 0.054 0.047 0.047 0.060 

0.044 0.066 0.056 0.054 0.072 

0.024 0.051 0.041 0.042 0.050 

0.032 0.066 0.048 0.048 0.076 

0.044 0.063 0.063 0.053 0.072 

0.020 0.023 0.025 0.026 0.025 

0.028 0.055 0.044 0.050 0.055 

0.023 0.065 0.075 0.052 0.060 

0.032 0.062 0.053 0.059 0.071 

All Lab R epor t G5 P age 4 / 7 
Round Robin XLVIII Laboratory Results 

All Results in μg/mL 

Lab 264 

Total Zeaxanthin 

265 266 267 

Total Lutein&Zeaxanthin Coenzyme Q10 

268 

Phylloquinone (K1) x1000 

FSV-BA
 

FSV-BB
 0.042 0.045 0.035 0.043 0.048 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 0.021 0.040 0.020 0.011 0.041 

FSV-BH 0.017 0.041 0.029 0.034 0.043 

FSV-BI 0.019 0.040 0.027 0.035 0.044 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.028 0.052 0.035 0.061 0.054 

FSV-BO 0.088 0.095 0.065 0.077 0.095 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BT 0.021 0.047 0.026 0.029 0.057 

FSV-BU 

FSV-BV 

FSV-BW 

FSV-BX 0.023 0.048 0.028 0.039 0.045 

FSV-CB - 0.037 0.027 0.041 0.037 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CG 

FSV-CH 

FSV-CI
 

FSV-CK
 0.001 0.002 0.001 0.002 0.002 

FSV-CL 

FSV-CN 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CV 

FSV-CW 0.021 0.038 0.026 0.047 0.042 

FSV-CX 0.021 0.044 0.024 0.031 0.043 

FSV-DA 0.030 0.025 0.036 0.032 0.038 

FSV-DB 

FSV-DF 

FSV-DI 

FSV-DK 

FSV-DP 

FSV-DQ 0.018 0.014 0.011 0.018 0.028 

FSV-DR 

FSV-DU 

FSV-EM 

FSV-EQ 

FSV-ES 0.024 0.048 0.028 0.040 0.055 

FSV-FH 

FSV-FJ 

FSV-FT 

FSV-FW 

264 265 266 267 268 

0.122 0.228 0.121 0.150 0.256 

0.140 0.217 0.124 0.145 0.237 

0.106 0.217 0.100 0.129 0.255 

0.117 0.235 0.116 0.079 0.265 

0.088 0.183 0.101 0.112 0.196 

0.097 0.212 0.118 0.124 0.233 

0.078 0.149 0.092 0.104 0.169 

0.230 0.371 0.244 0.261 0.402 

0.093 0.200 0.096 0.104 0.222 

0.111 0.228 0.125 0.167 0.268 

0.093 0.273 0.123 0.156 0.273 

0.102 0.212 0.114 0.134 0.224 

0.105 0.214 0.110 0.142 0.226 

0.105 0.196 0.114 0.124 0.204 

0.110 0.208 0.097 0.118 0.224 

0.124 0.233 0.122 0.152 0.261 

0.090 0.186 0.099 0.102 0.179 

0.121 0.219 0.123 0.152 0.256 

0.100 0.207 0.106 0.133 0.217 

0.109 0.241 0.118 0.144 0.296 

0.102 0.200 0.105 0.116 0.214 

0.099 0.178 0.100 0.146 0.197 

0.084 0.172 0.088 0.092 0.172 

0.120 0.178 0.120 0.126 0.208 

0.108 0.207 0.131 0.136 0.240 

0.018 0.056 0.071 0.207 0.290 

0.080 0.165 0.074 0.074 0.165 

0.127 0.200 0.132 0.242 0.254 

0.132 0.258 0.126 0.135 0.287 

264 265 266 267 268 

1.202 0.882 0.884 1.245 0.872 

0.820 0.640 0.610 0.680 0.630 

0.388 0.267 0.317 0.318 0.292 

264 265 266 267 268 

0.94 1.16 0.42 1.64 1.38 

1.43 1.28 0.42 1.42 1.61 

N 14 15 15 15 15 29 29 29 29 29 3 3 3 3 3 2 2 2 2 2 

Min 0.001 0.002 0.001 0.002 0.002 0.018 0.056 0.071 0.074 0.165 0.388 0.267 0.317 0.318 0.292 0.94 1.16 0.42 1.42 1.38 

Median 0.021 0.041 0.027 0.035 0.043 0.105 0.208 0.114 0.134 0.233 0.820 0.640 0.610 0.680 0.630 1.19 1.22 0.42 1.53 1.50 

Max 0.088 0.095 0.065 0.077 0.095 0.230 0.371 0.244 0.261 0.402 1.202 0.882 0.884 1.245 0.872 1.43 1.28 0.42 1.64 1.61 

eSD 0.005 0.008 0.005 0.009 0.007 0.018 0.030 0.017 0.027 0.042 

eCV 23 21 18 27 17 17 14 15 20 18 

Npas t 15 0 0 0 0 27 0 0 0 0 0 0 0 0 0 0 0 0 0 0 

Medianpas t 0.024 0.110 

SDpas t 0.007 0.028 

NISTa 0.019 0.030 nd 0.040 0.036 0.107 0.217 0.100 0.136 0.231 

NISTb 0.031 0.050 0.031 0.041 0.050 0.107 0.202 0.107 0.119 0.208 

NNIST 6 5 3 6 6 6 5 6 6 6 

MeanNIST 0.024 0.040 0.031 0.040 0.043 0.107 0.210 0.103 0.128 0.219
 

Sr ep 0.003 0.002 0.003 0.003 0.005 0.005 0.004 0.008 0.006 0.010
 

Shet 0.004 0.000 0.002 0.003 0.003 0.006 0.002 0.004 0.004 0.003
 

Sanl 0.008 0.013 0.001 0.010 0.002 0.011 0.005 0.012 0.016
 

SNIST 0.010 0.014 0.004 0.004 0.012 0.008 0.011 0.010 0.014 0.019 

NAV 0.023 0.041 0.029 0.039 0.043 0.106 0.210 0.109 0.129 0.222
 

NAU
 0.010 0.014 0.008 0.011 0.012 0.022 0.044 0.025 0.028 0.047 

All Lab R epor t G6 P age 5 / 7 
 

 

 

 

 

Round Robin XLVIII Laboratory Results
 

All Results in μg/mL
 

Analytes Reported By One Laboratory 

Term 

N 

Min 

Medianpart 

Max 

SD 

CV 

Npast 

Medianpast 

SDpast 

NISTa, NISTb 

NNIST 

MeanNIST 

Srep 

Shet 

Sanl 

SNIST 

NAV 

NAU 

-

nd 

nq 

<x 

! 

italics 

Analyte Code 264 265 266 267 268 

trans-β-Cryptoxanthin NISTb 0.025 0.044 0.042 0.043 0.051 

3'-dehydro-Lutein FSV-BH 0.03 0.05 0.03 0.03 0.06 

Total Carotenoids FSV-BT 1.16 1.15 0.95 1.08 1.30 

Phytofluene FSV-CL 0.051 0.030 0.046 0.024 0.152 

Phytoene FSV-CL 0.109 0.122 0.109 0.038 0.282 

25-hydroxyvitamin D FSV-BN nq 0.018 0.041 0.009 0.017 

25-hydroxyvitamin D3 FSV-EM 0.03 0.02 0.01 0.00 0.02 

Table 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

 Standard deviation for (non-NIST) results: 0.741*(3rd Quartile - 1st Quartile)

 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)

 Mean of all analyses (vials x duplicates) reported by given NIST analyst

 Number of total vials analyzed in duplicate by NIST analysts

 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

 = (Medianpart + MeanNIST)/2 for analytes reported by NIST analyst(s)

 = Medianpart 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 Medianpart and MeanNIST. The expected long-term SD, eSD,

 is defined in: Duewer, et al. Anal Chem 1997;69(7):1406-1413.

 Not analyzed

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

 Detected but not quantitatively determined

 Concentration greater than x 

 Non-quantitative value: heterogeneous serum, damaged sample, malfunction, etc.

 Not explicitly reported but calculated by NIST from reported values

All Lab Report 

G7

Page 6 / 7 
 

 

 

 

 

 

Round Robin XLVIII Laboratory Results
 

Comparability Summary
 

Lab 

FSV-BA 

FSV-BB 

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-BT 

FSV-BU 

FSV-BV 

FSV-BW
 

FSV-BX
 

FSV-CB
 

FSV-CC
 

FSV-CD
 

FSV-CE
 

FSV-CF
 

FSV-CG
 

FSV-CH
 

FSV-CI
 

FSV-CK
 

FSV-CL
 

TR aT gT bC tbC aC TLy TbX TLu TZ L&Z 

1 1 1 1 1 1 2 1 1 1 

1 1 1 1 1 1 1 1 1 2 2 

1 1 

1 1 1 4 1 

1 1 1 2 1 1 1 

1 1 1 1 1 1 1 1 

1 1 1 1 1 1 1 1 1 2 1 

1 1 1 1 1 1 1 1 1 1 

1 1 1 2 1 2 1 3 1 

1 1 1 1 1 

1 2 

1 1 1 

2 1 3 1 1 1 1 1 

2 1 3 3 4 1 1 1 

1 3 1 1 2 2 

1 1 

1 2 1 

2 1 2 1 1 1 1 1 2 1 2 

2 2 2 2 2 2 3 1 1 1 

2 2 1 1 1 1 2 1 

1 1 2 1 1 1 2 2 2 

1 1 1 1 1 1 1 4 4 4 

2 1 2 1 2 2 2 1 1 

1 1 

1 1 1 1 1 1 1 

3 4 2 1 

2 2 

3 2 1 1 1 1 1 1 

1 1 3 1 1 1 1 

1 2 1 

3 3 2 3 1 2 1 1 

1 3 4 2 1 2 1 1 

Label

Lab 

TR 

aT

gT

bC 

tbC 

aC 

TLy

TbX 

TLu 

TZ 

L&Z

n 

% 1 

% 2 

% 3 

% 4 

 Definition 

 Participant code 

 Total Retinol 

α-Tocopherol 

 γ/β-Tocopherol 

 Total β-Carotene 

 trans-β-Carotene 

 Total α-Carotene 

 Total Lycopene 

 Total β-Cryptoxanthin 

 Total Lutein 

 Total Zeaxanthin 

 Total Lutein & Zeaxanthin 

 number of participants providing quantitative data 

 Percent of CS = 1 (within 1 SD of medians) 

 Percent of CS = 2 (within 2 SD of medians) 

 Percent of CS = 3 (within 3 SD of medians) 

 Percent of CS = 4 (3 or more SD from medians) 

“Comparability Score” 

The Comparability Score (CS) summarizes your measurement 

performance for a given analyte relative to the consensus 

medians in this study. CS is the average distance (in units of 

standard deviation) of your measurement performance 

characteristics from the consensus performance. CS is 

calculated when the number of quantitative values you reported 

Nyou, is at least two and at least six participants reported 

quantitative values for the analyte. 

We define CS as follows: 





 MINIMUM 4,INTEGER 1 



 





 

2 2 CS = + + C AP 



 

i Median i

you You − N 

NAU i

N you 

i 1 

∑ 

= C = Concordance = 

you 



 



 ∑ 

= 

N Youi 

NAU 

Me

i 

− 

i 1 

i 

 





2

dian 

N 1 

FSV-CR 2 2 

FSV-CU 1 1 1 

FSV-CN 1 1 1 1 1 1 1 1 1 1 1 

AP = Apparent Precision = 

you −

FSV-CS 1 1 1 1 1 2 1 1 1 

FSV-CV 4 1 1 2 1 

FSV-CW 2 2 2 1 1 1 1 1 

FSV-CX 2 2 2 1 1 1 

FSV-DB 1 1 1 1 1 

FSV-DF 2 NAU = NIST Assigned Uncertainty 

FSV-DI 1 1 1 1 1 4 2 4 

FSV-DK 1 2 2 1 1 2 For further details, please see 

FSV-DA 1 1 1 2 3 1 1 1 1 

FSV-DP
 

FSV-DQ
 

FSV-DR
 

FSV-DU
 

FSV-EM
 

FSV-EQ
 

FSV-ES
 

FSV-FH
 

FSV-FJ
 

FSV-FT
 

FSV-FW 

NISTa 

NISTb 

n 

% 1 

% 2 

% 3 

% 4 

1 

3 3 2 2 2 3 

1 1 2 2 1 1 

3 4 3 3 

2 2 2 1 1 1 

1 2 4 4 4 4 1 2 

1 1 1 1 1 1 1 1 

3 1 

4 2 3 2 1 

2 2 1 1 1 

2 

1 1 1 1 1 1 1 1 1 1 

1 1 1 1 1 1 1 1 1 1 1 

56 54 31 41 19 34 30 31 18 17 31 

TR aT g/bT bC tbC aC TLy TbX TLu TZ L&Z 

63 61 65 56 79 85 73 81 67 65 77 

25 28 19 32 0 9 23 13 22 24 16 

9 7 13 7 16 0 0 6 0 6 0 

4 4 3 5 5 6 3 0 11 6 6 

Duewer DL, Kline MC, Sharpless KE, Brown Thomas J, Gar 

KT. Micronutrients Measurement Quality Assurance 

Program: Helping participants use interlaboratory compariso 

exercise results to improve their long-term measurement 

performance. Anal Chem 1999;71(9):1870-8. 

All Lab Report G8 Page 7 / 7 
Appendix H. Representative “Individualized Report” for RR48 

Each participant in RR48 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 

• trans-Retinol 

• Retinyl Palmitate 

• α-Tocopherol 

• γ-Tocopherol 

• δ-Tocopherol 

• Total β-Carotene 

• trans-β-Carotene 

• Total cis-β-Carotene 

• Total α-Carotene 

• Total Lycopene 

• trans-Lycopene 

• Total β-Cryptoxanthin 

• Total α-Cryptoxanthin 

• Total Lutein 

• Total Zeaxanthin 

• Total Lutein & Zeaxanthin 

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

participant FSV-BA. 

H1
 

 Set 1 of 57

Individualized Round Robin XLVIII Report: FSV-BA 

Summary 

Serum 264 Serum 265 Serum 266 Serum 267 

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

Total Retinol 0.504 0.486 44 0.628 0.599 44 0.457 0.449 44 0.687 0.682 4

Retinyl Palmitate 0.10 0.08 15 0.2 0.2 15 0.1 0.1 15 nd 0.03 1

α-Tocopherol 16.37 16.82 52 15.45 14.99 52 6.92 6.93 52 6.37 6.30 5

γ/β-Tocopherol 1.482 1.574 29 1.921 1.846 29 1.876 1.897 29 2.401 2.401 2

Total β-Carotene 0.419 0.422 33 0.276 0.266 33 0.326 0.317 33 0.515 0.512 3

trans-β-Carotene 0.385 0.377 17 0.255 0.237 17 0.300 0.293 17 0.491 0.466 1

Total cis-β-Carotene 0.034 0.031 11 0.021 0.018 11 0.025 0.020 11 0.024 0.024 1

Total α-Carotene 0.096 0.099 29 0.102 0.102 29 0.030 0.032 29 0.020 0.020 2

Total Lycopene !0.544 0.429 29 !0.39 0.300 29 !0.465 0.332 29 !0.313 0.235 2

trans-Lycopene 0.229 0.200 12 0.159 0.142 12 0.187 0.165 12 0.155 0.135 1

Total β-Cryptoxanthin 0.059 0.034 29 0.070 0.059 29 0.083 0.056 29 0.078 0.056 2

Total Lutein&Zeaxanthin 0.122 0.106 29 0.23 0.21 29 0.12 0.11 29 0.150 0.129 2

H2

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

NAV : NIST Assigned Values, equal to (NIST's average-of-averages + this RR's median) / 2 

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

* : Non-quantitative value: heterogeneous serum, damaged sample, procedural error, etc. 

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

Micronutrients Measurement Quality Assurance Program 

National Institute of Standards and Technology 

100 Bureau Drive Stop 8392 

Gaithersburg, MD 20899-8392 USA Ema

 Individualized Report 
 

 

 Set 1 of 57

Individualized RR XLVIII Report: FSV-BA 

Total Retinol 

249 256 264 268 265 266 267

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see: 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem 1999;71(9):1870-8. 

Serum History Comments 

#264 #249 in RR44 (9/98), #256 in RR46 (9/99) SRM 968c, Level II 

#265 Lyophilized, same pool as #268 

#266 Lyophilized 

#267 Fresh frozen 

#268 Fresh frozen, same pool as #265 

 Individualized Report 

H3

Page 2 / 12 
 

 

 Set 1 of 57

Individualized RR XLVIII Report: FSV-BA 

Retinyl Palmitate 

249 256 264 268 265 266 267

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see: 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem 1999;71(9):1870-8. 

Serum History Comments 

#264 #249 in RR44 (9/98), #256 in RR46 (9/99) SRM 968c, Level II 

#265 Lyophilized, same pool as #268 

#266 Lyophilized 

#267 Fresh frozen 

#268 Fresh frozen, same pool as #265 

 Individualized Report 

H4

Page 3 / 12 
 

 

 Set 1 of 57

Individualized RR XLVIII Report: FSV-BA 

α-Tocopherol 

249 256 264 268 265 266 267

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see: 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem 1999;71(9):1870-8. 

Serum History Comments 

#264 #249 in RR44 (9/98), #256 in RR46 (9/99) SRM 968c, Level II 

#265 Lyophilized, same pool as #268 

#266 Lyophilized 

#267 Fresh frozen 

#268 Fresh frozen, same pool as #265 

 Individualized Report 

H5

Page 4 / 12 
 

 

 Set 1 of 57

Individualized RR XLVIII Report: FSV-BA 

γ/β-Tocopherol 

249 256 264 268 265 266 267

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see: 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem 1999;71(9):1870-8. 

Serum History Comments 

#264 #249 in RR44 (9/98), #256 in RR46 (9/99) SRM 968c, Level II 

#265 Lyophilized, same pool as #268 

#266 Lyophilized 

#267 Fresh frozen 

#268 Fresh frozen, same pool as #265 

 Individualized Report 

H6

Page 5 / 12 
 

 

 Set 1 of 57

Individualized RR XLVIII Report: FSV-BA 

Total β-Carotene 

249 256 264 268 265 266 267

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see: 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem 1999;71(9):1870-8. 

Serum History Comments 

#264 #249 in RR44 (9/98), #256 in RR46 (9/99) SRM 968c, Level II 

#265 Lyophilized, same pool as #268 

#266 Lyophilized 

#267 Fresh frozen 

#268 Fresh frozen, same pool as #265 

 Individualized Report 

H7

Page 6 / 12 
 

 

 Set 1 of 57

Individualized RR XLVIII Report: FSV-BA 

trans-β-Carotene 

249 256 264 268 265 266 267

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see: 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem 1999;71(9):1870-8. 

Serum History Comments 

#264 #249 in RR44 (9/98), #256 in RR46 (9/99) SRM 968c, Level II 

#265 Lyophilized, same pool as #268 

#266 Lyophilized 

#267 Fresh frozen 

#268 Fresh frozen, same pool as #265 

 Individualized Report H8 Page 7 / 12 
 

 

 Set 1 of 57

Individualized RR XLVIII Report: FSV-BA 

Total α-Carotene 

249 256 264 268 265 266 267

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see: 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem 1999;71(9):1870-8. 

Serum History Comments 

#264 #249 in RR44 (9/98), #256 in RR46 (9/99) SRM 968c, Level II 

#265 Lyophilized, same pool as #268 

#266 Lyophilized 

#267 Fresh frozen 

#268 Fresh frozen, same pool as #265 

 Individualized Report 

H9

Page 8 / 12 
 

 

 Set 1 of 57

Individualized RR XLVIII Report: FSV-BA 

trans-Lycopene 

249 256 264 268 265 266 267

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see: 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem 1999;71(9):1870-8. 

Serum History Comments 

#264 #249 in RR44 (9/98), #256 in RR46 (9/99) SRM 968c, Level II 

#265 Lyophilized, same pool as #268 

#266 Lyophilized 

#267 Fresh frozen 

#268 Fresh frozen, same pool as #265 

 Individualized Report 

H10

Page 9 / 12 
 

 

 Set 1 of 57

Individualized RR XLVIII Report: FSV-BA 

Total β-Cryptoxanthin 

249 256 264 268 265 266 267

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see: 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem 1999;71(9):1870-8. 

Serum History Comments 

#264 #249 in RR44 (9/98), #256 in RR46 (9/99) SRM 968c, Level II 

#265 Lyophilized, same pool as #268 

#266 Lyophilized 

#267 Fresh frozen 

#268 Fresh frozen, same pool as #265 

 Individualized Report 

H11

Page 10 / 12 
 

 

 Set 1 of 57

Individualized RR XLVIII Report: FSV-BA 

Total Lutein&Zeaxanthin 

249 256 264 268 265 266 267

[Analyte], μg/mL 

Your [Analyte], μg/mL

Serum Median [Analyte], μg/mL 

Apparent Precision, SD 

Apparent Precision, SD 

Concordance, SD Long-term Precision, SD 

3rd Quartile (75%) 

You, this RR You, >x, this RR NIST, this RR SRM 968c 

Median (50%) 95% confidence limits You, >x, past RRs You, past RRs Others, this RR 1st Quartile (25%) 

For details of the construction and interpretation of these plots, see: 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem 1999;71(9):1870-8. 

Serum History Comments 

#264 #249 in RR44 (9/98), #256 in RR46 (9/99) SRM 968c, Level II 

#265 Lyophilized, same pool as #268 

#266 Lyophilized 

#267 Fresh frozen 

#268 Fresh frozen, same pool as #265 

 Individualized Report 

H12

Page 11 / 12 
Set 1 of 57 

Individualized Round Robin XLVIII Report: FSV-BA
 

Graphical Comparability Summary
 

Total Retinol α-Tocopherol Total β-Carotene 

H13

Retinyl Palmitate γ/β-Tocopherol trans-β-Carotene To

Total Lycopene δ-Tocopherol Total cis-β-Carotene Total L

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

Individualized Report 
 

 

Appendix I. Shipping Package Inserts for RR13 

The following four items were included in each package shipped to an RR13 participant: 

• Cover letter 

• Protocol for Analyzing Samples 

• Preparation of Stock Solution and Diluted Solution Datasheet 

• Control and Test Samples Datasheet 

The cover letter, preparation protocol, and the two datasheets were enclosed in a sealed 

waterproof bag along with the samples themselves. 

I1
• # 

June 13, 2000 

Dear Colleague: 

UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899-

For the past 15 years the National Institute of Standards and Technology (NIST) has coordinated a 

Micronutrients Measurement Quality Assurance (QA) Program for laboratories making vitamin 

measurements in human serum. Frozen and/or freeze dried sera are sent to laboratories for analysis as an 

interlaboratory comparison exercise. Results are returned to NIST for data tabulation and evaluation. 

Value-assignment of the sample pools is based on the median of all the laboratory results, with 

confirmation based on measurements at NIST. We provide consultation and trouble-shooting regarding 

methods of analysis, and a certificate of participation in the QA program is issued at the end of each 

calendar year. We also host a micronutrient analysis QA workshop for fat-soluble vitamin, carotenoid, 

and ascorbic acid measurements in serum. 

The enclosed set of samples constitute the round robin exercise for vitamin C (Round Robin XIII) for 

2000. Four vials of frozen serum (test samples), and a vial of solid ascorbic acid (a control sample), are 

enclosed. Please follow the attached protocol when you analyze these samples. 

Report your results using the attached form by July 14, 2000. We also request that you send us a 

representative chromatogram from the analysis of each sample and indicate whether peak height or peak 

area was used in the calculation of the ascorbic acid concentration. Your results will be kept 

confidential. Results received two weeks after the due date will not be included in the summary report of 

this round robin study. The summary report concerning this study will be provided near the end of June. 

Please mail your results to: 

Micronutrients Measurement Quality Assurance Program 

NIST 

100 Bureau Drive, Stop 8392 

Gaithersburg, MD 20899-8392 

or Fax: 301.977.0685 E-mail: sam.margolis@nist.gov 

If you have any questions or concerns please call me at 301.975.3137 or contact me by Fax or E-mail. 

Thank you for your participation and we look forward to receiving your results. 

Sincerely, 

~~.~~~ Sam A. Margolis, Ph.D. 

Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

Enclosures \ 

NISI 

I2
 

 

 

 

 

 

Protocol for analyzing samples 

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 100 mL of 5% 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. Record the wavelength in the region of 240-245 nm at which 

you observe the maximum absorbance and record the absorbance at that wavelength. 

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 purpose of measuring the absorbance at the wave-length maximum is to check the concentration 

of your sample. If your spectrophotometer is properly calibrated the maximum absorbance should 

be between 243 and 244 nm and if the concentration is correct the molar extinction coefficient (E1%) 

of ascorbic acid at this wavelength (using a cell with a 1 cm path length) should be close to 550 ± 30. 

The extinction coefficient of your solution can be calculated using the following equation: 

E1% = observed OD ÷ g AA/100 mL of the diluted solution 

In the last three collaborative studies a significant number of laboratories reported total ascorbic acid 

(AA) values that were above the AA level of the samples but were significantly lower than the values 

for the total AA. This would suggest that the dehydroascorbic acid (DHAA) was not completely 

reduced to AA. In order to evaluate this possibility, we are asking those who utilize either 

dithiothreitol (DTT) or homocysteine (HS) to reduce DHAA to AA to use one of the following 

protocols. 

DTT Add 0.200 mL serum sample to 0.200 mL of a solution containing 0.5 mol/L K 2HPO4 and 

1 mg/mL DTT, mix, and incubate for 30 min at 21 °C. Add 0.160 mL of metaphosphoric 

acid (MPA) 400 g/L and assay by your method. 

HS Add 0.200 mL serum sample to 0.200 mL of a solution containing 0.5 mol/L K 2HPO4 and 

10 mmol/L HS, mix, and incubate for 30 min at 21 °C. Add 0.160 mL of metaphosphoric 

acid (MPA) 400 g/L and assay by your method. 

If you require larger samples increase the volumes but maintain the ratio of the sample to the 

reducing mixture. 

I3
The test samples are in sealed ampules and were prepared by adding equal volumes of 10% 

metaphosphoric acid to spiked human serum. We have checked the samples for stability and 

homogeneity and the total ascorbic acid appears to be sufficiently stable however, these samples 

contain some dehydroascorbic acid. The test samples should be defrosted by warming at 20 °C for 

not more than 10 min otherwise some irreversible oxidation of ascorbic acid may occur. 

Each ampule should contain between 0 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). 

I4
 

 

 

 

 

 

 

 

 

 

 

 

 

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 

Were samples frozen upon receipt? Yes No 

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 

Wavelength of maximum absorbance

Calculated molar absorptivity 

nm 

COMMENTS: (use other side if necessary) 

Mail by July 14, 2000 to: 

Micronutrients Measurement Quality Program 

NIST, 100 Bureau Drive, Stop 8392 

Gaithersburg, MD 20899-8392 

Fax: 301-977-0685 Micronutrients 

E-mail: sam.margolis@nist.gov 

I5
REPORT OF ANALYSIS
 

RESULTS (μmol/L of Sample)
 

CONTROL SAMPLE 1 

REPLICATE 1 μmol/L 

REPLICATE 2 μmol/L 

TEST SAMPLE #1 

REPLICATE 1 μmol/L 

REPLICATE 2 μmol/L 

TEST SAMPLE #2 

REPLICATE 1 μmol/L 

REPLICATE 2 μmol/L 

TEST SAMPLE #3 

REPLICATE 1 μmol/L 

REPLICATE 2 μmol/L 

TEST SAMPLE #4 

REPLICATE 1 μmol/L 

REPLICATE 2 μmol/L 

Mail by July 14, 2000 to: Fax: 301-977-0685 Micronutrients 

Micronutrients Measurement Quality Program E-mail: sam.margolis@nist.gov 

NIST, 100 Bureau Drive, Stop 8392 

Gaithersburg, MD 20899-8392 

I6
 

 

Appendix J. Final Report for RR13 

The following ten 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 content of the “Individualized” 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
 

 

 

 

 

December 4, 2000 

«Name» Dr. Margolis printed a separate cover letter «Company» for each RR13 participant. The words «Address1» within the “«»” are parameters for a mail­ «Address2» merge macro routine. «City», «State» «PostalCode» 

«Country» 

Dear «Name»: 

This report describes the results of Round Robin 13 (RR13) for the measurement of total 

ascorbic acid (TAA, ascorbic acid (AA) + dehydroascorbic acid (DHAA))) in human 

serum. Your results are designated as Lab. No. ~ in the accompanying table and figures 

of the “All laboratory” report. We also include an “Individalized” report of your own 

results that is very similar in format to that used in the fat-soluble Vitamin Quality 

Assurance Program (QAP). 

RR13 involved the duplicate analyses of a solid ascorbic acid sample and four human 

serum samples: 

S13:1, SRM 970 Level I, distributed as blind replicates in RRs 11 and 12 

S13:2, SRM 970 Level II, distributed as blind replicates in RRs 11 and 12 

S13:3, a 1:1 serum:metaphosphoric (MPA) material prepared 3/95 to have a 28.9 

μmol/L TAA level 

S13:4, a 1:1 serum:MPA material prepared 8/93 to have a 77.2 μmol/L TAA level. 

Table 1 summarizes the data for these samples and for the control solution each 

participant prepared from the solid ascorbic acid sample. As in the fat-soluble QAP, the 

estimated standard deviations (eSD) for the measurements are defined as 

0.74*(interquartile range) and the estimated coefficients of variation (eCV) are defined as 

100*eSD/median. NIST data are not included in the statistical analyses. 

Figures 1 through 4 detail the individual measurements reported by all participants. 

These plots suggest that many of the laboratories are not measuring all of the DHAA or 

that the AA is being degraded at some point during the assay procedure. 

Figure 5 presents an analysis of the components of variation, using data from RR11 and 

RR12 as well as RR13. The average duplicability (SDduplicability, within-sample withinRR) and repeatability (SDrepeatability, among-blind replicate within RR) represent the shortterm precision typical of the vitamin QAP participants. The agreement between these 

two short-term precision estimates suggests both that participants are reporting “true” 

duplicates (independently processed aliquots from one sample) and that both levels of the 

J2
 

 

 

 

 

 

SRM are homogenous. The average reproducibility (SDreproducibility , within-laboratory 

among RR) represents the long-term precision typical of the vitamin QAP participants. 

The interlaboratory variability (SDinterlaboratory ) is somewhat larger than SDreproducibility, 

reflecting among-participant discordances as well as within-participant imprecision. The 

dashed denotes Horwitz’s predicted interlaboratory variance for generic analytes at these 

concentrations (Horwitz W, Britton P, Chirtel SJ. A simple method for evaluating data 

from an interlaboratory study. JAOAC International 1998;81(6):1257-1265.) The 

SDinterlaboratory are about equal to Horwitz’s values, suggesting that TAA is not an 

unusually difficult measurand. However, the difference between SDinterlaboratory and 

SDreproducibility suggests that interlaboratory comparability can be improved. 

Using the data that you submitted to us, we calculated the density (DMPA) of your MPA 

solution. This value was low for one laboratory indicating a possible error in the 

preparation of the MPA solution. We also calculated the concentration of the TAA in the 

standard solution (AAcal , Table 1) that each of you made and assumed that the error in 

concentration was no greater than the error in weighing solutions. The amount of TAA 

that you actually measured in your assay of the standard solution is listed in Table 1, 

AAobs . To compare the measurements on the standard solutions, we calculated the ratio 

of the observed value to the calculated value. The median ratio was 0.97±0.06. If the 

estimated error in weighing and in filling the volumetric flasks is small (1 - 2%), then the 

major source of error is in the assay itself. Potential sources of such error include: 

1) inaccurate volume delivery of sample standard and/or serum delivered to the assay 

mixture, 2) inaccurate standards (impurities and/or degradation), 3) inaccurate constants 

and/or calculations, and 4) instability of the AA during the preparation and analysis steps 

(e.g., in the glassware, vials etc). 

We also asked each of you to measure the absorbance of your standard solution at 243 

nm and 244 nm (AA in MPA exhibits its maximum absorbance within these 

wavelengths). Every laboratory obtained similar values at each wavelength indicating 

that the wavelength was correct. The median E1% for a 1 cm cell was 565 AU/mole/cm, 

very close to the literature value of 560 AU/mole/cm at 243 nm. However, the range of 

results (526 AU/mole/cm to 613 AU/mole/cm) indicates a need for some laboratories to 

calibrate the absorbance scale of their spectrophotometers (e.g., NIST SRM 2031, Metalon-Quartz Filters, Transmittance). 

After the distribution of this set of samples, we made several significant observations that 

may affect the accuracy of the measurement of TAA. The first of these was the 

accidental observation that autosampler vials may catalyze the degradation of AA. In 

many vials we observed significant degradation (7%) within 4 hours. This occurs to 

some extent in all vials as well as other tubes used for sample handling. We believe that 

the variation in the composition of the glassware may account for a significant amount of 

interlaboratory variation and low values. It may also account for the formation of DHAA 

acid during the processing of blood samples. A manuscript describing several cleaning 

procedures to remedy this problem is in preparation and will be provided at a later date. 

J3
 

 

 

 

 

 

 

 

 

 

We also observed a significant increase in the AA levels in sample S13:3 between the 

time we distributed the samples to most participants and the time we assayed the samples 

in our laboratory. Two laboratories (VC-MR and VC-NQ) received samples late and 

their results are similar to the results that we obtained. This event was not unique to a 

single sample but was characteristic of four sets of samples prepared in 1995; we have 

not observed any change in any samples prepared in 1989, 1993, or 1998. All samples 

are sealed in glass ampoules and have been continuously stored together at –70 °C. 

Samples from different years were assayed together and only the 1995 samples were high 

thus this was not a function of the assay method. We have no explanation as to the cause 

of this increase. However, all of the material in the AA peak was electrochemically 

active and treatment with ascorbic acid oxidase chemically modified all of the material in 

the AA peak. We do not use S13:3 results in any of the comparability calculations. 

In a very recent study we observed that AA dissolved in 5% MPA is not as stable as AA 

dissolved in a solution of 75% acetonitrile, 25% water and 1 mg dithiothreitol (DTT)/mL. 

The AA in the MPA started degrading within 24 h (15% at the end of 24 h) whereas the 

DTT solution remained stable for 5 days. 

In conclusion we can identify the following sources of systematic bias in the results 

reported by participating laboratories: 

1) Pipetting of aqueous solutions (median 3-4% above expected value). 

2) Weighing of samples 0.5-100 g (CV of 1 and 2% respectively). 

3) Measurement of the concentration of a 50 μmol/L standard solution (CV of 9-10%). 

The median value is close to the expected value; therefore the error probably lies in 

the accuracy of the measurement of the sample or the values used for making your 

calculations. 

4) Measurement of the serum TAA. This could either reflect inaccurate dispensing of 

the total sample to the assay because of the viscosity of the sample, inaccurate 

values used in calculating the TAA concentration, or incomplete reduction of the 

DHAA. 

5) The variable degradation of TAA caused by the variation in the composition of the 

glassware or autosampler vials. 

6) Degradation of the TAA in a 5% MPA solution 

If your values differed from the medians by more than 2 eSDs (see target plot on your 

individual report) we suggest that you evaluate whether you accurately deliver the correct 

sample volume. This can vary either as a function of the sample viscosity or the accuracy 

of the pipette. We also suggest that you evaluate 1) the accuracy of the constants that you 

use in converting the assay results to a final AA concentration in the serum, 2) the 

completeness of the reduction of the DHAA, or 3) the possible oxidation of the AA to 

DHAA. If your results still differ significantly from the interlaboratory medians, you 

should reexamine your methods for possible systematic errors particularly degradation 

due to contaminated glassware (see enclosed preprint). If you need to validate your 

method, SRM 970 Ascorbic Acid in Frozen Human Serum is now available for purchase 

(http:/ts.nist.gov/ts/htdocs/230/232/232.htm). 

J4
If you have any questions concerning this report please contact Dave Duewer at 

david.duewer@nist,gov, or me at e-mail: sam.margolis@nist.gov; tel: 301/975-3137; fax: 

301/977-0685. 

Sincerely, 

<;;,___ ~ -~1:. ·Sam A. Margolis, Ph.D. 

Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

Enclosures 

J5
 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Figure Captions 

Figure 1. Summary of the Results of Round Robin 13 for the Measurement of 

TAA in Sample 1. Each point represents an individual measurement. The solid 

line represent the NIST certified value for AA + DHAA. 

Figure 2. Summary of the Results of Round Robin 13 for the Measurement of 

TAA in Sample 2. Each point represents an individual measurement. The solid 

line represent the NIST certified value for AA + DHAA. 

Figure 3. Summary of the Results of Round Robin 13 for the Measurement of 

TAA in Sample 3. Each point represents an individual measurement. The solid 

line represents the NIST value for AA + DHAA (combined gravimetric and LC 

measurements) assigned at the time the samples were prepared. 

Figure 4. Summary of the Results of Round Robin 13 for the Measurement of 

TAA in Sample 4. Each point represents an individual measurement. The solid 

lines represent the NIST value for AA + DHAA (combined gravimetric and LC 

measurements) assigned at the time the samples were prepared. 

Figure 5. Summary of the Statistical Analysis of the Combined Results of Round 

Robins 11- 13. 

J6
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J10
 

Figure 5. 

SDduplicability

CV ~ 3% 

SDrepeatability

CV ~4% 

SDreproducibility

CV ~ 8% 

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0 

2 

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Variance Component SDs, 

μmol/Lsample 

Horwitz 

0 20
 

Lv-II

S13-3

40
 

Interlaboratory Median, μmol/Lsample 

Lv-I

Adjusted

Control

S13-4 

J11
 

Appendix K. “All-Lab Report” for RR13 

The following single page is 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
Vitamin C "Round Robin" 13 Laboratory Results
 

Control Solution 

ODmax DMPA E1% [TAA] μmol/L 

Lab Method au g

/mL 

dL/gcm Cal Obs Obs/Cal 

VC-MA HPLC-EC 0.523 1.031 572 56.0 55.4 0.99 

VC-MB AO-OPD, Cobas Fara 0.578 1.032 559 58.7 63.5 1.08 

VC-MC HPLC-EC 0.565 1.031 573 56.2 56.9 1.01 

VC-MD 24DNPH 0.565 " " 56.2 46.6 0.83 

VC-ME HPLC-UV 0.520 1.030 574 51.4 48.9 0.95 

VC-MG HPLC-UV 0.614 1.036 613 56.9 56.5 0.99 

VC-MH HPLC-OPD/f 0.581 1.033 564 58.6 57.0 0.97 

VC-MI HPLC-UV 1.032 62.3 61.6 0.99 

VC-ML HPLC-UV 0.573 1.032 543 60.7 48.7 0.80 

VC-MO HPLC-OPD 0.551 1.030 550 56.9 61.4 1.08 

VC-MP Ferrozine/Beckman LX20 0.539 1.006 566 54.1 13.6 0.25 

VC-MR HPLC-EC 0.588 1.034 569 58.7 53.5 0.91 

VC-MS HPLC-EC 0.471 1.031 571 46.8 39.5 0.84 

VC-NE HPLC-UV 0.545 1.018 533 58.4 56.3 0.96 

VC-NI AO-OPD, Cobas Mira S 0.531 1.031 550 55.4 54.5 0.98 

VC-NK 24DNPH 0.527 1.031 526 56.9 71.3 1.25 

VC-NL HPLC-EC 0.576 1.035 569 57.4 56.0 0.98 

VC-NQ HPLC-OPD/f 0.549 1.030 547 57.0 54.1 0.95 

N 17 17 16 18 18 18 

Average 0.553 1.029 561 56.6 53.1 0.94 

Min 0.471 1.006 526 46.8 13.6 0.25 

Median 0.551 1.031 565 56.9 55.7 0.97 

Max 0.614 1.036 613 62.3 71.3 1.25 

eSD 0.035 0.001 12.7 2.3 5.9 0.05 

eCV 6 0.1 2 4 11 5 

NNIST 

Mean 

Expected 

Srep 

Shet 

SNIST 

Total Ascorbic Acid, μmol/L 

S13:1 S13:2 S13:3 S13:4 

8.5 27.7 57.1 69.2 

12.0 31.8 33.0 65.5 

7.9 26.5 29.3 61.0 

7.2 30.2 28.7 51.4 

6.3 21.9 22.0 54.7 

15.5 35.5 36.1 69.4 

8.6 27.8 29.6 55.1 

10.2 33.0 27.9 66.2 

9.3 25.4 27.5 51.6 

7.8 27.3 29.0 62.0 

1.7 6.0 6.8 16.2 

9.0 26.4 57.4 70.8 

10.9 21.4 20.7 41.0 

22.2 39.6 46.6 74.6 

7.5 29.0 29.5 59.3 

11.4 21.3 32.1 45.1 

7.5 25.8 26.0 54.9 

7.8 27.4 58.5 69.7 

18 18 18 18 

9.5 26.9 33.2 57.6 

1.7 6.0 6.8 16.2 

8.5 27.3 29.4 60.1 

22.2 39.6 58.5 74.6 

1.7 3.5 5.2 12.8 

20 13 18 21 

6 6 6 6 

9.7 29.6 63.9 75.5 

10.7 31.8 28.9 77.2 

0.42 0.52 1.52 1.27 

0.20 0.61 0.09 0.66 

0.47 0.80 1.52 1.43 

Note 

The S13:3 samples were intended to be the material originally designated "682b". Examination of Dr. 

Margolis's sample storage containers in 2007 strongly suggested that some of the S13:3 samples were 

actually a material originally designated "188a". Likewise, the S13:4 samples were intended to have all 

been the "179b" material but it is likely some were actually the "682b" material. 

All Lab Report 

K2

Page 1 / 1 
Appendix L. Representative “Individualized Report” for RR13 

Each participant in RR13 received an “Individualized Report” reflecting their reported 

results. The following two pages are the “Individualized Report” for participant 

“VC-MA”. 

L1
 

Set 1 of 18 

Vitamin C "Round Robin" 13 Report: Participant VC-MA
 

AA MPA Stock MPA 

mg g mg g 

[TAA]cal 

μmol/L 

A243 

OD 

200.0 103.09 526.0 102.45 

215.0 103.10 517.1 102.52 

200.8 103.16 508.0 102.58 

57.8 

61.1 

0.0 

0.0525 0

0.0721 0

0.5650 0

RR Date Sample 

11 09/23/98 Control 

12 04/02/99 Control 

13 09/17/01 Control 

Replicates, [TAA]obs μmol/Lsample Duplic

Method RR Date Sample 

HPLC-EC (Height) 11 09/23/98 11-Ctrl 

HPLC-EC (Height) 12 04/02/99 12-Ctrl 

HPLC-EC (Height) 13 09/17/01 13-Ctrl 

Rep1 Rep2 Factor Mean SDdup Mean 

6.3 5.9 1.0 6.1 0.3 0.487 

53.3 53.0 1.0 53.1 0.2 

55.9 55.0 1.0 55.4 0.7 

L2

Replicates, [TAA] μmol/Lsample Duplica

HPLC-EC (Height) 11 09/23/98 SRM Lv I, S11:1 

HPLC-EC (Height) 11 09/23/98 SRM Lv I, S11:1 

HPLC-EC (Height) 12 04/02/99 SRM Lv I, S12:1 

HPLC-EC (Height) 12 04/02/99 SRM Lv I, S12:1 

HPLC-EC (Height) 13 09/17/01 SRM Lv I, S13:1 

HPLC-EC (Height) 11 09/23/98 SRM Lv II, S11;2 

HPLC-EC (Height) 11 09/23/98 SRM Lv II, S11;2 

HPLC-EC (Height) 12 04/02/99 SRM Lv II, S12:2 

HPLC-EC (Height) 12 04/02/99 SRM Lv II, S12:2 

HPLC-EC (Height) 13 09/17/01 SRM Lv II, S13:2 

15.5 13.9 0.5 7.4 0.6 Mean 

14.0 14.5 0.5 7.1 0.2 7.8 

14.5 15.8 0.5 7.6 0.5 

16.1 15.1 0.5 7.8 0.3 

8.4 8.5 1.0 8.5 0.1 

50.7 47.7 0.5 24.6 1.1 Mean 

48.8 54.0 0.5 25.7 1.8 25.5 

49.5 45.9 0.5 23.9 1.3 

46.2 47.9 0.5 23.5 0.6 

27.6 27.7 1.0 27.7 0.1 

58.3 55.9 1.0 57.1 1.7 

69.6 68.7 1.0 69.2 0.7 

HPLC-EC (Height) 13 09/17/01 S13:3 (682B) 

HPLC-EC (Height) 13 09/17/01 S13:4 (179B) 

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

Micronutrients Measurement Quality Assurance Program 

National Institute of Standards and Technology 

100 Bureau Drive Stop 8392 

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Individualized Report 
 

oncor e,

 

 

Set 1 of 18 

Vitamin C "Round Robin" 13 Report: Participant VC-MA 

Total Ascorbic Acid 

[Total Ascorbic Acid], μmol/L 

11-Ctrl12-Ctrl13-Ctrl

S11:1S12:1S13:1S11:2S12:2S13:2S13:3S13:4 

Your [Total Ascorbic Acid], μmol/L

Median [Total Ascorbic Acid], μmol/L 

Apparent Precision, SD 

C danc SD 

You, RR 13 

You, RR 11-12 

NIST, RR 13 

Others, RR 11-12 

1st Quartile (25%) 

Median (50%) 

3rd Quartile (75%) 

For details of the construction and interpretation of these plots, see: 

Duewer, Kline, Sharpless, Brown Thomas, Gary, Sowell. Anal Chem May 1, 1999. 

Sample Comments 

Ctrl Nominal 100 mg/L (56 μmol/mL) standard "control" solution prepared by participant from solid 

ascorbic acid provided by NIST. These data are not used in the target-plot calculations. 

S13:1 SRM 970 Level I 

S13:2 SRM 970 Level II 

S13:3 Serum 682B, prepared 3/1995. NIST's and the last-distributed RR samples of this serum assayed

 much higher than the historical value. These data are not used in the target-plot calculations. 

S13:4 Serum 179B, prepared 4/1993. 

Individualized Report page 2 / 2 

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