Post on 23-Oct-2020
NISTIR 7880-8
NIST Micronutrients Measurement Quality Assurance Program
Summer 2008 Comparability Studies
Results for Round Robin LXIV Fat-Soluble Vitamins and Carotenoids in Human Serum
and Round Robin 29 Ascorbic Acid in Human Serum
David L. Duewer Jeanice B. Thomas
karenwTypewritten Texthttp://dx.doi.org/10.6028/NIST.IR.7880-8
karenwTypewritten Text
karenwTypewritten Text
NISTIR 7880-8
NIST Micronutrients Measurement Quality Assurance Program
Summer 2008 Comparability Studies
Results for Round Robin LXIV Fat-Soluble Vitamins and Carotenoids in Human Serum
and Round Robin 29 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
karenwTypewritten Text
karenwTypewritten Texthttp://dx.doi.org/10.6028/NIST.IR.7880-8
karenwTypewritten Text
karenwTypewritten Text
karenwTypewritten Text
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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 Summer 2008 MMQAP measurement comparability improvement studies: 1) Round Robin LXIV Fat-Soluble Vitamins and Carotenoids in Human Serum and 2) Round Robin 29 Total Ascorbic Acid in Human Serum. The materials for both studies were shipped to participants in May 2008; participants were requested to provide their measurement results by September 12, 2008.
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 LXIV: Fat-Soluble Vitamins and Carotenoids in Human Serum ......................... 1 Round Robin 29: Vitamin C in Human Serum............................................................................... 2 References ............................................................................................................................................ 3
Appendix A. Shipping Package Inserts for RR64........................................................................ A1 Appendix B. Final Report for RR64 ..............................................................................................B1 Appendix C. “All-Lab Report” for RR64 ......................................................................................C1 Appendix D. Representative “Individualized Report” for RR64 ............................................... D1 Appendix E. Shipping Package Inserts for RR29 ......................................................................... E1 Appendix F. Final Report for RR29............................................................................................... F1 Appendix G. “All-Lab Report” for RR29..................................................................................... G1 Appendix H. Representative “Individualized Report” for RR29............................................... 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 LXIV: Fat-Soluble Vitamins and Carotenoids in Human Serum
Participants in the MMQAP Fat-Soluble Vitamins and Carotenoids in Human Serum Round Robin LXIV comparability study (hereafter referred to as RR64) received two lyophilized and three 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 May 2008. 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 RR64 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 29: Vitamin C in Human Serum
Participants in the MMQAP Vitamin C in Human Serum Round Robin 29 comparability study (hereafter referred to as RR29) 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 May 2008. 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 RR29 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 RR64
The following three items were included in each package shipped to an RR64 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
May 12, 2008
Dear Colleague:
UNITED STATES DEPARTMENT OF COMMERCE National Institute at Standards and Technology Gaithersburg, Maryland 20899-
Enclosed are the samples (Sera 347-351) forthe second fat-soluble vitamins and carotenoids in serum round robin study (Round Robin LXN) for the fiscal year (FY) 08 NIST Micronutrients Measurement Quality Assurance Program. You will find one vial of each of three liquid-frozen serum samples and two lyophilized 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 September 12, 2008. Results received more than two weeks after the due date will not be included in the summary report for this round robin study. For your convenience, we have also included one vial of Serum 198 (which was distributed in four past round robin studies) that can be used as a control and to help validate your method. We have included the averaged assigned values for the measurands in this serum as well.
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 intermittent 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 mteriiiittenfContact of the liql.iid sample wifh-thestopper. 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.
For consistency, we request that laboratories use the following absorptivities (dLJg.cm): retinal, 1843 at 325 nm (ethanol); retinyl palmitate, 975 at 325 run (ethanol); a.-tocopherol, 75.8 at 292 nm (ethanol); ytocopherol, 91.4 at 298 nm (ethanol); a-carotene, 2800 at 444 nm (hexane); ~-carotene, 2560 at 450 nm (ethanol), 2592 at 452 nm (hexane); lycopene, 3450 at 472 nm (hexane).
Please mail or fax your results to:
Micronutrients Measurement Quality Assurance Program NIST . 100 Bureau Drive Stop 8392 Gaithersburg, MD 20899-8392 Fax: (301) 977-0685
If you have questions or comments regarding this study, please call me at (301) 975-3120; e-mail me at jbthomas@nist.gov; or mail/fax, the above address.
l anic Brown Thomas ese ch Chemist
An ytical Chemistry Division Chemical Science and Technology Laboratory
Enclosures
A2
c
Reference Values for NIST Serum 198, µg/mL
Analyte Valuea U95 b P95 c
Total Retinol 0.73 0.02 0.11 Retinyl Palmitate 0.25 0.04 0.14
α-Tocopherol 14.1 0.3 2.0 β/γ-Tocopherol 2.57 0.06 0.31
Total β-Carotene 0.68 0.01 0.15 trans- β-Carotene 0.634 0.006 0.093
Total cis- β-Carotene 0.055 0.011 0.036 Total α-Carotene 0.039 0.007 0.020
Total Lycopene 0.155 0.030 0.079 trans-Lycopene 0.070 0.008 0.031
Total β-Cryptoxanthin 0.019 0.004 0.012 Total Lutein 0.052 0.003 0.019
Total Zeaxanthin 0.020 0.003 0.011 Total Lutein&Zeaxanthin 0.073 0.006 0.030
a Expected value; the average of the interlaboratory median results and mean of NIST results in M2QAP RR31, RR35, RR43, and RR57
b Approximate 95% uncertainty interval; the interval Value ± U95 is believed with approximately 95% confidence to contain the true value of the analyte
Approximate 95% prediction interval; the interval Value ± P95 contains approximately 95% of valid measurements obtained with measurement systems similar to those in use in M2QAP RR31, RR35, RR43, and RR57
A3
Participant #: ________ Date: _____________
Round Robin LXIV: Human Sera NIST Micronutrients Measurement Quality Assurance Program
Analyte 347 348 349 350 351 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 (349 to 351) frozen when received? Yes | No
Comments:
Mail: M2QAP NIST, Stop 8392 Please return results before 12-Sep-2008 Fax: 301-977-0685 Gaithersburg, MD 20899-8392 Email: David.Duewer@NIST.gov
A4
mailto:David.Duewer@NIST.gov
Participant #: ________ Date: _____________
Fat-Soluble Vitamins Round Robin LXIV 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 #347 #348
Form Lyophilized Lyophilized
Reconstitute? Yes (1 ml H2O) Yes (1 ml H2O)
Vial/Cap 5 mL clear, silver 2 mL amber, blue
#349 Liquid frozen No 2 mL amber, silver #350 Liquid frozen No 2 mL amber, silver #351 Liquid frozen No 10 mL amber, silver
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 david.duewer@nist.gov)
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: David.Duewer@NIST.gov
A5
mailto:David.Duewer@NIST.govmailto:david.duewer@nist.gov
Appendix B. Final Report for RR64
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.
B1
November 20, 2008
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 LXN (RR64) of the 2008 NIST Micronutrients Measurement Quality Assurance Program (M2QAP) for the fat-soluble vitamins and carotenoids in human serum. Included in this report are: 1) 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 co1:11parability.
Your overall measurement comparability is summarized in the "Score Card" summary, page 6 of the All Lab Report. Combined results rated 1to3 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 graphically in the "target plots" that are the last page of your Individualized Report. If you · have concerns regarding your laboratory's performance, please contact us for consultation.
We have received your inquiries regarding the availability of the renewal material SRM 968d, FatSoluble Vitamins, Carotenoids, and Cholesterol in Human Serum. The material has been value-assigned. Our SRM office is c~rrently finalizing the packaging of the SRM prior to sale. Orders can be placed directly through our on-line SRM order request system at: https://srmors.nist.gov/index.cfrn. You can
• also call the SRM office directly at (301) 975-2200 for more details regarding the SRM's availability.
Samples for the first 2009 QA inter laboratory exercise will be shipped during the week of December 8, 2009. If you have any questions regarding this report, please contact Dave Duewer at david.duewer@nist.gov or me atjbthomas@nist.gov, tel: 301/975-3120, or fax: 301/977-0685.
I I l)L-'
/
ea ice Brown Tho:r;nas Re earch Chemist A alytical Chemistry Division
. emical Science and Technology Laboratory
Cc: L.C. Sander D.L. Duewer
NISI B2
The NIST M2QAP Round Robin LXIV (RR64) report consists of:
Page “All Lab” Report
1-4 A listing of all results and statistics for all analytes. 5 A legend for the list of results and statistics. 6 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. Five samples were distributed in RR64.
Serum Description Prior Distributions
347 Lyophilized, augmented, multi-donor serum #195:RR31-6/94, #214:RR35-9/95; prepared in 1994. This material is a 1:1 blend of #244:RR43-6/98, #328:RR60-9/06
stripped serum and a serum pool augmented with
retinol, retinyl palmitate, and α-tocopherol.
348 Lyophilized, native, single-donor, commercially #290:RR53-2/03, #300:RR55-3/04, obtained serum prepared in 2002. The same #312:RR57-3/05, #322:RR59-3/06, material was used to prepare #349. #333:RR61-3/07
349 Fresh-frozen, native, single-donor, commercially #292:RR53-2/03, #301:RR55-3/04, obtained serum prepared in 2002. The same #313:RR57-3/05, #323:RR59-3/06, material was used to prepare #348. #332:RR61-3/07
350 Fresh-frozen, native, multi-donor plasma #340:RR63-3/08 commercially prepared in 2006.
351 Fresh-frozen, native, multi-donor serum prepared in #341 & #344:RR63-3/08 Fall, 2007 (SRM 968d)
Results
1) Sera Stability. There was no significant change in the median level or measurement variability of any measurand in any of the lyophilized or fresh-frozen materials.
2) Candidate SRM 1950, Metabolites in Human Plasma (#350). As in RR63, no analysis problems were reported for this material. We anticipate this material being available for purchase mid-2009.
3) SRM 968d Fat-Soluble Vitamins and Carotenoids in Human Serum (#351). As in RR63, no analysis problems were reported for this material. It will be available for purchase in the near future.
B3
Appendix C. “All-Lab Report” for RR64
The following six pages are the “All-Lab Report” as provided to all participants, with two exceptions:
• the participant identifiers (Lab) have been altered. • the order in which the participant results are listed has been altered.
The data summary in the “All-Lab Report” has been altered to ensure confidentiality of identification codes assigned to laboratories. The only attributed results are those reported by NIST. The NIST results are not used in the assessment of the consensus summary results of the study.
C1
Rou
nd R
obin
LXI
V La
bora
tory
Res
ults
Tota
l Ret
inol
, μg/
mL
trans
-Ret
inol
, μg/
mL
Ret
inyl
Pal
mita
te, μ
g/m
L α-
Toco
pher
ol, μ
g/m
L γ/β-
Toco
pher
ol, μ
g/m
L δ-
Toco
pher
ol, μ
g/m
L La
b 34
7 34
8 34
9 35
0 35
1
C2
FSV-
BA
0.40
9 0.
633
0.66
5 0.
431
0.35
6 FS
V-BB
0.
429
0.68
0 0.
679
0.43
8 0.
396
FSV-
BC
0.35
5 0.
630
0.67
3 0.
419
0.37
0 FS
V-BD
0.
407
0.58
9 0.
604
0.41
3 0.
334
FSV-
BE
0.44
8 0.
696
0.74
6 0.
464
!0.2
94
FSV-
BF
0.35
0 0.
590
0.60
0 0.
410
0.33
0 FS
V-BG
0.
383
0.60
7 0.
644
0.42
8 0.
358
FSV-
BH
0.30
5 0.
558
0.62
0 0.
381
0.31
2 FS
V-BI
0.
385
0.58
3 0.
616
0.39
7 0.
323
FSV-
BJ
0.36
8 0.
545
0.60
6 0.
385
0.31
4 FS
V-BK
0.
472
0.70
2 0.
738
0.52
6 0.
470
FSV-
BL
0.34
0 0.
660
0.69
0 0.
430
0.34
0 FS
V-BM
0.
350
0.62
0 0.
650
0.42
0 0.
350
FSV-
BN
0.36
4 0.
548
0.55
4 0.
372
0.31
4 FS
V-BO
0.
344
0.73
9 0.
633
0.46
4 0.
438
FSV-
BP
0.44
4 0.
633
0.64
8 0.
447
0.35
8 FS
V-BQ
0.
382
0.63
4 0.
656
0.42
5 0.
323
FSV-
BR ≥0
.420
≥0
.690
≥0
.630
≥0
.430
≥0
.340
≥0
.392
≥0
.424
≥0
.353
≥0
.592
≥0
.694
FS
V-BS
FS
V-BT
0.
409
0.66
1 0.
568
0.44
0 0.
438
FSV-
BU
0.34
2 0.
557
0.60
6 0.
442
0.32
4 FS
V-BV
0.
305
0.64
2 0.
648
0.39
4 0.
330
FSV-
BW
0.40
0 0.
620
0.69
0 0.
430
0.35
0 FS
V-C
D
0.32
0 0.
550
0.57
0 0.
370
0.29
0 FS
V-C
E 0.
380
0.66
0 0.
700
0.45
0 0.
340
FSV-
CF
0.44
7 0.
685
0.72
4 0.
483
0.39
4 FS
V-C
G
0.36
9 0.
625
0.60
8 0.
401
0.33
6 FS
V-C
I 0.
288
0.67
6 0.
701
0.45
8 0.
379
FSV-
CW
0.
350
0.59
3 0.
605
0.40
4 0.
339
FSV-
CZ
0.32
2 0.
552
0.56
5 0.
363
0.31
4 FS
V-D
D
0.36
0 0.
530
0.58
0 0.
360
0.30
0 FS
V-D
Q
FSV-
DV ≥0
.386
≥0
.603
≥0
.641
≥0
.407
≥0
.334
FS
V-EE
0.
335
0.56
2 0.
569
0.36
6 0.
291
347
348
349
350
351
0.42
0 0.
690
0.63
0 0.
430
0.34
0 0.
392
0.42
4 0.
353
0.59
2 0.
694
0.38
6 0.
603
0.64
1 0.
407
0.33
4
347
348
349
350
351
0.09
1 0.
070
0.08
7 0.
023
0.02
5 0.
079
0.06
6 0.
067
0.01
2 0.
007
0.10
1 0.
094
0.10
4 0.
014
nd
0.11
6 0.
102
0.10
2 nd
nd
0.
116
0.07
1 0.
082
nq
nq
0.12
2 0.
084
0.08
8 0.
026
0.01
8
0.14
3 0.
122
0.13
1 0.
017
0.00
7
0.15
2 0.
093
0.10
9 0.
015
Rou
nd R
obin
LXI
V La
bora
tory
Res
ults
Tota
l β-C
arot
ene,
μg/
mL
trans
-β-C
arot
ene,
μg/
mL
Tota
l cis
-β-C
arot
ene,
μg/
mL
Tota
l α-C
arot
ene,
μg/
mL
Tota
l Lyc
open
e, μ
g/m
L tra
ns-L
ycop
ene,
μg/
mL
Lab
347
348
349
350
351
C3
FSV-
BA
0.34
8 0.
111
0.12
2 0.
081
0.08
4 FS
V-BB
0.
309
0.10
7 0.
110
0.07
3 0.
075
FSV-
BC
FSV-
BD
FSV-
BE
0.17
5 0.
084
0.07
9 0.
068
!0.0
387
FSV-
BF
0.36
7 0.
099
0.09
9 0.
064
0.07
5 FS
V-BG
0.
354
0.14
6 0.
153
0.08
7 0.
093
FSV-
BH
0.37
1 0.
118
0.12
1 0.
075
0.07
8 FS
V-BI
0.
325
0.11
7 0.
116
0.07
4 0.
070
FSV-
BJ
0.31
4 0.
107
0.11
0 0.
061
0.06
9 FS
V-BK
FS
V-BL
FS
V-BM
FS
V-BN
0.
320
0.10
8 0.
108
0.07
2 0.
077
FSV-
BO
0.37
3 0.
136
0.12
7 0.
083
0.08
9 FS
V-BP
0.
064
0.07
0 0.
082
0.09
0 0.
040
FSV-
BQ
FSV-
BR
FSV-
BS ≥0
.314
≥0
.123
≥0
.115
≥0
.057
≥0
.067
FS
V-BT
0.
382
0.12
8 0.
127
0.09
4 0.
094
FSV-
BU
0.34
1 0.
126
0.13
5 0.
083
0.08
3 FS
V-BV
0.
330
0.12
3 0.
124
0.06
7 0.
067
FSV-
BW
0.40
0 0.
130
0.14
5 0.
083
0.08
2 FS
V-C
D
0.42
2 0.
197
0.20
1 0.
168
0.18
2 FS
V-C
E 0.
280
0.03
1 0.
140
0.11
0 0.
070
FSV-
CF
FSV-
CG
0.
301
0.11
2 0.
113
0.06
6 0.
054
FSV-
CI
0.29
4 0.
106
0.11
4 0.
057
0.05
0 FS
V-C
W
0.34
0 0.
132
0.13
5 0.
084
0.09
0 FS
V-C
Z FS
V-D
D
FSV-
DQ
0.
378
0.05
2 0.
088
0.06
1 0.
053
FSV-
DV
0.30
9 0.
136
0.13
5 0.
089
0.07
8 FS
V-EE
347
348
349
350
351
0.31
5 0.
107
0.11
8 0.
076
0.08
0 0.
287
0.10
3 0.
105
0.07
0 0.
071
0.34
6 0.
118
0.12
1 0.
075
0.07
8
0.27
9 0.
100
0.10
0 0.
066
0.06
9 0.
289
0.11
6 0.
108
0.07
7 0.
084
0.31
4 0.
123
0.11
5 0.
057
0.06
7 0.
355
0.12
3 0.
122
0.08
9 0.
088
0.27
4 0.
103
0.10
6 0.
061
0.04
8
347
348
349
350
351
0.03
3 0.
004
0.00
4 0.
005
0.00
4 0.
022
0.00
4 0.
004
0.00
4 0.
004
0.02
5 nq
nq
nq
nq
0.03
8 0.
006
0.00
4 0.
003
0.00
5 0.
084
0.02
0 0.
019
0.00
5 0.
005
0.03
3 0.
007
0.00
7 0.
007
0.00
7
0.02
8 0.
009
0.00
7 0.
006
0.00
6
347
348
349
350
351
0.01
6 0.
073
0.08
0 0.
026
0.00
9 0.
015
0.06
5 0.
066
0.02
2 0.
008
0.01
7 0.
085
0.09
1 0.
024
0.01
0 nq
0.
086
0.09
0 nq
nq
0.
014
0.07
2 0.
078
0.02
5 0.
007
0.02
9 0.
080
0.09
2 0.
020
0.01
5
-0.
072
0.07
8 0.
024
0.00
8 0.
018
0.07
9 0.
089
0.02
6 0.
005
nd
0.03
1 0.
038
0.01
4 0.
013
0.02
3 0.
097
0.10
4 0.
034
0.02
2 0.
022
0.11
1 0.
110
0.04
4 0.
021
0.01
8 0.
092
0.09
7 0.
027
0.01
1 0.
018
0.09
0 0.
090
0.02
4 0.
007
0.00
9 0.
059
0.06
5 0.
019
0.00
4 0.
019
0.06
1 0.
071
0.02
2
Rou
nd R
obin
LXI
V La
bora
tory
Res
ults
Tota
l β-C
rypt
oxan
thin
, μg/
mL
Tota
l α-C
rypt
oxan
thin
, μg/
mL
Tota
l Lut
ein,
μg/
mL
Tota
l Zea
xant
hin,
μg/
mL
Tota
l Lut
ein&
Zeax
anth
in, μ
g/m
L La
b 34
7 34
8 34
9 35
0 35
1
C4
347
348
349
350
351
0.00
3 0.
029
0.03
2 0.
022
0.01
9 0.
003
0.02
2 0.
023
0.01
4 0.
015
0.00
2 0.
013
0.01
3 0.
004
0.00
7
347
348
349
350
351
0.03
7 0.
099
0.10
1 0.
085
0.07
0
0.02
5 0.
084
0.08
8 0.
058
0.04
5 0.
013
0.04
6 0.
036
0.04
5 0.
045
0.02
4 0.
071
0.07
4 0.
061
0.04
9 0.
023
0.07
1 0.
079
0.06
2 0.
054
0.03
3 0.
077
0.07
9 0.
064
0.05
9 0.
021
0.07
2 0.
073
0.06
6 0.
057
0.02
9 0.
086
0.07
5 0.
072
0.09
8
0.02
1 0.
055
0.05
4 0.
047
0.03
0 0.
026
0.07
9 0.
080
0.06
9 0.
058
0.01
0 0.
098
0.10
1 0.
091
0.07
7
FSV-
BA 0
.009
0.0
64 0
.069
0.0
49 0
.046
FS
V-BB
0.0
10 0
.052
0.0
53 0
.036
0.0
40
FSV-
BC
FSV-
BD
FSV-
BE
FSV-
BF
FSV-
BG 0
.009
0.0
63 0
.069
0.0
40 0
.050
FS
V-BH
nq
0.
059
0.06
2 0.
041
0.04
6 FS
V-BI
0.0
08 0
.051
0.0
53 0
.033
0.0
36
FSV-
BJ
nq
0.03
7 0.
045
0.02
6 0.
032
FSV-
BK
FSV-
BL
FSV-
BM
FSV-
BN 0
.027
0.0
39 0
.040
0.0
25 0
.031
FS
V-BO
0.0
10 0
.048
0.0
51 0
.034
0.0
44
FSV-
BP 0
.008
0.0
18 0
.015
0.0
25 0
.018
FS
V-BQ
FS
V-BR
FS
V-BS
0.0
16 0
.075
0.0
80 0
.041
0.0
56
FSV-
BT 0
.010
0.0
49 0
.050
0.0
36 0
.040
FS
V-BU
0.0
11 0
.048
0.0
47 0
.032
0.0
34
FSV-
BV 0
.007
0.0
55 0
.055
0.0
33 0
.034
FS
V-BW
nq
0.
052
0.05
7 0.
031
0.03
8 FS
V-C
D 0
.006
0.0
45 0
.046
0.0
32 0
.039
FS
V-C
E FS
V-C
F FS
V-C
G 0
.015
0.0
77 0
.077
0.0
49 0
.047
FS
V-C
I FS
V-C
W 0
.005
0.0
51 0
.053
0.0
31 0
.036
FS
V-C
Z FS
V-D
D
FSV-
DQ
0.0
16 0
.035
0.0
56 0
.034
0.0
33
FSV-
DV
FSV-
EE
347
348
349
350
351
0.01
4 0.
048
0.05
0 0.
037
0.03
7
0.00
8 0.
032
0.02
7 0.
018
0.00
9 0.
006
0.01
9 0.
015
0.01
5 0.
020
0.01
0 0.
031
0.03
2 0.
021
0.02
5
0.00
9 0.
027
0.03
0 0.
017
0.02
0 0.
006
0.02
6 0.
027
0.02
2 0.
023
0.01
2 0.
045
0.03
7 0.
029
0.04
0
Rou
nd R
obin
LXI
V La
bora
tory
Res
ults
Coe
nzym
e Q
10, μ
g/m
L Ph
yllo
quin
one
(K1)
, ng/
mL
C5
Lab
347
348
349
350
351
347
348
349
350
351
FSV-
BA
FSV-
BB
FSV-
BC
FSV-
BD
FSV-
BE 0
.306
0.7
64 0
.791
0.8
50 0
.786
0.
534
0.49
2 0.
466
0.52
6 0.
280
FSV-
BF
FSV-
BG
FSV-
BH
FSV-
BI
FSV-
BJ 0
.276
0.6
97 0
.763
0.5
40 0
.573
FS
V-BK
FS
V-BL
FS
V-BM
FS
V-BN
FS
V-BO
FS
V-BP
FS
V-BQ
FS
V-BR
FS
V-BS
FS
V-BT
0.1
27 0
.223
0.2
52 0
.349
0.3
54
FSV-
BU
FSV-
BV
FSV-
BW 0
.356
0.7
83 0
.787
0.6
33 0
.602
FS
V-C
D
FSV-
CE
FSV-
CF
FSV-
CG
FS
V-C
I 0.
310
0.76
0 0.
800
0.85
0 0.
750
0.62
5 0.
421
0.38
6 0.
424
0.20
6 FS
V-C
W 0
.109
0.3
10 0
.279
0.2
47 0
.207
FS
V-C
Z
0
.323
0.8
48 0
.696
0.7
43 0
.626
FS
V-D
D
FSV-
DQ
FS
V-D
V FS
V-EE
0.2
85 0
.634
0.6
53 0
.700
0.4
96
N
Min
M
edia
n M
ax
SD
CV
Npa
st
Med
ianp
ast
SDpa
st
Mea
nNIS
T Sr
ep
Shet
SN
IST
NAV
N
AU
88
88
8 2
22
22
0.10
9 0.
223
0.25
2 0.
247
0.20
7 0.
53
0.42
0.
39
0.42
0.
21
0.29
6 0.
729
0.73
0 0.
667
0.58
8 0.
58
0.46
0.
43
0.48
0.
24
0.35
6 0.
848
0.80
0 0.
850
0.78
6 0.
63
0.49
0.
47
0.53
0.
28
0.05
5 0.
160
0.17
0 0.
206
0.14
6 19
22
23
31
25
6 5
5 9
9 0.
350
0.70
1 0.
751
0.68
3 0.
633
0.01
8 0.
096
0.10
4 0.
166
0.12
2
0.29
6 0.
729
0.73
0 0.
667
0.58
8 0.
055
0.16
0 0.
170
0.20
6 0.
146
All L
ab R
epor
t Pa
ge 4
/ 6
Term N Number of (non-NIST) quantitative values reported for this analyte
Min Minimum (non-NIST) quantitative value reportedMedian Median (non-NIST) quantitative value reported
Max Maximum (non-NIST) quantitative value reportedSD 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)
MeanNIST Mean of NIST resultsSrep NIST's within-vial pooled standard deviationShet NIST's among-vial pooled standard deviation
SNIST Combined standard deviation for NIST analyses: (Srep 2 + Shet 2)0.5
NAV NIST Assigned Value = (Median + MeanNIST)/2 for analytes reported by NIST analyst(s) = Median for analytes reported by ≥ 5 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 Median and MeanNIST. The expected long-term SD, eSD, is defined in: Duewer et al. Anal Chem 1997;69(7):1406-1413.
- Not analyzednd 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
! Discrepant value: heterogeneous serum, damaged sample, malfunction, etc.
italics Not explicitly reported but calculated by NIST from reported values
Round Robin LXIV Laboratory Results
Analytes Reported By One Laboratory
Analyte Code 347 348 349 350 351 Ubiquinol FSV-BW 0.277 0.620 0.725 0.568 0.135
Ubiquinone FSV-BW nq 0.163 0.062 0.065 0.467
Legend
All Lab Report Page 5 / 6
C6
Round Robin LXIV 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-BP FSV-BQ FSV-BR FSV-BS FSV-BT FSV-BU FSV-BV
FSV-BW FSV-CD FSV-CE FSV-CF FSV-CG FSV-CI
FSV-CW FSV-CZ FSV-DD FSV-DQ FSV-DV FSV-EE
NIST n
% 1 % 2 % 3 % 4
TR aT g/bT bC tbC aC TLy TbX TLu TZ L&Z 1 1 1 1 1 1 1 2 1 2 1 1 1 1 1 1 1 2 2 2 1 1 1 2 1 1 3 1 1 1 1 1 1 2 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 1 1 1 3 1 1 1 1 1 2 2 1 1 1 1 1 3 1 1 1 2 1 1 1 1 1 2 1 1 1 1 1 2 4 2 4 3 3 1 2 1 3 4 1 1 2 2 2 1 2 1 1 1 2 2 1 1 2 2 2 1 2 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 1 1 2 1 1 4 1 1 4 1 4 3 2 1 1 2 2 1 2 1 1 2 2 2 1 2 2 1 2 2 2 1 1 1 1 1 1 1 2 1 2 2 3 2
2 1 3 2 3 2 2 2 1 1 2 1 2 1 1 1 1 1 1 1 1 1 1 1 34 32 20 24 8 20 17 19 12 11 19
TR aT g/bT bC tbC aC TLy TbX TLu TZ L&Z 62 69 85 71 75 75 71 68 58 45 63 32 25 10 8 25 25 18 21 42 55 26 3 3 5 13 0 0 6 11 0 0 5 3 3 0 8 0 0 6 0 0 0 5
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
yo u N You i − Median i 2
AP = Apparent Precision = ∑ (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 6 / 6
C7
Appendix D. Representative “Individualized Report” for RR64
Each participant in RR64 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 RR64:
• Total Retinol • Retinyl Palmitate • α-Tocopherol • γ/β-Tocopherol • Total β-Carotene • 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 fourteen pages are the “Individualized Report” for the analytes evaluated by participant FSV-BA.
D1
Set
1 o
f 40
Indi
vidu
aliz
ed R
ound
Rob
in L
XIV
Rep
ort:
FSV-
BA
Sum
mar
y Se
rum
347
Se
rum
348
Se
rum
349
Se
rum
350
Se
rum
351
D2
Anal
yte
You
NAV
n
You
NAV
n
You
NAV
n
You
NAV
n
You
NAV
n
Tota
l Ret
inol
0.4
09 0
.350
30
0.63
3 0.
612
30
0.66
5 0.
643
30
0.43
1 0.
415
30
0.35
6 0.
338
29
Ret
inyl
Pal
mita
te 0
.09
0.12
9
0.1
0.1
9 0.
1 0.
1 9
0.02
0.
02
7 0.
03
0.01
5
α-To
copherol 7
.11
6.83
31
9.
04
10.1
1 31
9.
59
10.8
1 31
7.
78
8.25
31
5.
80
5.94
29
γ/β-To
copherol 1
.351
1.3
33 1
9 1.
629
1.75
3 19
1.
742
1.81
6 19
1.
733
1.79
2 19
1.
480
1.44
8 18
δ-To
copherol 0
.081
0.0
75
3 0.
046
0.04
6 3
0.05
3 0.
053
3 0.
075
0.07
5 3
0.08
0 0.
083
4 To
tal β-Carotene
0.34
8 0.
334
22
0.11
1 0.
115
22
0.12
2 0.
125
22
0.08
1 0.
079
22
0.08
4 0.
079
21
trans-β-Carotene
0.31
5 0.
302
8 0.
107
0.11
2 8
0.11
8 0.
111
8 0.
076
0.07
3 8
0.08
0 0.
075
8 To
tal cis-β-Carotene
0.03
3 0.
033
7 0.
004
0.00
7 6
0.00
4 0.
005
6 0.
005
0.00
5 6
0.00
4 0.
005
6 To
tal α-Carotene
0.01
6 0.
017
16
0.07
3 0.
079
19
0.08
0 0.
083
19
0.02
6 0.
028
18
0.00
9 0.
009
16
Tota
l Lyc
open
e 0.
079
0.07
3 16
0.
446
0.45
1 16
0.
517
0.46
9 16
0.
328
0.31
0 16
0.
259
0.26
8 16
tra
ns-L
ycop
ene
0.03
4 0.
034
8 0.
259
0.26
6 8
0.30
2 0.
288
8 0.
170
0.14
8 8
0.12
5 0.
120
8 To
tal β-Cryptoxanthin 0
.009
0.0
10 1
5 0.
064
0.05
0 18
0.
069
0.05
1 18
0.
049
0.03
4 18
0.
046
0.03
6 18
To
tal α-Cryptoxanthin 0
.003
0.0
03
3 0.
029
0.02
2 3
0.03
2 0.
023
3 0.
022
0.01
4 3
0.01
9 0.
015
3 To
tal L
utei
n&Ze
axan
thin
0.0
36 0
.037
17
0.10
1 0.
107
18
0.10
4 0.
109
18
0.09
2 0.
094
18
0.08
2 0.
077
18
You
: Yo
ur re
porte
d va
lues
for t
he li
sted
ana
lyte
s (m
icro
gram
s/m
illilit
er)
NAV
: N
IST
Assi
gned
Val
ues,
her
e eq
ual t
o th
is R
R's
med
ian
n :
Num
ber o
f non
-NIS
T la
bora
torie
s re
porti
ng q
uant
itativ
e va
lues
for t
his
anal
yte
in th
is s
erum
Plea
se c
heck
our
reco
rds
agai
nst y
our r
ecor
ds.
Sen
d co
rrect
ions
and
/or u
pdat
es to
...
Mic
ronu
trien
ts M
easu
rem
ent Q
ualit
y As
sura
nce
Prog
ram
N
atio
nal I
nstit
ute
of S
tand
ards
and
Tec
hnol
ogy
Tel:
(301
) 975
-393
5 10
0 Bu
reau
Driv
e St
op 8
392
Fax:
(301
) 977
-068
5 G
aith
ersb
urg,
MD
208
99-8
392
USA
Em
ail:
davi
d.du
ewer
@ni
st.g
ov
Indi
vidu
aliz
ed R
epor
t Pa
ge 1
/ 14
NIST, this RR
D3
Set 1 of 40
Individualized RR LXIV Report: FSV-BA Total Retinol, μg/mL
Appa
rent
Pre
cisio
n, S
D [A
nalyt
e], µ
g/m
L
195
214
244
328
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[Ana
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, µg/
mL
Appa
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Pre
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D
Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 2 / 14
NIST, this RR
D4
Set 1 of 40
Individualized RR LXIV Report: FSV-BA Retinyl Palmitate, μg/mL
Appa
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g/m
L
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[Ana
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, µg/
mL
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Pre
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Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 3 / 14
NIST, this RR
D5
Set 1 of 40
Individualized RR LXIV Report: FSV-BA α-Tocopherol, μg/mL
Appa
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D [A
nalyt
e], µ
g/m
L
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[Ana
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, µg/
mL
Appa
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Pre
cisio
n, S
D
Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 4 / 14
NIST, this RR
D6
Set 1 of 40
Individualized RR LXIV Report: FSV-BA γ/β-Tocopherol, μg/mL
Appa
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n, S
D [A
nalyt
e], µ
g/m
L
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[Ana
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, µg/
mL
Appa
rent
Pre
cisio
n, S
D
Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 5 / 14
NIST, this RR
D7
Set 1 of 40
Individualized RR LXIV Report: FSV-BA Total β-Carotene, μg/mL
Appa
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g/m
L
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[Ana
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, µg/
mL
Appa
rent
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cisio
n, S
D
Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 6 / 14
NIST, this RR
D8
Set 1 of 40
Individualized RR LXIV Report: FSV-BA trans-β-Carotene, μg/mL
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D [A
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e], µ
g/m
L
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[Ana
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, µg/
mL
Appa
rent
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cisio
n, S
D
Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 7 / 14
NIST, this RR
D9
Set 1 of 40
Individualized RR LXIV Report: FSV-BA Total cis-β-Carotene, μg/mL
Appa
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g/m
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[Ana
lyte]
, µg/
mL
Appa
rent
Pre
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n, S
D
Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 8 / 14
NIST, this RR
D10
Set 1 of 40
Individualized RR LXIV Report: FSV-BA Total α-Carotene, μg/mL
Appa
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L
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[Ana
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, µg/
mL
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rent
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n, S
D
Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 9 / 14
NIST, this RR
D11
Set 1 of 40
Individualized RR LXIV Report: FSV-BA Total Lycopene, μg/mL
Appa
rent
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e], µ
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L
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[Ana
lyte]
, µg/
mL
Appa
rent
Pre
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n, S
D
Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 10 / 14
NIST, this RR
D12
Set 1 of 40
Individualized RR LXIV Report: FSV-BA trans-Lycopene, μg/mL
Appa
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n, S
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L
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[Ana
lyte]
, µg/
mL
Appa
rent
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n, S
D
Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 11 / 14
NIST, this RR
D13
Set 1 of 40
Individualized RR LXIV Report: FSV-BA Total β-Cryptoxanthin, μg/mL
Appa
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, µg/
mL
Appa
rent
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n, S
D
Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 12 / 14
NIST, this RR
D14
Set 1 of 40
Individualized RR LXIV Report: FSV-BA Total Lutein&Zeaxanthin, μg/mL
Appa
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, µg/
mL
Appa
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n, S
D
Concordance, SD
3rd Quartile (75%) You, this RR You, ≥x, this RR
Median [Analyte], µg/mL
Long-term Precision, SD
Median (50%) You, past RRs You, ≥x, past RRs Others, this RR
1st Quartile (25%) Expectation
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 #347 31:#195, 35:#214, 43:#244, 60:#328 Lyophilized, multi-donor, aug(TR, RP,aT) #348 53:#290, 55:#300,57:#312, 59:#322:RR59,61:#333 Lyophilized, native, single-donor #349 53:#292, 55:#301,57:#313, 59:#323:RR59,61:#332 Fresh-frozen, native, single-donor #350 63:#340 Plasma, fresh-frozen, native, multi-donor #351 63:#341, 63:#344 Fresh-frozen, native, multi-donor
Individualized Report Page 13 / 14
D15
Set
1 o
f 40
Indi
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Rob
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Rep
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V-BA
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phic
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rabi
lity
Sum
mar
y
Tota
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α
-Toc
ophe
rol
Tota
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ene
Tota
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trans
-Ret
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γ/β
-Toc
ophe
rol
Tota
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open
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Ret
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Pal
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Tota
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trans
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4
Appendix E. Shipping Package Inserts for RR29
The following five items were included in each package shipped to an RR29 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
May 12, 2008
Dear Colleague:
UNITED STATES DEPARTMENT OF COMMERCE National Institute of Standards and Technology Gaithersburg, Maryland 20899-
The samples within this package constitute Vitamin C Round Robin 29 (RR29) of the 2008 Micronutrients Measurement Quality Assurance Program.
RR29 consists of four vials of frozen serum test samples (#15, #73, #90, and #111 ), one vial of frozen control serum (CS #2) and one vial of ascorbic acid solid control material (Control) Please fo_llow 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 the control serum to validate the performance of your measurement system before you analyze the test samples. The target value and ~95% confidence interval for target value and ~95% confidence interval for CS #2 is 28.1 ±1.0 µmol/L of sample.
The report for RR28 was mailed May 2, 2008. If you find your results for RR28 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: srminfo@nist.gov).
Please be aware that sample contact with any oxidant-contaminated surface (vials, glassware, etc.) may degrade your measurement system's performance (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.
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: jbthomas@nist.gov.
We ask that you return your results for these RR29 samples before Sep 12, 2008. We would appreciate receiving your results as soon as they become available. Please use-the attached form. Your results will be kept confidential.
es a ical Chemistry Division
·c mical Science and Technology Laboratory
Enclosures: Protocols, Preparation and Analysis of Control Materials and Analysis of Test Samples RR29 Report Form for Ascorbic Acid Solid Control Material Preparation RR29 Report Form for Control Material and Test Sample Analyses
NISI 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.
Dilute Solution 2: Weigh 0.250 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.
Dilute Solution 3: Weigh 0.125 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 = 29.4 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 recalibrate 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 at 301975-3120 or jbthomas@NIST.gov. 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).
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Participant #: Date:
Vitamin C Round Robin 29 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
Mass of 5% MPA Diluent added to the 100 mL volumetric flask .................__________ g
Absorbance of Dilute Solution 1 at 242 nm...................................................__________ AU
Absorbance of Dilute Solution 1 at 243 nm...................................................__________ AU
Absorbance of Dilute Solution 1 at 244 nm...................................................__________ AU
Absorbance of Dilute Solution 1 at 245 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
Calculated [TAA]DS2......................................................................................__________ μmol/L
DILUTE SOLUTION 3
Mass of added stock solution (0.125 mL) ......................................................__________ g
Mass of 5% MPA Diluent added to the 100 mL volumetric flask .................__________ g
Calculated [TAA]DS3......................................................................................__________ μmol/L
Please return before 12-Sep-2008 MMQAP Fax: 301-977-0685 100 Bureau Drive, Stop 8392 Email: david.duewer@nist.gov Gaithersburg, MD 20899-8392
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Participant #: Date:
Vitamin C Round Robin 29 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
Dilute Solution 2 μmol/L of Dilute Solution
Dilute Solution 3 μmol/L of Dilute Solution
5% MPA Diluent μmol/L of Diluent
μmol/L of Sample CS #2 Target: 28.1 ±1.0 μmol/L
Serum Test Sample #15 μmol/L of Sample
Serum Test Sample #73 μmol/L of Sample
Serum Test Sample #90 μmol/L of Sample
Serum Test Sample #111 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 before 12-Sep-2008 MMQAP Fax: 301-977-0685 100 Bureau Drive, Stop 8392 Email: david.duewer@nist.gov Gaithersburg, MD 20899-8392
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Participant #: ________ Date: _____________
Vitamin C Round Robin 29 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 #15 Liquid frozen (1:1 serum:10% MPA) VitC #73 Liquid frozen (1:1 serum:10% MPA) VitC #90 Liquid frozen (1:1 serum:10% MPA)
VitC #111 Liquid frozen (1:1 serum:10% MPA) CS #2 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 david.duewer@nist.gov)
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: David.Duewer@NIST.gov
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Appendix F. Final Report for RR29
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.
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November 25, 2008
Dear Colleague:
UNITED STATES DEPARTMENT OF COMMERCE National lnatimte Df St:andarda and Technology Gaithersburg, Maryland 2089!}.
Enclosed is the summary report of the results for Round Robin 29 (RR29) 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 I 00 xMADe/median.
RR 29 consisted of four test samples (#15, #73, #90, and #111), one serum control material (CS#2), 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 iaboratory'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 first vitamin C round robin (RR30) of the 2009 M2QAP will be shipped during the week of December 8, 2009. If you have questions or concerns regarding this report, please contact David Duewer at 301-975-3935; e-mail: david.duewer@nist.gov or me at 301-975-3120; e-mail: jbthomas@nist ov; fax: 301-977-0685.
. -t..-t anice Brown Tho esearch Chemist
7\.nalytical Chemistry Division Chemical Science and Technology Laboratory
Enclosures
Cc: L. C. Sander D.L. Duewer
NISI
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The NIST M2QAP Vitamin C Round Robin 29 (RR29) 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 RR29 sample measurements.
Page “All Lab” Report 1 A tabulation of results and summary statistics for Total Ascorbic Acid [TAA] in the RR29
samples and control/calibration solutions.
Serum-based Samples. One serum control and four unknowns were distributed in RR29. CS#2 SRM 970 level 2, ampouled in mid-1998. S29:1 A “blank” stripped serum, ampouled in late 2001, previously distributed as sample S19:1
(RR19, 9/03), S21:1 (RR21, 9/04), S23:1 (RR23, 9/05), and S26:1 (RR26, 3/07).
S29:1 SRM 970 level 1, ampouled in mid-1998.
S29:2 SRM 970 level 2, amp