NIST Micronutrients Measurement Quality Assurance ... of our analysis of the overall results that...

NISTIR 7880-11

NIST Micronutrients Measurement Quality Assurance Program

Winter 2007 Comparability Studies

Results for Round Robin LXI Fat-Soluble Vitamins and Carotenoids in Human Serum

and Round Robin 26 Ascorbic Acid in Human Serum

David L. Duewer Jeanice B. Thomas

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http://dx.doi.org/10.6028/NIST.IR.7880-11

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NISTIR 7880-11

NIST Micronutrients Measurement Quality Assurance Program

Winter 2007 Comparability Studies

Results for Round Robin LXI Fat-Soluble Vitamins and Carotenoids in Human Serum

and Round Robin 26 Ascorbic Acid in Human Serum

David L. Duewer Jeanice B. Thomas

Chemical Sciences Division Materials Measurement Laboratory

April, 2013

U.S. Department of Commerce Rebecca Blank, Acting Secretary

National Institute of Standards and Technology Patrick D. Gallagher, Under Secretary of Commerce for Standards and Technology and Director

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http://dx.doi.org/10.6028/NIST.IR.7880-11

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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 2007 MMQAP measurement comparability improvement studies: 1) Round Robin LXI Fat-Soluble Vitamins and Carotenoids in Human Serum and 2) Round Robin 26 Total Ascorbic Acid in Human Serum. The materials for both studies were shipped to participants in November 2006; participants were requested to provide their measurement results by March 5, 2007.

Keywords

Human SerumRetinol, α-Tocopherol, γ-Tocopherol, Total and Trans-β-Carotene

Total Ascorbic Acid

iii

Table of Contents

Abstract............................................................................................................................................... iiiKeywords ............................................................................................................................................ iiiTable of Contents ............................................................................................................................... ivIntroduction......................................................................................................................................... 1Round Robin LXI: Fat-Soluble Vitamins and Carotenoids in Human Serum ............................ 1Round Robin 26: Vitamin C in Human Serum............................................................................... 2References ............................................................................................................................................ 3

Appendix A. Shipping Package Inserts for RR61........................................................................ A1Appendix B. Final Report for RR61 .............................................................................................. B1 Appendix C. “All-Lab Report” for RR61 ...................................................................................... C1Appendix D. Representative “Individualized Report” for RR61 ............................................... D1Appendix E. Shipping Package Inserts for RR26 ......................................................................... E1Appendix F. Final Report for RR26............................................................................................... F1Appendix G. “All-Lab Report” for RR26..................................................................................... G1Appendix H. Representative “Individualized Report” for RR26............................................... H1

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, alpha-tocopherol, 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 LXI: Fat-Soluble Vitamins and Carotenoids in Human Serum

Participants in the MMQAP Fat-Soluble Vitamins and Carotenoids in Human Serum Round Robin LXI comparability study (hereafter referred to as RR61) received one lyophilized and four 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 November 2006. 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 RR61 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 all analytes reported by at least five participants. 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 26: Vitamin C in Human Serum

Participants in the MMQAP Vitamin C in Human Serum Round Robin 26 comparability study (hereafter referred to as RR26) received four frozen serum test samples, one frozen control serum, 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 November 2006. The communication materials included in the sample shipment are provided in Appendix E.

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 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 RR26 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 F.

• The “All-Lab Report” that summarizes all of the reported measurement results and provides several consensus statistics. This report is reproduced as Appendix G.

• 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 H.

2

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 RR61

The following three items were included in each package shipped to an RR61 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.

A1

UNITED STATES DEPARTMENT OF COMMERCE National Institute of Standards and Technology Gaithersburg, Maryland 20899-

November 8, 2006

Dear Colleague:

Enclosed are the samples (Sera 329-333) for the first fat-soluble vitamins and carotenoids in serum round robin study (Round Robin LXI) for the fiscal year (FY) 07 NIST Micronutrients M.e~surement Quality Assurance Program. You will find one vial of each of four liquid-frozen and one lyophilized serum samples for analysis along with a form for reporting your results. When reporting your results, please submit one value for each'analyte for a given serum sample. If a value is obtained below your limit of quantification, please indicate this result on the form by using NQ (Not Quantified). Results are due to NIST by March 5, 2007. Results received more than two weeks after the due date will not be included in the summary report for this round robin study.

Lyophilized samples should be reconstituted with 1.0 mL of HPLC-grade water or equivalent. We recommend that dissolution be facilitated with 3 to 5 min agitation in an ultrasonic bath or at least 30 min at room temperature with int~rmittent swirling. (CAUTION: Vigorous shaking will cause foaming and possibly interfere with accurate measurement. The rubber stopper contains phthalate esters that may 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. Water should not be added to the liquid-frozen samples (Sera 329-332).

For consistency, we request that laboratories use the following absorptivities (dL/g.cm): retinal, 1843 at 325 nm (ethanol); retinyl palmitate, 975 at 325 nm (ethanol); a-tocopherol, 75.8 at 292 nm (ethanol); ytocopherol, 91.4 at 298 nm (ethanol); a-carotene, 2800 at 444 nm (hexane); P-carotene, 2560 at 450 nm (ethanol), 2592 at 452 nm (hexane); lycopene, 3450 at 472 nm (hexane).

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

Micronutrients Measurement Quality Assurance Program NIST 100 Bureau Drive Stop 8392 Gaithersburg, MD ~0899-8392 Fax: (301) 977-0685

If you have questions or comments regarding this study, please call me at (301) 975-3120; e-mail me at '[email protected]; or mai fax queries to_t hove address.

.~ Brown Thomas

ch Chemist ical Chemistry Division

· Chemical Science and Technology Laboratory

Enclosures

. ·r

NISI A2

Participant #: ________ Date: _____________

Round Robin LXI: Human Sera NIST Micronutrients Measurement Quality Assurance Program

Analyte 329 330 331 332 333 Units* total retinol

trans-retinol didehydroretinol retinyl palmitate

α-tocopherol γ/β-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 total coenzyme Q10

ubiquinol (QH2) ubiquinone (Qox)

phylloquinone (K1) 25-hydroxyvitamin D

Other measurands?

* we prefer µg/mL Were the liquid frozen samples #329, 330, 331, and 332 frozen when received? Yes | No

Comments:

Mail: M2QAP NIST, Stop 8392 Please return results before Fax: 301-977-0685 Gaithersburg, MD 20899-8392 5-Mar-2007 Email: [email protected]

A3

mailto:[email protected]


Fat-Soluble Vitamins Round Robin LXI NIST Micronutrients Measurement Quality Assurance Program

Packing List and Shipment Receipt Confirmation Form

This box contains: one vial each of the following five FSV M2QAP sera

Serum Form Reconstitute? #329 #330 #331 #332 #333

Liquid frozen Liquid frozen Liquid frozen Liquid frozen Lyophilized

No No No No

Yes (1 ml H2O)

Please 1) Open the pack immediately 2) Check that it contains all of the above samples 3) Check if the vials are intact 4) Store the sera 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 [email protected])

1) Date this shipment arrived: ___________________________ 2) Are all five sera vials intact? Yes | No

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

3) Was there any dry-ice left in cooler? Yes | No 4) Did the liquid frozen samples arrive frozen? Yes | No 5) At what temperature are you storing the serum samples? _______ ˚C 6) When do you anticipate analyzing these samples? ________________________

Your prompt return of this information is appreciated.

The M2QAP Gang

Mail: M2QAP NIST, Stop 8392 Fax: 301-977-0685 Gaithersburg, MD 20899-8392 Email: [email protected]

A4



Appendix B. Final Report for RR61

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 their previous distributions,

if any, and o summarizes aspects of the study that we believe may be of interest to the

participants.

B1

April 26, 2007

Dear Colleague:


Enclosed is the summary report of the results for round robin LXI (RR6 I) of the 2007 NIST Micronutrients Measurement Quality Assurance Program (M2QAP) for the fat-soluble vitamins and carotenoids in human serum. Included in this report are: l) a summary of data and measurement comparability scores for all laboratories, 2) a detailed graphical analysis of your results; and 3) a graphical summary of your measurement comparability.

Data for evaluating laboratory performance in RR6 l are provided in text "Score Card" summary, page 7 of the All Lab Report. Laboratory comparability is summarized as follows: results rated 1 to 3 are within 1 to 3 standard deviations of the assigned value, respectively; those rated 4 are >3 standard deviations from the assigned value. Similar information is presented in the graphical "target plot" summary, last

· page of your Individualized Report.

If you have concerns regarding your laboratory's performance, we suggest that you obtain and analyze a unit ofSRM 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.

Samples for the second 2007 QA interlaboratory exercise will be shipped starting the week of June 4, 2007. We will send you a reminder via e-mail or fax a week prior to shipment. It is critical that you carefully inspect all samples upon arrival and that you promptly confirm to us that they have arrived. We will replace samples (lost or damaged in shipment or miss-packaged by us) only for participants who report the problem within one calendar week after the package arrives.

We look forward to meeting with you at the Micronutrients Measurement Quality Assurance Workshop that is being held in conjunction with the Experimental Biology meeting on May 2, 2007 at the Convention Center in Washington, DC.

If you have any questions regarding this report, please contact Dave Duewer at [email protected] or me [email protected], tel: 301/975-3120, or fax: 301/977-0685.

~ i' e Brown Thomas ~ rch Chemist

A a ical Chemistry Division Chemical Science and Technology Laboratory

Cc: L.C. Sander D.L. Duewer

N•Si B2

The NIST M2QAP Round Robin LXI (RR61) report consists of:

Page “All Lab” Report 1-5 A listing of all results and statistics for all analytes. 6 A legend for the list of results and statistics. 7 The text Comparability Summary (“Score Card”) of measurement performance.

Page “Individualized” Report 1 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 8 other participants.

n+1 The graphical Comparability Summary (target plot) of measurement performance.

Samples. The five sera below were distributed in RR61.

Serum

329

330

331

332

333

Description

Fresh-frozen, native, single-donor serum prepared in Spring, 2006.

Fresh-frozen, a 15:16 blend of the #329 and #331 sera (i.e., #330 = (15×#324 + 16×#326)/31, prepared in Spring, 2006.

Fresh-frozen, native, single-donor serum prepared in Spring, 2006.

Fresh-frozen, native, single-donor, commercially obtained serum prepared in 2002. The same material was used to prepare #333.

Lyophilized, native, single-donor, commercially obtained serum prepared in 2002. The same material was used to prepare #332.

Prior Distributions

#326:RR60-9/06

#292:RR53-2/03, #301:RR55-3/04, #313:RR57-3/05, #323:RR59-3/06

#290:RR53-2/03, #300:RR55-3/04, #312:RR57-3/05, #322:RR59-3/06

Results

1) Sera Stability. There was no significant change in the median level or variability of any measurand in either the fresh-frozen or lyophilized serum of the {332, 333} pair. These materials have been in --80 °C storage for more than four years. The stability of the fresh-frozen material in this and other sera pairs provides strong support for continued use of fresh-frozen rather than lyophilized materials in this program.

2) Measurand Additivity. Serum 330 was prepared as a mixture of two native, single-donor sera. Using the correct method of analysis, the median values in Serum 325 are as expected from the Sera 329 and 331 medians and their 15:16 blending ratio. (Previous additivity studies were incorrectly analyzed. The curved lines connecting the three sera in the current graphs are correct for reporting results on a logarithmic y-axis. This topic will be discussed in more detail at the Workshop.)

B3

3) Report of Unusual Performance of High-purity Retinol Standards. Our colleague Fernando Granado-Lorencio, Hospital Universitario Puerta de Hierro (Madrid), reports unusually high chromatographic response per ng injected for recently purchased high-purity retinol standards from Sigma. The new material appears to be of about 20% higher purity than the older material. Similar behavior was noted by other members of the European Standardization Methods Committee during their revision of a candidate reference method for vitamin A in foods.

B4

Appendix C. “All-Lab Report” for RR61

The following eight 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

Rou

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LXI

Lab

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Res

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Al

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in µ

g/m

L

Tota

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tra

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Ret

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Pal

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α-To

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C2

Lab

329

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331

332

333

329

330

331

332

333

329

330

331

332

333

329

330

331

332

333

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24.4

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8.66

10

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0.

485

0.38

8 0.

284

0.62

8 0.

617

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3 25

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16.3

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0.51

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0.30

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0.61

9 FS

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536

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4 0.

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0.69

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24.5

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0 7.

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8.

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N

32

32

32

32

32

5 5

5 5

5 10

9

9 10

10

33

33

33

33

33

M

in

0.32

9 0.

309

0.25

1 0.

550

0.47

1 0.

462

0.34

0 0.

274

0.58

8 0.

557

0.03

6 0.

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0.00

7 0.

077

0.07

3 19

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13.1

0 7.

10

9.10

5.

80

Med

ian

0.52

0 0.

399

0.30

4 0.

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0.61

8 0.

510

0.36

6 0.

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0.64

7 0.

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0.05

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0.09

8 23

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15.3

9 8.

50

10.5

0 9.

98

Max

0.

602

0.47

1 0.

352

0.78

9 0.

765

0.60

0 0.

430

0.38

0 0.

730

0.68

0 0.

106

0.08

4 0.

070

0.26

0 0.

230

28.5

8 17

.63

10.3

4 12

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11.6

9 SD

0.

042

0.03

5 0.

029

0.04

3 0.

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0.02

6 0.

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0.01

0 0.

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0.01

8 1.

56

0.98

0.

51

0.62

0.

77

CV

8 9

10

7 6

45

54

87

19

19

7 6

6 6

8

Npa

st

0 0

32

33

34

0 0

5 7

7 0

0 8

12

12

0 0

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36

37

Med

ianp

ast

0.30

9 0.

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0.60

5 0.

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0.64

3 0.

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3 8.

32

10.3

9 9.

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SDpa

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0.02

3 0.

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0.04

4 0.

000

0.02

0 0.

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0.03

0 0.

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0.01

9 0.

58

0.66

0.

68

NAV

N

AU

0.52

0 0.

399

0.30

4 0.

646

0.61

8 0.

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0.03

5 0.

029

0.05

1 0.

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0.48

9 0.

378

0.29

8 0.

622

0.60

7 0.

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0.03

5 0.

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0.05

1 0.

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0.05

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0.01

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0.02

6 0.

026

23.6

9 15

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8.50

10

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9.98

1.

89

1.19

0.

68

0.82

0.

78

All L

ab R

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Rou

nd R

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LXI

Lab

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Res

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Al

l Res

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in µ

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L

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Toco

pher

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δ-To

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To

tal β

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C3

Lab

329

330

331

332

333

329

330

331

332

333

329

330

331

332

333

329

330

331

332

333

FSV-

BA

1.06

2.

569

3.83

1.

94

1.87

0.

065

0.06

5 0.

079

0.06

4 0.

052

0.58

0 0.

351

0.15

8 0.

132

0.12

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548

0.33

0 0.

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0.12

6 0.

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FSV-

BB

0.90

2.

325

3.54

1.

74

1.67

0.

045

0.03

8 0.

059

0.03

7 0.

032

0.53

3 0.

306

0.13

0 0.

106

0.10

9 0.

507

0.29

2 0.

124

0.10

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104

FSV-

BC

FSV-

BD

FSV-

BE

1.10

2.

743

4.33

2.

06

1.95

0.

528

0.35

6 0.

169

0.13

4 0.

106

FS

V-BF

0.

81

2.34

0 3.

54

1.79

1.

77

0.43

6 0.

272

0.12

1 0.

102

0.09

3 FS

V-BG

0.

86

2.63

0 4.

07

2.14

1.

98

0.67

4 0.

410

0.17

9 0.

172

0.17

7 FS

V-BH

0.

67

2.18

1 3.

16

1.57

1.

53

0.58

0 0.

362

0.14

5 0.

119

0.11

6 0.

548

0.34

4 0.

145

0.11

9 0.

116

FSV-

BI

0.91

2.

380

3.71

1.

95

1.82

0.

544

0.31

3 0.

139

0.11

1 0.

108

FS

V-BJ

0.

94

2.57

3 3.

84

1.76

1.

72

0.61

7 0.

359

0.12

8 0.

130

0.12

6 FS

V-BK

FS

V-BL

FS

V-BM

FS

V-BN

0.

69

2.04

1 3.

01

1.52

1.

48

0.49

1 0.

323

0.13

6 0.

113

0.10

9 0.

453

0.30

0 0.

127

0.10

8 0.

103

FSV-

BO

0.90

2.

400

3.60

1.

70

1.60

0.

573

0.35

8 0.

177

0.16

5 0.

114

0.50

0 0.

309

0.15

0 0.

139

0.11

4 FS

V-BQ

FS

V-BR

FS

V-BS

1.

24

2.38

7 3.

45

1.80

1.

84

≥0.5

54 ≥0

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0.

554

0.34

5 0.

167

0.13

4 0.

129

FSV-

BT

0.86

2.

021

3.12

1.

52

1.49

0.

381

0.28

4 0.

282

0.28

2 0.

289

0.52

0 0.

336

0.13

6 0.

135

0.13

5 0.

488

0.31

7 0.

129

0.12

9 0.

129

FSV-

BU

1.05

2.

690

4.26

2.

04

2.25

0.

466

0.27

8 0.

097

0.12

6 0.

110

FSV-

BV

0.83

2.

181

3.46

1.

71

1.60

0.

584

0.33

7 0.

160

0.12

1 0.

114

FSV-

BW

1.24

3.

470

5.41

2.

50

2.39

0.

520

0.34

0 0.

160

0.14

0 0.

130

FSV-

BX

1.01

2.

475

3.56

1.

77

1.72

≥0

.527

≥0

.307

≥0

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≥0

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≥0

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0.

527

0.30

7 0.

139

0.11

9 0.

110

FSV-

CC

FS

V-C

E 0.

780

0.44

0 0.

150

0.22

0 0.

040

FSV-

CF

FSV-

CG

0.

88

2.55

7 3.

90

1.92

1.

82

0.20

9 0.

260

0.29

6 0.

159

0.12

1 0.

548

0.32

2 0.

143

0.11

7 0.

115

0.50

7 0.

298

0.13

3 0.

110

0.10

8 FS

V-C

I 0.

80

2.34

9 4.

12

1.82

1.

69

≥0.4

80 ≥0

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≥0

.150

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≥0

.139

0.

480

0.31

6 0.

150

0.13

4 0.

139

FSV-

CS

1.23

3.

033

4.05

2.

30

2.08

0.

556

0.31

0 0.

131

0.13

6 0.

107

FSV-

CW

1.

25

2.69

0 3.

80

2.10

2.

00

0.05

0 0.

080

0.12

0 0.

080

0.07

0 ≥0

.531

≥0

.284

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.141

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.138

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.134

0.

531

0.28

4 0.

141

0.13

8 0.

134

FSV-

CZ

0.69

3 0.

396

0.15

3 0.

180

0.17

1 FS

V-D

D

FSV-

DF

FSV-

DI

0.90

2.

430

3.63

1.

84

1.78

0.

033

0.04

8 0.

061

0.04

2 0.

042

0.49

8 0.

315

0.14

9 0.

113

0.11

1 FS

V-D

V FS

V-EE

N

M

in

Med

ian

Max

SD

C

V

Npa

st

Med

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SDpa

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NAV

N

AU

21

0.67

0.

90

1.25

0.

15

17 0

21

2.02

1 2.

430

3.47

0 0.

215 9 0

21

3.01

3.

71

5.41

0.

38

10

24

3.62

0.

24

21

1.52

1.

82

2.50

0.

22

12

22

1.83

0.

14

21

1.48

1.

78

2.39

0.

21

12

22

1.74

0.

11

6 0.

033

0.05

8 0.

381

0.09

4 16

4 0

6 0.

038

0.07

3 0.

284

0.12

1 16

7 0

6 0.

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0.10

0 0.

296

0.13

1 13

1 5 0.

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4

6 0.

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2 0.

282

0.06

8 95 6

0.06

3 0.

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1 0.

289

0.04

7 78 6

0.06

7 0.

023

19

0.43

6 0.

548

0.78

0 0.

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19

0.27

2 0.

337

0.44

0 0.

033 10 0

19

0.09

7 0.

145

0.17

9 0.

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26

0.14

7 0.

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19

0.10

2 0.

130

0.22

0 0.

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26

0.12

0 0.

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19

0.04

0 0.

114

0.17

7 0.

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26

0.11

4 0.

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11

0.45

3 0.

507

0.55

4 0.

034 7 0

11

11

11

11

0.28

4 0.

124

0.10

2 0.

103

0.30

9 0.

141

0.12

6 0.

116

0.34

5 0.

167

0.13

9 0.

139

0.01

8 0.

013

0.01

5 0.

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6 10

12

13

0 8

11

11

0.12

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116

0.10

9 0.

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0 0.

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0.90

2.

43

3.71

1.

82

1.78

0.

15

0.24

0.

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0.22

0.

21

0.05

8 0.

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0.10

0 0.

072

0.06

1 0.

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0.12

1 0.

131

0.06

8 0.

047

0.54

8 0.

337

0.14

5 0.

130

0.11

4 0.

076

0.04

9 0.

023

0.02

1 0.

019

0.50

7 0.

309

0.14

1 0.

126

0.11

6 0.

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0.03

3 0.

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0.01

5 0.

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All L

ab R

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Rou

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LXI

Lab

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Res

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Al

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l cis

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Tota

l α-C

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Tota

l Lyc

open

e tra

ns-L

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Lab

329

330

331

332

333

C4

FSV-

BA

0.03

3 0.

021

0.01

0 0.

006

0.00

6 FS

V-BB

0.

026

0.01

3 0.

005

0.00

4 0.

005

FSV-

BC

FSV-

BD

FSV-

BE

FSV-

BF

FSV-

BG

FSV-

BH

0.03

2 0.

018

na

na

na

FSV-

BI

FSV-

BJ

FSV-

BK

FSV-

BL

FSV-

BM

FSV-

BN

0.04

0 0.

026

0.01

2 0.

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0.00

9 FS

V-BO

0.

073

0.04

8 0.

026

0.02

6 nd

FS

V-BQ

FS

V-BR

FS

V-BS

FS

V-BT

0.

027

0.01

7 0.

007

0.00

5 0.

005

FSV-

BU

FSV-

BV

FSV-

BW

FSV-

BX

FSV-

CC

FS

V-C

E FS

V-C

F FS

V-C

G

0.04

1 0.

024

0.01

0 0.

007

0.00

7 FS

V-C

I FS

V-C

S FS

V-C

W

FSV-

CZ

FSV-

DD

FS

V-D

F FS

V-D

I FS

V-D

V FS

V-EE

329

330

331

332

333

0.31

6 0.

154

0.01

6 0.

084

0.08

2 0.

284

0.13

4 0.

013

0.06

8 0.

069

0.35

3 0.

155

0.01

4 0.

087

0.08

9 0.

292

0.14

6 0.

022

0.09

3 0.

091

0.31

9 0.

160

0.01

0 0.

078

0.07

7 0.

304

0.14

5 0.

016

0.07

5 0.

070

0.40

4 0.

172

0.01

2 0.

089

0.09

2

0.29

0 0.

151

0.01

4 0.

080

0.07

8 0.

325

0.16

2 0.

017

0.10

5 0.

089

0.35

3 0.

187

0.04

6 0.

113

0.10

9 0.

225

0.13

2 0.

021

0.08

3 0.

080

0.29

9 0.

138

0.01

8 0.

082

0.07

0 0.

394

0.16

1 0.

014

0.08

7 0.

082

0.26

0 0.

130

0.01

0 0.

060

0.05

2 ≥0

.285

≥0

.140

≥0

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≥0

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≥0

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0.36

5 0.

173

0.30

2 0.

180

0.32

7 0.

148

0.34

8 0.

143

0.24

7 0.

126

0.01

8 0.

092

0.09

1 0.

055

0.12

0 0.

113

0.01

2 0.

094

0.07

7 0.

007

0.08

3 0.

082

0.05

5 0.

094

0.09

0

329

330

331

332

333

0.26

2 0.

427

0.57

7 0.

507

0.48

6 0.

263

0.41

6 0.

550

0.48

6 0.

468

0.26

1 0.

421

0.59

3 0.

541

0.49

4 0.

300

0.53

4 0.

654

0.63

1 0.

626

0.28

0 0.

499

0.63

6 0.

566

0.56

3 0.

228

0.37

4 0.

487

0.43

8 0.

389

0.26

9 0.

421

0.53

7 0.

508

0.48

3

0.23

6 0.

445

0.54

2 0.

494

0.48

9 0.

307

0.49

0 0.

737

0.71

0 0.

525

0.30

6 0.

496

0.65

8 0.

552

0.53

1 0.

228

0.41

2 0.

513

0.49

8 0.

470

0.26

1 0.

410

0.33

2 0.

508

0.42

6 0.

293

0.47

5 0.

634

0.55

9 0.

508

0.26

0 0.

480

0.72

0 0.

690

0.64

0

0.29

1 0.

455

0.59

2 0.

502

0.49

6

0.30

1 0.

433

0.56

9 0.

601

0.52

2

0.27

8 0.

447

0.58

3 0.

537

0.51

9

329

330

331

332

333

0.12

1 0.

231

0.32

7 0.

300

0.28

6 0.

096

0.19

0 0.

269

0.24

7 0.

234

0.13

3 0.

261

0.33

8 0.

337

0.33

9

0.10

0 0.

225

0.29

0 0.

274

0.26

4

0.08

5 0.

159

0.23

3 0.

250

0.22

9

0.11

9 0.

223

0.31

7 0.

283

0.27

7

0.10

0 0.

148

0.19

5 0.

205

0.19

9

N

7 7

6 6

5 19

19

19

19

19

17

17

17

17

17

7

7 7

7 7

Min

0.

026

0.01

3 0.

005

0.00

4 0.

005

0.22

5 0.

126

0.00

7 0.

060

0.05

2 0.

228

0.37

4 0.

332

0.43

8 0.

389

0.08

5 0.

148

0.19

5 0.

205

0.19

9 M

edia

n 0.

033

0.02

1 0.

010

0.00

7 0.

006

0.31

6 0.

151

0.01

6 0.

087

0.08

2 0.

269

0.44

5 0.

583

0.53

7 0.

496

0.10

0 0.

223

0.29

0 0.

274

0.26

4 M

ax

0.07

3 0.

048

0.02

6 0.

026

0.00

9 0.

404

0.18

7 0.

055

0.12

0 0.

113

0.30

7 0.

534

0.73

7 0.

710

0.64

0 0.

133

0.26

1 0.

338

0.33

7 0.

339

SD

0.00

8 0.

006

0.00

3 0.

002

0.00

1 0.

044

0.01

5 0.

005

0.00

9 0.

010

0.02

4 0.

044

0.07

0 0.

047

0.03

1 0.

016

0.04

0 0.

053

0.03

2 0.

037

CV

25

27

28

37

25

14

10

32

11

12

9 10

12

9

6 16

18

18

12

14

Npa

st

0 0

5 6

6 0

0 19

22

22

0

0 22

22

22

0

0 7

9 9

Med

ianp

ast

0.00

9 0.

007

0.00

7 0.

017

0.07

9 0.

074

0.58

7 0.

506

0.47

9 0.

306

0.26

2 0.

247

SDpa

st

0.00

6 0.

002

0.00

3 0.

004

0.01

2 0.

012

0.05

6 0.

067

0.05

9 0.

045

0.05

1 0.

046

NAV

0.

033

0.02

1 0.

010

0.00

7 0.

006

0.31

6 0.

151

0.01

6 0.

087

0.08

2 0.

269

0.44

5 0.

583

0.53

7 0.

496

0.10

0 0.

223

0.29

0 0.

274

0.26

4 N

AU

0.01

2 0.

007

0.00

4 0.

003

0.00

3 0.

080

0.04

1 0.

006

0.02

5 0.

024

0.06

2 0.

094

0.11

7 0.

110

0.10

3 0.

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0.04

0 0.

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0.05

0 0.

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All L

ab R

epor

t Pa

ge 3

/ 8

Rou

nd R

obin

LXI

Lab

orat

ory

Res

ults

Al

l Res

ults

in µ

g/m

L

Tota

l β-C

rypt

oxan

thin

To

tal α

-Cry

ptox

anth

in

Tota

l Lut

ein

Tota

l Zea

xant

hin

C5

Lab

329

330

331

332

333

329

330

331

332

333

329

330

331

332

333

329

330

331

332

333

FSV-

BA

0.10

5 0.

121

0.12

8 0.

067

0.06

4 0.

021

0.03

6 0.

045

0.02

9 0.

028

FSV-

BB

0.09

3 0.

100

0.10

4 0.

057

0.05

4 0.

021

0.02

9 0.

035

0.02

6 0.

025

0.16

1 0.

150

0.15

4 0.

082

0.08

3 0.

026

0.05

6 0.

073

0.04

1 0.

045

FSV-

BC

FSV-

BD

FSV-

BE

FSV-

BF

0.09

1 0.

095

0.10

0 0.

050

0.04

5 FS

V-BG

0.

110

0.12

0 0.

127

0.07

4 0.

070

0.15

7 0.

142

0.12

8 0.

098

0.09

5 0.

028

0.02

9 0.

031

0.03

0 0.

026

FSV-

BH

0.11

9 0.

135

0.13

0 0.

065

0.06

1 0.

113

0.10

9 0.

100

0.05

7 0.

057

0.02

3 0.

054

0.07

0 0.

030

0.02

8 FS

V-BI

0.

100

0.10

6 0.

111

0.05

7 0.

052

0.13

9 0.

132

0.12

3 0.

081

0.07

5 0.

026

0.04

7 0.

062

0.03

1 0.

031

FSV-

BJ

0.10

5 0.

108

0.10

5 0.

053

0.04

8 0.

152

0.14

9 0.

146

0.08

7 0.

083

FSV-

BK

FSV-

BL

FSV-

BM

FSV-

BN

0.07

9 0.

097

0.09

9 0.

051

0.04

9 0.

013

0.02

6 0.

033

0.02

2 0.

021

0.15

7 0.

174

0.16

7 0.

100

0.09

4 0.

032

0.10

7 0.

151

0.04

1 0.

040

FSV-

BO

0.10

3 0.

112

0.12

6 0.

066

0.05

4 0.

199

0.20

1 0.

200

0.10

5 0.

103

0.03

0 0.

055

0.07

7 0.

022

0.03

0 FS

V-BQ

FS

V-BR

FS

V-BS

0.

138

0.13

2 0.

184

0.09

6 0.

010

FS

V-BT

0.

087

0.08

6 0.

092

0.05

1 0.

050

0.02

3 0.

027

0.03

3 0.

025

0.02

4 0.

123

0.12

6 0.

138

0.05

9 0.

055

0.04

3 0.

040

0.04

2 0.

026

0.02

5 FS

V-BU

0.

076

0.07

9 0.

062

0.05

7 0.

055

FSV-

BV

0.07

2 0.

074

0.07

8 0.

037

0.03

5 FS

V-BW

FS

V-BX

0.

074

0.07

9 0.

088

0.04

8 0.

045

0.15

9 0.

154

0.15

9 0.

082

0.07

7 0.

022

0.03

8 0.

052

0.02

7 0.

028

FSV-

CC

FS

V-C

E FS

V-C

F FS

V-C

G

0.13

3 0.

142

0.15

0 0.

078

0.07

8

FSV-

CI

0.16

1 0.

190

0.19

1 0.

100

0.09

3 0.

030

0.05

4 0.

068

0.03

7 0.

033

FSV-

CS

0.08

2 0.

081

0.08

6 0.

054

0.04

7 0.

122

0.11

5 0.

116

0.07

2 0.

061

0.02

6 0.

043

0.06

6 0.

042

0.03

9 FS

V-C

W

0.09

7 0.

098

0.09

3 0.

055

0.05

2 0.

170

0.15

1 0.

147

0.09

6 0.

092

0.02

2 0.

035

0.04

1 0.

027

0.02

5 FS

V-C

Z FS

V-D

D

FSV-

DF

FSV-

DI

0.14

9 0.

166

0.17

9 0.

090

0.08

5 FS

V-D

V FS

V-EE

N

M

in

Med

ian

Max

SD

C

V

Npa

st

Med

ianp

ast

SDpa

st

NAV

N

AU

17

0.07

2 0.

097

0.13

8 0.

017 18 0

17

0.07

4 0.

100

0.14

2 0.

025 25 0

17

0.06

2 0.

104

0.18

4 0.

026 25

23

0.11

2 0.

027

17

0.03

7 0.

057

0.09

6 0.

011 19

22

0.05

5 0.

009

17

0.01

0 0.

052

0.07

8 0.

006 11

22

0.05

2 0.

008

4 0.

013

0.02

1 0.

023

0.00

2 9 0

4 0.

026

0.02

8 0.

036

0.00

3 11 0

4 0.

033

0.03

4 0.

045

0.00

3 10 4

0.04

0 0.

004

4 0.

022

0.02

6 0.

029

0.00

2 7 5 0.

027

0.00

7

4 0.

021

0.02

5 0.

028

0.00

2 8 7 0.

024

0.00

7

13

0.11

3 0.

157

0.19

9 0.

016 10 0

13

0.10

9 0.

150

0.20

1 0.

025 17 0

13

0.10

0 0.

147

0.20

0 0.

029 20

14

0.14

5 0.

042

13

0.05

7 0.

087

0.10

5 0.

013 15

15

0.08

0 0.

015

13

0.05

5 0.

083

0.10

3 0.

013 16

15

0.07

8 0.

015

11

0.02

2 0.

026

0.04

3 0.

004 16 0

11

11

11

11

0.02

9 0.

031

0.02

2 0.

025

0.04

7 0.

066

0.03

0 0.

030

0.10

7 0.

151

0.04

2 0.

045

0.01

2 0.

018

0.00

9 0.

007

25

27

29

23

0 11

13

13

0.

057

0.03

2 0.

030

0.01

8 0.

007

0.00

7

0.09

7 0.

100

0.10

4 0.

057

0.05

2 0.

022

0.02

5 0.

026

0.01

4 0.

013

0.02

1 0.

028

0.03

4 0.

026

0.02

5 0.

157

0.15

0 0.

147

0.08

7 0.

083

0.02

9 0.

027

0.02

9 0.

017

0.01

6 0.

026

0.04

7 0.

066

0.03

0 0.

030

0.00

7 0.

013

0.01

8 0.

009

0.00

8

All L

ab R

epor

t Pa

ge 4

/ 8

Rou

nd R

obin

LXI

Lab

orat

ory

Res

ults

Al

l Res

ults

in µ

g/m

L

Tota

l Lut

ein&

Zeax

anth

in

Coe

nzym

e Q

10

Ubi

quin

ol

Ubi

quin

one

C6

Lab

329

330

331

332

333

329

330

331

332

333

329

330

331

332

333

329

330

331

332

333

FSV-

BA

0.19

2 0.

220

0.25

2 0.

126

0.11

9 FS

V-BB

0.

187

0.20

6 0.

228

0.12

3 0.

128

FSV-

BC

FSV-

BD

FSV-

BE

FSV-

BF

0.18

0 0.

191

0.19

5 0.

115

0.11

2 FS

V-BG

0.

167

0.15

5 0.

140

0.11

2 0.

105

FSV-

BH

0.13

6 0.

163

0.17

0 0.

087

0.08

5

FSV-

BI

0.16

5 0.

179

0.18

5 0.

112

0.10

6 FS

V-BJ

0.

781

1.11

9 1.

194

0.80

4 0.

740

FSV-

BK

FSV-

BL

FSV-

BM

FSV-

BN

0.18

9 0.

282

0.31

8 0.

141

0.13

4 FS

V-BO

0.

229

0.25

6 0.

277

0.12

6 0.

133

FSV-

BQ

FSV-

BR

FSV-

BS

0.19

1 0.

229

0.25

6 0.

119

0.10

2

FSV-

BT

0.16

4 0.

190

0.20

5 0.

102

0.09

6 FS

V-BU

0.

152

0.16

6 0.

116

0.10

1 0.

093

FSV-

BV

0.20

1 0.

219

0.23

6 0.

127

0.11

8 FS

V-BW

0.

436

0.59

5 1.

032

0.71

5 0.

709

0.17

9 0.

211

0.81

4 0.

528

0.61

9 0.

257

0.38

4 0.

218

0.18

7 0.

090

FSV-

BX

0.18

1 0.

192

0.21

2 0.

109

0.10

5 FS

V-C

C

FSV-

CE

FSV-

CF

FSV-

CG

0.

238

0.26

5 0.

293

0.15

2 0.

149

FS

V-C

I 0.

191

0.24

4 0.

259

0.13

7 0.

126

0.70

0 0.

880

1.10

0 0.

650

0.59

0 FS

V-C

S 0.

148

0.15

8 0.

182

0.11

4 0.

100

FSV-

CW

0.

192

0.18

5 0.

188

0.12

4 0.

117

0.63

0 0.

730

0.82

0 0.

660

0.50

0 FS

V-C

Z 0.

680

0.85

0 0.

960

0.67

0 0.

690

FSV-

DD

FS

V-D

F FS

V-D

I 0.

715

0.94

1 1.

090

0.74

8 0.

727

0.01

0 0.

405

1.26

0 0.

824

0.72

7 0.

780

0.69

5 0.

152

0.18

6 0.

201

FSV-

DV

FSV-

EE

0.72

0 0.

911

1.31

1 0.

754

0.72

6 N

17

17

17

17

17

7

7 7

7 7

2 2

2 2

2 2

2 2

2 2

Min

0.

136

0.15

5 0.

116

0.08

7 0.

085

0.43

6 0.

595

0.82

0 0.

650

0.50

0 0.

010

0.21

1 0.

814

0.52

8 0.

619

0.25

7 0.

384

0.15

2 0.

186

0.09

0 M

edia

n 0.

187

0.19

2 0.

212

0.11

9 0.

112

0.70

0 0.

880

1.09

0 0.

715

0.70

9 0.

095

0.30

8 1.

037

0.67

6 0.

673

0.51

9 0.

540

0.18

5 0.

187

0.14

6 M

ax

0.23

8 0.

282

0.31

8 0.

152

0.14

9 0.

781

1.11

9 1.

311

0.80

4 0.

740

0.17

9 0.

405

1.26

0 0.

824

0.72

7 0.

780

0.69

5 0.

218

0.18

7 0.

201

SD

0.02

0 0.

037

0.05

3 0.

011

0.01

8 0.

046

0.10

1 0.

112

0.06

4 0.

064

CV

11

19

25

9 16

7

11

10

9 9

Npa

st

0 0

22

23

23

0 0

5 5

5 0

0 0

0 0

0 0

0 0

0 M

edia

npas

t 0.

211

0.11

3 0.

108

1.19

0 0.

760

0.69

9 SD

past

0.

056

0.01

7 0.

018

0.06

0 0.

169

0.16

2

NAV

N

AU

0.18

7 0.

192

0.21

2 0.

119

0.11

2 0.

700

0.88

0 1.

090

0.71

5 0.

709

0.03

9 0.

040

0.05

3 0.

025

0.02

3 0.

070

0.10

1 0.

112

0.07

2 0.

071

All L

ab R

epor

t Pa

ge 5

/ 8

Rou

nd R

obin

LXI

Lab

orat

ory

Res

ults

Al

l Res

ults

in µ

g/m

L

Phyl

loqu

inon

e (K

1) x

1000

25

-hyd

roxy

vita

min

D

C7

Lab

329

330

331

332

333

329

330

331

332

333

FSV-

BA

0.01

5 0.

014

0.00

8 0.

020

0.02

0 FS

V-BB

0.

016

0.01

2 0.

010

0.02

0 0.

025

FSV-

BC

FSV-

BD

FSV-

BE

1.58

6 0.

995

0.59

9 0.

389

0.35

7 FS

V-BF

FS

V-BG

FS

V-BH

0.

015

0.01

1 0.

007

0.02

1 0.

020

FSV-

BI

FSV-

BJ

FSV-

BK

FSV-

BL

FSV-

BM

FSV-

BN

0.01

7 0.

011

0.00

8 0.

019

0.01

8 FS

V-BO

FS

V-BQ

FS

V-BR

FS

V-BS

FS

V-BT

FS

V-BU

FS

V-BV

FS

V-BW

FS

V-BX

FS

V-C

C

FSV-

CE

FSV-

CF

FSV-

CG

FS

V-C

I 1.

339

0.88

7 0.

530

0.40

2 0.

308

FS

V-C

S

FSV-

CW

FS

V-C

Z FS

V-D

D

FSV-

DF

FSV-

DI

0.88

0 0.

700

0.50

0 0.

370

0.33

0

FSV-

DV

FS

V-EE

N

33

33

3 4

44

44

Min

0.

880

0.70

0 0.

500

0.37

0 0.

308

0.01

5 0.

011

0.00

7 0.

019

0.01

8 M

edia

n 1.

339

0.88

7 0.

530

0.38

9 0.

330

0.01

5 0.

012

0.00

8 0.

020

0.02

0 M

ax

1.58

6 0.

995

0.59

9 0.

402

0.35

7 0.

017

0.01

4 0.

010

0.02

1 0.

025

SD

0.00

1 0.

001

0.00

1 0.

001

0.00

1 C

V 5

10

7 5

7

Npa

st

0 0

0 0

0 0

0 0

5 4

Med

ianp

ast

0.01

7 SD

past

0.

004

NAV

N

AU

1.33

9 0.

887

0.53

0 0.

389

0.33

0 0.

015

0.01

2 0.

008

0.02

0 0.

020

All L

ab R

epor

t Pa

ge 6

/ 8

Round Robin LXI Laboratory Results All Results in µg/mL

Analytes Reported By One Laboratory

Analyte Code 329 330 331 332 333 Total cis-β-Cryptoxanthin FSV-BT 0.029 0.032 0.036 0.022 0.022

trans-α-Carotene FSV-BX 0.285 0.140 0.021 0.081 0.075

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

Min Minimum (non-NIST) quantitative value reported Medianpart Median (non-NIST) quantitative value reported

Max Maximum (non-NIST) quantitative value reported SD Standard deviation for (non-NIST) results: 0.741*(3rd Quartile - 1st Quartile) CV Coefficient of Variation for (non-NIST) results: 100*SD/Median

Npast Mean of N(s) from past RR(s) Medianpast Mean of Median(s) from past RR(s)

SDpast Pooled SD from past RR(s)

NAV NIST Assigned Value = (Medianpart + MeanNIST)/2 for analytes reported by NIST analyst(s) = Medianpart for analytes reported by ≥ 10 labs but not NIST

NAU NIST Assigned Uncertainty: (S2 + Sbtw 2)0.5

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

- Not analyzed nd Not detected (i.e., no detectable peak for analyte) nq Detected but not quantitatively determined ≤x Concentration at or below the limit of quantification, x ≥x Concentration greater than or equal to x ? Non-quantitative value: extrapolated beyond upper limit of calibration curve * Non-quantitative value: heterogeneous serum, damaged sample, malfunctio

italics Not explictly reported but calculated by NIST from reported values

Legend

All Lab Report Page 7 / 8

C8

Round Robin LXI Laboratory Results

Comparability Summary

Lab FSV-BA FSV-BB FSV-BC 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-BQ FSV-BR FSV-BS FSV-BT FSV-BU FSV-BV

FSV-BW FSV-BX FSV-CC FSV-CE FSV-CF FSV-CG FSV-CI

FSV-CS FSV-CW FSV-CZ FSV-DD FSV-DF FSV-DI

FSV-DV FSV-EE

n

% 1 % 2 % 3 % 4

TR aT g/bT bC tbC aC TLy TbX TLu TZ L&Z 2 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 1 1 1 1 1 3 2 1 1 1 1 2 1 1 1 1 1 2 2 3 1 1 2 1 2 1 2 2 2 1 1 1 1 1 2 1 2 2 1 1 1 1 1 1 1 1 1 1 2 1 1 1 1 1 1 2 1 1 1 1 1 2 1 2 1 1 1 1 1 1 4 2 1 2 1 2 1 1 2 1 2 1 2 2 2 1 2 2 1 2 1 2 3 1 3 1 2 1 2 1 1 1 1 1 2 2 1 3 2 2 2 1 2 1 2 2 1 1 1 1 1 2 1 1 1 4 1 1 2 1 1 1 1 1 1 1 1 1 1 1 1 2 3 4 1 2 1 1 1 1 1 1 1 2 2 1 1 1 1 1 4 2 1 1 2 1 2 1 1 1 1 2 1 1 2 1 2 1 1 1 1 1 1 1 1 1 3 3 2 1 1 1 1 4 1 1 2 2 2 2 36 33 21 23 11 20 17 17 13 11 17

TR aT g/bT bC tbC aC TLy TbX TLu TZ L&Z 53 64 52 74 91 85 82 76 62 64 71 42 30 43 13 9 0 18 18 38 27 29 6 6 0 9 0 5 0 6 0 0 0 0 0 5 4 0 10 0 0 0 9 0

LabelLabTR aT

g/bTbCtbC 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) of summarizes your measurement performance for a given measurand, relative to the consensus medians. CS is the average distance, in standard deviation units, that your measurement performance characteristics are from the consensus performance. CS is calculated when the number of quantitative values you reported for a measurand, Nyou, is at least two and the measurand has been reported by 10 or more participants.

CS = MIN(4, INT(1 + C2 + AP 2 ))

yo uN You − Median C = Concordanc e = i i Ny ou ∑ NAU i i

N You i − Median i 2

AP = Apparent Precision = ∑yo u

(Ny ou − 1)NAU i i

NAU = NIST Assigned Uncertainty, our estimate of the overall measurement standard deviation for each sample. The estimate includes serum heterogeneity, analytical repeatability, and among-participant reproducibility variance components.

For further details, please see: Duewer DL, Kline MC, Sharpless KE, Brown Thomas J, Gary KT. Micronutrients Measurement Quality Assurance Program: Helping participants use interlaboratory comparison exercise results to improve their long-term measurement performance. Anal Chem 1999;71(9):1870-8.

All Lab Report Page 8 / 8

C9

Appendix D. Representative “Individualized Report” for RR61

Each participant in RR61 received an “Individualized Report” reflecting their reported results. Each report included a detailed analysis for analytes that were assayed by at least five participants. The following analytes met this criterion in RR61:

• Total Retinol • trans-Retinol • Retinyl Palmitate • α-Tocopherol • γ/β-Tocopherol • δ-Tocopherol • trans-β-Carotene • Total cis-β-Carotene • Total α-Carotene • Total Lycopene • trans-Lycopene • Total β-Cryptoxanthin • Total Lutein • Total Zeaxanthin • Total Lutein & Zeaxanthin • Coenzyme Q10

The following 14 pages are the “Individualized Report” for the analytes evaluated by participant FSV-BA.

D1

Set 1

of 3

2

Indi

vidu

aliz

ed R

ound

Rob

in L

XI R

epor

t: FS

V-BA

Su

mm

ary

Seru

m 3

29

Seru

m 3

30

Seru

m 3

31

Seru

m 3

32

Seru

m 3

33

D2

Anal

yte

You

NAV

n

You

NAV

n

You

NAV

n

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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.

NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA Total Retinol

[Ana

lyte

], µg

/mL

Your

[Ana

lyte

], µg

/mL

Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Appa

rent

Pre

cisi

on, S

D

Median [Analyte], µg/mL

Long-term Precision, SD Concordance, SD

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

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

1st Quartile (25%) Expectation

Serum History Comments #329 Fresh frozen: New Native, single-source #330 Fresh frozen: New 15:16 blend of #329 and #331 #331 Fresh frozen: 60:#326 Native, single-source #332 Fresh-frozen: 53:#292, 55:#301, 57:#313, 59:#323 Native, same single-source as #333 #333 Lyophilized: 53:#290, 55:#300, 57:#312, 59:#322 Native, same single-source as #332

Individualized Report Page 2 / 14 D3


NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA Retinyl Palmitate

[Ana

lyte

], µg

/mL

Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Your

[Ana

lyte

], µg

/mL

Appa

rent

Pre

cisi

on, S

D


Concordance, SD Long-term Precision, SD







NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA α-Tocopherol

Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Appa

rent

Pre

cisi

on, S

D

[Ana

lyte

], µg

/mL

Your

[Ana

lyte

], µg

/mL









NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA γ/β-Tocopherol

Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Appa

rent

Pre

cisi

on, S

D

[Ana

lyte

], µg

/mL

Your

[Ana

lyte

], µg

/mL









NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA δ-Tocopherol

[Ana

lyte

], µg

/mL

Your

[Ana

lyte

], µg

/mL

Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Appa

rent

Pre

cisi

on, S

D









NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA Total β-Carotene

Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Appa

rent

Pre

cisi

on, S

D

[Ana

lyte

], µg

/mL

Your

[Ana

lyte

], µg

/mL









NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA trans-β-Carotene

Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Appa

rent

Pre

cisi

on, S

D

[Ana

lyte

], µg

/mL

Your

[Ana

lyte

], µg

/mL









NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA Total α-Carotene

Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Appa

rent

Pre

cisi

on, S

D

[Ana

lyte

], µg

/mL

Your

[Ana

lyte

], µg

/mL









NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA Total Lycopene

[Ana

lyte

], µg

/mL

Your

[Ana

lyte

], µg

/mL


Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Appa

rent

Pre

cisi

on, S

D








NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA trans-Lycopene

Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Appa

rent

Pre

cisi

on, S

D

[Ana

lyte

], µg

/mL

Your

[Ana

lyte

], µg

/mL









NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA Total β-Cryptoxanthin

Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Appa

rent

Pre

cisi

on, S

D

[Ana

lyte

], µg

/mL

Your

[Ana

lyte

], µg

/mL









NIST, this RR

Set 1 of 32

Individualized RR LXI Report: FSV-BA Total Lutein&Zeaxanthin

[Ana

lyte

], µg

/mL

Your

[Ana

lyte

], µg

/mL


Appa

rent

Pre

cisi

on, S

D

329

330

331

326

292

301

313

323

332

290

300

312

322

333

Appa

rent

Pre

cisi

on, S

D







Set 1

of 3

2

Indi

vidu

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4

Appendix E. Shipping Package Inserts for RR26

The following five items were included in each package shipped to an RR26 participant: • Cover letter • Protocol for Preparation and Analysis of the Ascorbic Acid Solid Control

Material• Preparation and Validation of Ascorbic Acid Solid Control Material Datasheet • Analysis of Control Materials and Test Samples Datasheet • Packing List and Shipment Receipt Confirmation Form

The cover letter, preparation protocol, and the two datasheets 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

November 8, 2006

Dear Colleague:


The samples within this package constitute the first Vitamin C Round Robin (RR26) of the fiscal year (FY) 07 Micronutrients Measurement Quality Assurance Program. RR26 consists of four vials of frozen serum test samples(# 13, #42, #I I 2, and # 113), one vial of ascorbic acid solid control material, and one vial of SRM 970 Ascorbic Acid in Serum-Level I to be used as the serum control material. Please follow the attached protocols when you prepare and analyze these samples. If you cannot prepare the solid control solutions gravimetrically, please prepare equivalent solutions volumetrically and report the exact volumes used. (Routine 0.5 g gravimetric measurements are generally 10-fold more accurate than routine 0.5 mL volumetric measurements.)

Please use SRM 970 to validate the performance of your measurement system before you analyze the test samples. The target value and ::::95% confidence interval for SRM 970-Level I is 8.41 ± 0.61 µmol/L of sample.

Please be aware that sample contact with any oxidant-contaminated surface (vials, glassware, etc.) may degrade your measurement system's perfonnance (SA Margolis and E Park, "Stability of Ascorbic Acid in Solutions in · Autosampler Vials", Clinical Chemistry 2001, 47(8), 1463-1464). You should suspect such degradation if you observe unusually large variation in replicate analyses,

The report for RR25 was mailed mid-October. If you find your results for _RIUS unsatisfactory, we _ recommend that you obtain Standard Reference Material (SRM) 970 Ascorbic-Acid in Serum to validate your methodology and value assign in-house control materials. This SRM may be purchased from the Standard Materials Reference Program at NIST (Tel: 301-975-6776, Fax: 301-948-3730, or e-mail: [email protected]).

If you have any questions or concerns about the Vitamin C Micronutrients Measurement Quality Assurance Program please contact Jeanice Brown Thomas at tel: 301-975-3120, fax: 301-977-0685, or e-mail: [email protected].

We ask that you return your results for the RR26 samples by March 5, 2007. We would appreciate receiving your results as soon as they become available. Please use the attached form. Your results will be kept confidential.

Brown Thomas ese ch Chemist

ytical Chemistry Division Chemical Science and Technology Laboratory

Enclosures: Protocols, Preparation and Analysis of Control Materials and Analysis of Test Samples . RR26 Report Form for Ascorbic Acid Solid Control Material Preparation RR26 Report Form for Control Material and Test Sample Analyses

N•Si E2

Micronutrient Measurement Quality Assurance Program for Vitamin C

Please Read Through Completely BEFORE Analyzing Samples

Protocol for Preparation and Analysis of the Ascorbic Acid Solid Control Material

The ascorbic acid solid control material (in the amber vial) should be prepared and used in the following manner:

1) Prepare at least 500 mL of 5% mass fraction metaphosphoric acid (MPA) in distilled water. This solution will be referred to as the “Diluent” below.

2) Weigh 0.20 to 0.22 g of the ascorbic acid solid control material to 0.0001 g (if possible), dissolve it in the Diluent in a 100 mL volumetric flask, and dilute with the Diluent to the 100 mL mark. Weigh the amount of Diluent added to 0.1 g. Record the weights. The resulting material will be referred to as the “Stock Solution” below.

3) Prepare three dilute solutions of the Stock Solution as follows:

Dilute Solution 1: Weigh 0.500 mL of the Stock Solution to 0.0001 g into a 100 mL volumetric flask; dilute with Diluent to the 100 mL mark. Record the weight.



4) Calculate and record the total ascorbic acid concentrations, [TAA], in these Dilute Solutions. If you follow the above gravimetric preparation directions, the [TAA] in μmol/L is calculated:

( ) ( ⋅ 56785 mol/g ⋅ L)g Stock Solution in Dilute Solution ⋅ g AA in Stock Solution ) ( µ[TAA] DS = (g AA in Stock Solution ) + (g Diluent in Stock Solution)

For example, if you prepared the Stock Solution with 0.2000 g of solid ascorbic acid and 103.0 g of Diluent, then 0.5 mL of the Stock Solution should weigh (0.2+103)/200 = 0.52 g and [TAA] DS1 = (0.52 g)(0.2 g)∙(56785 μmol/g·L)/(0.2 + 103 g) = 57.2 μmol/L. Likewise, 0.25 mL of the Stock Solution should weigh 0.26 g and [TAA] DS2 = 28.4 μmol/L and 0.125 mL should weigh 0.13 g and [TAA] DS3 = 14.2 μmol/L.

5) Measure the ultraviolet absorbance spectrum of Dilute Solution 1 against the Diluent as the blank using paired 1 cm path length cuvettes. Record the absorbance at 242, 243, 244, and 245 nm. Record the maximum absorbance (Amax ) within this region. Record the wavelength (λmax ) at which this maximum occurs.

The extinction coefficient (E1%) of ascorbic acid at λmax (using a cell with a 1 cm path length) of Dilute Solution #1 can be calculated:

E3

1% dL (A max ) ( ( g AA in Stock Solution ) + (g Diluent in Stock Solution )⋅ )E ( ) =

g ⋅ cm (g Stock Solution in Dilute Solution 1) (⋅ g AA in Stock Solution) If your spectrophotometer is properly calibrated, λmax should be between 243 and 244 nm and E1% should be 550 ± 30 dL/g·cm. If they are not, you should calibrate the wavelength and/or absorbance axes of your spectrophotometer and repeat the measurements.

6) Measure and record the concentration of total ascorbic acid in all three dilute solutions and in the 5% MPA Diluent in duplicate using exactly the same method that you will use for the serum control materials and test samples, including any enzymatic treatment. We recommend that you analyze these solutions in the following order: Diluent, Dilute Solution 1, Dilute Solution 2, Dilute Solution 3, Dilute Solution 3, Dilute Solution 2, Dilute Solution 1, Diluent. a) Compare the values of the duplicate measurements. Are you satisfied that your measurement

precision is adequate? b) Compare the measured with the calculated [TAA] values. This is most conveniently done by

plotting the measured values on the y-axis of a scatterplot against the calculated values on the x-axis. The line through the four {calculated, measured} data pairs should go through the origin with a slope of 1.0. Are you satisfied with the agreement between the measured and calculated values?

Do not analyze the serum control materials or test samples until you are satisfied that your system is performing properly!

7) Once you have confirmed that your system is properly calibrated, analyze the serum control CS #2 (see protocol below). The target values for this materials is 28.1 ±1.0 µmol/L of sample.

If your measured values are not close to this value, please review your sample preparation procedure and whether you followed exactly the same measurement protocol the solutions prepared from the solid control material as you used for these serum controls. If the protocols differ, please repeat from Step 6 using the proper protocol. If the proper protocol was used, your measurement system may not be suitable for MPA-preserved samples. Please contact us: 301-975-3120 or [email protected]. Do not analyze the test samples until you are satisfied that your system is performing properly and is suitable for the analysis of MPA-preserved serum!

Protocol for Analysis of the Serum Control Materials and Test Samples

The serum control material and test samples are in sealed ampoules. They were prepared by adding equal volumes of 10% MPA to spiked human serum. We have checked the samples for stability and homogeneity. Only the total ascorbic acid is stable. While these samples contain some dehydroascorbic acid, its content is variable. Therefore, only total ascorbic acid should be reported. The serum control material and test samples should be defrosted by warming at 20 °C for not more than 10 min otherwise some irreversible degradation may occur.

Each serum test sample contains between 0.0 and 80.0 μmol of total ascorbic acid/L of solution. The total ascorbic acid in each ampoule should be measured in duplicate. Please report your results in μmol/(L of the sample solution) rather than μmol/(L of serum NIST used to prepare the sample).

E4


Participant #: Date:

Vitamin C Round Robin 26 NIST Micronutrient Measurement Quality Assurance Program

Preparation and Validation of Ascorbic Acid Solid Control Material

STOCK SOLUTION

Mass of ascorbic acid in the Stock Solution ..................................................__________ g

Mass of 5% MPA Diluent added to the 100 mL volumetric flask .................__________ g

DILUTE SOLUTION 1

Mass of added stock solution (0.5 mL) ..........................................................__________ g


Absorbance of Dilute Solution 1 at 242 nm...................................................__________ AU




Absorbance of Dilute Solution absorbance maximum ..................................__________ AU

Wavelength of maximum absorbance............................................................__________ nm

Calculated E1% ...............................................................................................__________ dL/g·cm

Calculated [TAA] DS1 .....................................................................................__________ μmol/L

DILUTE SOLUTION 2

Mass of added stock solution (0.25 mL) ........................................................__________ g

Mass of 5% MPA Diluent added to the 100 mL volumetric flask.................__________ g


DILUTE SOLUTION 3

Mass of added stock solution (0.125 mL) ......................................................__________ g



Please return by March 5, 2007 MMQAP Fax: 301-977-0685 100 Bureau Drive, Stop 8392 Email: [email protected] Gaithersburg, MD 20899-8392

E5


Participant #: Date:

Vitamin C Round Robin 26 NIST Micronutrient Measurement Quality Assurance Program

Analysis of Control Materials and Test Samples

Sample Replicate 1 Replicate 2 Units

Dilute Solution 1 μmol/L of Dilute Solution



5% MPA Diluent μmol/L of Diluent

μmol/L of Sample SRM 970-Level I Target: 8.41 ±0.61 μmol/L

Serum Test Sample #13 μmol/L of Sample




Were samples frozen upon receipt? Yes | No

Analysis method: HPLC-EC | HPLC-Fluor DAB | HPLC-OPD | HPLC-UV | AO-OPD | Other If “Other”, please describe:

COMMENTS:

Please return by March 5, 2007 MMQAP Fax: 301-977-0685 100 Bureau Drive, Stop 8392 Email: [email protected] Gaithersburg, MD 20899-8392

E6



Vitamin C Round Robin 26 NIST Micronutrients Measurement Quality Assurance Program

Packing List and Shipment Receipt Confirmation Form

This box contains one vial each of the following six VitC M2QAP samples:

Label Form

VitC #13 Liquid frozen (1:1 serum:10% MPA) VitC #42 Liquid frozen (1:1 serum:10% MPA)

VitC #112 Liquid frozen (1:1 serum:10% MPA) VitC #113 Liquid frozen (1:1 serum:10% MPA)

SRM 970 Lv1 Liquid frozen (1:1 serum:10% MPA) Control Solid AA

Please 1) Open the pack immediately 2) Check that it contains one vial each of the above samples 3) Check if the samples arrived frozen 4) Store the samples 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 [email protected])

1) Date this shipment arrived: ___________________________ 2) Are all of the vials intact? Yes | No

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

3) Was there any dry-ice left in cooler? Yes | No 4) Did the samples arrive frozen? Yes | No 5) At what temperature are you storing the samples? _______ ˚C 6) When do you anticipate analyzing these samples? ________________________

Your prompt return of this information is appreciated.

The M2QAP Gang

Mail: M2QAP NIST, Stop 8392 Fax: 301-977-0685 Gaithersburg, MD 20899-8392 Email: [email protected]

E7



Appendix F. Final Report for RR26

The following two 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 their previous distributions,

if any, and o summarizes aspects of the study that we believe may be of interest to the

participants.

F1

April 26, 2007

Dear _Colleague:

UNITED STATES DEPARTMENT OF COMMERCE National Institute Df Standards and Technology Gaithersburg, Maryland 20899-

Enclosed is the summary report of the results for Round Robin 26 (RR 26) for the measurement of total ascorbic acid (T AA, ascorbic acid plus dehydroascorbic .acid) in human serum. Included in this report are a summary of data for all laboratories and an individualized summary of your laboratory's measurement performance. The robust median is used.to estimate the consensus value for all samples, the "median absolute deviation from the median" (MADe) is used to estimate the expected standard deviation, and the coefficient of variation (CV) is defined as 1 OOxMADe/median.

RR 26 consisted of four test samples ( 13, 4 2, 112, and 113 ), one serum control material, and one solid control material for preparation of T AA control solutions. Details regarding the samples can be found in the enclosed report.

If you have concerns regarding your laboratory's perfonnance, we suggest that you obtain and analyze a unit of Standard Reference Material (SRM) 970 Vitamin C in Frozen Human Serum. SRM 970 can be purchased from the NIST SRM Program at phone: 301-975-6776; fax: 301-948-3730. If your measured values do not agree with the certified values, we suggest that you contact us for consultation.

Samples for the second vitamin C round robin (RR 27) of the 2007 M2QAP will be shipped during the week of June 4, 2007.

We look forward to meeting with you at the Micronutrients Measurement Quality Assurance Workshop that is being held in conjunction with the Experimental Biology meeting on May 2, 2007 at the Convention Center in Washington, DC.

Enclosures

Cc: L. C. Sander D.L. Duewer

egarding this report, please contact David Duewer at [email protected] or me at 301-975-3120; e-mail:

7-0685.

NISI F2

The NIST M2QAP Vitamin C Round Robin 26 (RR26) report consists of

Page “Individualized” Report 1 Summarizes your reported values for the nominal 55 mmol/L solution you prepared from the

ascorbic acid solid control sample, the serum control sample, and the four serum test samples.

2 Graphical summary of your RR26 sample measurements.

Page “All Lab” Report 1 A tabulation of results and summary statistics for Total Ascorbic Acid [TAA] in the RR26

samples and control/calibration solutions.

Serum-based Samples. One serum control and four unknowns were distributed in RR26. Control 1 SRM 970 level 1, ampouled in mid-1998. Sample 1 Serum 13, ampouled in late 2001, previously distributed as sample S19:1 (RR19, Fall

03), S21:1 (RR21, Fall 04) and S23:1 (RR23, Fall 05). A “blank” stripped serum. Sample 2 Serum 42, ampouled in late 2001, previously distributed as sample S18:2 (RR18, Spring

03), S19:3 (RR19, Fall 03), S21:3 (RR21, Fall 04), S22:3 (RR22, Spring 05) and S24:2 (RR24, Spring 06).

Sample 3 Serum 112, ampouled in 1993, previously distributed as sample 179B in RR4 (1993). Sample 4 Serum 113, ampouled in 1993, previously distributed as sample 180 in RR4 (1993), RR6

(1994) and RR14 (2001).

Results.

1) All participants who prepared the four 5% MPA control/calibration solutions (the three “Dilute Solutions” and the “Diluent”) did so correctly. The criteria used to evaluate this success are: the density of the 5% MPA (≈1.03 g/mL), the observed wavelength maximum of “Dilute Solution 1” (≈244 nm), the observed absorbance at that maximum (≈0.58 OD), the calculated E1% #1”(≈560 dL/g·cm).

2) Judging from the calibration parameters calculated for the control/calibration solutions (intercepts close to 0.0, slopes close to 1.0, R2 close to 1, and RMS close to 0.0), the measurement systems for all participants are linear and reasonably well calibrated. However, several participants continue to have measurement systems that perform somewhat differently for the control solutions and the test samples.

3) Somewhat remarkably, the median and the MADe for sera 112 (S26:3) and 113 (S26:4) are effectively unchanged from the TAA results obtained for these materials in the 1993 RR4 study.

F3

Appendix G. “All-Lab Report” for RR26

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.

G1

Mic

ronu

trien

ts M

easu

rem

ent Q

ualit

y As

sura

nce

Prog

ram

for T

otal

Asc

orbi

c Ac

id

"Rou

nd R

obin

" 26

- Mar

ch 2

007

Con

trol /

Cal

ibra

tion

Sam

ples

M

PA

Dilu

te S

olut

ion

1 Sa

mpl

es

G2

Den

sity

La

b D

ate

Dil:1

D

il:2

Dil:3

D

il:1

Dil:2

D

il:3

MPA

In

ter

Slop

e R

2 R

MS

g/m

L λ m

ax

A max

E1%

C

S#1

S26:

1 S2

6:2

S26:

3 S2

6:4

CS#

1 S2

6:1

S26:

2 S2

6:3

S26:

4 VC

-MA

20/0

3/07

58

.7

29.3

14

.3

58.8

29

.7

14.8

0.

0 0.

27

1.00

1.

000

0.3

1.03

3 24

4.

0.57

34

554.

3 8.

5 0.

0 35

.2

79.8

21

.3

8.2

0.0

34.9

79

.5

21.1

VC

-MB

26/1

1/06

57

.1

28.3

14

.1

59.4

28

.9

13.9

0.

0 -0

.39

1.04

1.

000

0.4

1.02

7 24

4.

0.56

30

560.

2 8.

3 0.

0 33

.0

71.0

19

.4

8.3

0.4

32.0

68

.4

18.9

VC

-MC

23

/01/

07

55.6

28

.2

14.2

60

.7

27.0

14

.0

0.0

-1.3

4 1.

09

0.99

5 2.

2 1.

029

243.

0.

5507

56

2.3

8.7

0.0

33.7

57

.2

15.1

9.

2 1.

2 32

.1

53.6

15

.1

VC-M

E 07

/03/

07

58.9

29

.6

14.6

57

.7

29.6

14

.6

0.0

0.20

0.

98

1.00

0 0.

3 1.

028

243.

0.

5843

56

3.5

9.1

0.5

32.3

68

.1

21.0

9.

1 0.

3 32

.7

69.2

21

.2

VC-M

G

26/0

1/07

58

.7

29.5

15

.0

58.1

27

.6

12.5

0.

0 -1

.24

1.00

0.

998

1.4

1.02

9 24

3.6

0.59

10

571.

8 9.

4 0.

0 35

.8

82.7

23

.8

10.7

1.

2 37

.0

84.0

25

.1

VC-M

H

20/0

2/07

61

.4

30.9

15

.0

62.7

31

.0

16.7

0.

0 0.

44

1.01

0.

999

1.0

1.03

2 24

4.

0.61

30

566.

6 8.

5 0.

6 32

.9

67.0

19

.2

7.9

0.1

32.0

65

.8

18.5

VC

-MI

21/0

2/07

55

.2

27.5

13

.9

55.2

27

.7

14.1

0.

0 0.

10

1.00

1.

000

0.1

1.03

1 8.

0 0.

0 33

.0

71.3

22

.4

7.9

0.0

32.9

71

.3

22.3

VC

-MJ

05/0

2/07

59

.7

29.9

15

.5

62.1

32

.4

16.1

0.

0 0.

24

1.04

0.

999

0.8

1.02

5 25

4 a

0.36

9 a

350.

9 a

11.9

4.

1 36

.5

83.2

27

.8

11.2

3.

7 34

.8

79.6

26

.4

VC-M

K 28

/02/

07

59.6

30

.1

15.3

58

.9

31.0

17

.3

2.8

2.81

0.

94

1.00

0 0.

1 1.

030

244.

0.

5948

56

6.6

10.5

3.

5 35

.7

82.0

26

.1

8.2

0.8

35.0

84

.2

24.8

VC

-MN

23

/03/

07

58.7

29

.3

14.1

60

.7

30.4

15

.1

-1.1

-0

.47

1.05

0.

999

0.8

1.02

9 24

3.8

0.56

16

543.

3 8.

9 0.

0 34

.1

75.9

23

.0

9.0

0.4

33.0

73

.0

22.5

VC

-MU

02

/03/

07

61.6

31

.0

17.6

59

.1

30.1

17

.0

0.0

0.13

0.

96

1.00

0 0.

2 1.

034

244.

0.

5881

54

2.0

7.7

0.3

29.0

68

.7

20.2

7.

9 0.

2 30

.1

71.5

20

.9

11

11

11

11

11

11

11

11

9 9

9 11

11

11

11

11

11

11

11

11

11

58

.7

29.4

14

.9

59.4

29

.6

15.1

0.

2 1.

030

243.

7 0.

5800

55

8.9

9.0

0.8

33.7

73

.4

21.8

8.

9 0.

8 33

.3

72.7

21

.5

2.1

1.1

1.0

2.1

1.6

1.5

1.0

0.00

3 0.

4 0.

0195

10

.4

1.2

1.5

2.1

8.2

3.5

1.1

1.1

1.9

9.0

3.3

55.2

27

.55

13.9

55

.2

27.0

2 12

.5

-1.1

1.

025

243.

0 0.

5507

54

2.0

7.7

0.0

29.0

57

.2

15.1

7.

9 0.

0 30

.1

53.6

15

.1

57.9

28

.76

14.2

58

.5

28.2

8 14

.0

0.0

1.02

8 24

3.6

0.56

30

554.

3 8.

4 0.

0 32

.9

68.4

19

.8

8.0

0.1

32.1

68

.8

19.9

58

.7

29.5

1 14

.6

59.1

29

.72

14.8

0.

0 1.

029

244.

0 0.

5843

56

2.3

8.7

0.0

33.7

71

.3

21.3

8.

3 0.

4 32

.9

71.5

21

.2

59.7

29

.95

15.2

60

.7

30.6

8 16

.4

0.0

1.03

1 24

4.0

0.59

10

566.

6 9.

3 0.

5 35

.4

80.9

23

.4

9.2

1.0

34.8

79

.5

23.6

61

.6

31.0

2 17

.6

62.7

32

.37

17.3

2.

8 1.

034

244.

0 0.

6130

57

1.8

11.9

4.

1 36

.5

83.2

27

.8

11.2

3.

7 37

.0

84.2

26

.4

1.4

0.8

0.8

1.9

1.8

1.3

0.0

0.00

3 0

0.01

62

6.4

0.7

0.0

2.1

6.8

2.9

0.6

0.6

1.4

8.6

3.4

2 3

5 3

6 9

0.26

0.

00

2.8

1.1

8 6

10

14

8 4

12

16

MAD

e eS

D

CV

CV

Med

ian

Med

ian

%75

%

75

Max

M

ax

Min

M

in

%25

%

25

N

N

Aver

age

Aver

age

SD

SD

Gra

vim

etric

, µm

ol/L

M

easu

red,

µm

ol/L

C

alib

ratio

n Pa

ram

eter

s Sp

ectro

phot

omet

ry

Mea

sure

d, µ

mol

/L

Cal

ibra

ted

to G

ravi

met

ric, µ

mol

/L

a)

5% T

richl

oroa

cetic

aci

d so

lutio

n

All L

ab re

port

Page

1 /

1

Appendix H. Representative “Individualized Report” for RR26

Each participant in RR26 received an “Individualized Report” reflecting their reported results. The following two pages are the “Individualized Report” for participant “VC-MA”.

H1

Set 1 of 11

Vitamin C "Round Robin" 26 Report: Participant VC-MA

MPA Dilute Solution 1 Control/Calibration Solutions Density Spectrophotometry Ymeas = Inter + Slope* Xgrav

Date RR Method 09/13/04 21 HPLC-EC 03/08/05 22 HPLC-EC 10/17/05 23 HPLC-EC 03/09/06 24 HPLC-EC 08/28/06 25 HPLC-EC 03/20/07 26 HPLC-EC

g/mL 1.030 1.034 1.030 1.031 1.039 1.033

λmax Amax E1%

244.0 0.555 562.2 243.0 0.559 562.9 244.0 0.562 567.9 244.0 0.568 586.7 242.0 0.555 557.4 244.0 0.573 554.3

Inter Slope R2 SEE -0.1 0.99 1.000 0.10 0.2 1.06 1.000 0.24

-0.6 1.09 0.998 1.47 0.2 1.13 1.000 0.41 0.8 0.95 0.999 0.92 0.3 1.00 1.000 0.31

Mean 1.033 243.5 0.56 565.2 0.57 SD 0.003 0.8 0.01 11.5 0.52 CV 0.34 0.34 1.3 2.0

[TAA] mmol/Lsample

2 0.0 0.0 0.0

6 35.1 0.3 1.1

2 72.1 0.1 10.8

4 19.7 0.4 1.3

Date RR Sample 09/13/04 21 CS#1 03/08/05 22 CS#1 10/17/05 23 CS#1 10/17/05 23 CS#1 03/09/06 24 CS#1 08/28/06 25 CS#1 03/20/07 26 CS#1

11/13/03 19 S19:1 09/13/04 21 S21:1 10/17/05 23 S23:1 03/20/07 26 S26:1

03/20/03 18 S18:2 11/13/03 19 S19:3 09/13/04 21 S21:3 03/08/05 22 S22:3 03/09/06 24 S24:2 03/20/07 26 S26:2

09/16/93 04 S04:2 03/20/07 26 S26:3

09/16/93 04 S04:3 05/25/95 06 S06:2 09/27/01 14 S14:1 03/20/07 26 S26:4

Rep1 Rep2 Fadj Mean SDdup

8.1 7.9 1.0 8.0 0.1 8.5 8.7 1.0 8.6 0.1 9.3 9.5 1.0 9.4 0.1 9.3 9.5 1.0 9.4 0.1 9.3 9.2 1.0 9.3 0.0 8.3 8.6 1.0 8.4 0.2 8.6 8.3 1.0 8.5 0.2

N Mean SDrepeat SDreprod

7 8.8 0.1 0.6

nd nd 1.0 nd nd 1.0 0.0 0.0 1.0 0.0 0.0 0.0 0.0 1.0 0.0 0.0

35.1 36.0 1.0 35.6 0.6 35.9 35.8 1.0 35.9 0.1 33.2 32.9 1.0 33.0 0.2 35.7 35.6 1.0 35.6 0.1 35.8 35.5 1.0 35.6 0.2 35.0 35.4 1.0 35.2 0.3

2.27 2.27 28.4 64.4 0.0 79.7 79.8 1.0 79.8 0.1

0.66 0.64 28.4 18.4 0.3 0.7 0.7 28.4 19.2 0.2

20.4 19.6 1.0 20.0 0.6 21.1 21.5 1.0 21.3 0.3

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 Fax: (301) 977-0685 Gaithersburg, MD 20899-8392 USA Email: [email protected]

Individualized Report Page 1/2

H2


NIST, RR 22

Set 1 of 11

Vitamin C "Round Robin" 26 Report: Participant VC-MA

Total Ascorbic Acid

[Tot

al A

scor

bic

Acid

], µm

ol/L

Your

[Tot

al A

scor

bic

Acid

], µm

ol/L

S18:

2S1

9:3

S21:

3S2

2:3

S24:

2Ap

pare

nt P

reci

sion

, SD

S2

6:2

S04:

2S2

6:3

S04:

3S0

6:2

S14:

1S2

6:4

Median [Total Ascorbic Acid], µmol/L

Concordance, SD

3rd Quartile (75%) You, this RR Median (50%) You, pat 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.

Sample Comments S26:1 VitC #13, a "blank" previously distributed in RRs 16, 19, 21, 22, and 24 S26:2 VitC #42, previously distributed in RRs 18, 19, 21, 22, and 24 S26:3 VitC #112, previous distributed in RR 4 S26:4 VitC #113, previous distributed in RR 4, 6 and 14

Individualized Report Page 2 / 2

H3

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