Interlaboratory comparison of 25-hydroxyvitamin D assays: Vitamin D Standardization Program (VDSP) Intercomparison Study 2 - Part 1 liquid chromatography - tandem mass spectrometry (LC-MS/MS) assays - impact of 3-epi-25-hydroxyvitamin D(3) on assay performance.
Wise, Stephen A.; Camara, Johanna E.; Burdette, Carolyn Q.et al.
2022 • In Analytical and Bioanalytical Chemistry, 414 (1), p. 333-349
24R,25-Dihydroxyvitamin D3 (24R,25(OH)3D3); 25-Hydroxyvitamin D2 (25(OH)D2); 25-Hydroxyvitamin D3 (25(OH)D3); 3-epi-25-Hydroxyvitamin D3 (3-epi-25(OH)D3); Liquid chromatography – tandem mass spectrometry (LC-MS/MS); Total serum 25-hydroxyvitamin D (25(OH)D)
Abstract :
[en] An interlaboratory comparison study was conducted by the Vitamin D Standardization Program (VDSP) to assess the performance of liquid chromatography - tandem mass spectrometry (LC-MS/MS) assays used for the determination of serum total 25-hydroxyvitamin D (25(OH)D), which is the sum of 25-hydroxyvitamin D(2) (25(OH)D(2)) and 25-hydroxyvitamin D(3) (25(OH)D(3)). A set of 50 single-donor samples was assigned target values for concentrations of 25(OH)D(2), 25(OH)D(3), 3-epi-25-hydroxyvitamin D(3) (3-epi-25(OH)D(3)), and 24R,25-dihydroxyvitamin D(3) (24R,25(OH)(2)D(3)) using isotope dilution liquid chromatography - tandem mass spectrometry (ID LC-MS/MS). VDSP Intercomparison Study 2 Part 1 includes results from 14 laboratories using 14 custom LC-MS/MS assays. Assay performance was evaluated using mean % bias compared to the assigned target values and using linear regression analysis of the test assay mean results and the target values. Only 53% of the LC-MS/MS assays met the VDSP criterion of mean % bias ≤ |±5%|. For the LC-MS/MS assays not meeting the ≤ |±5%| criterion, four assays had mean % bias of between 12 and 21%. Based on multivariable regression analysis using the concentrations of the four individual vitamin D metabolites in the 50 single-donor samples, the performance of several LC-MS/MS assays was found to be influenced by the presence of 3-epi-25(OH)D(3). The results of this interlaboratory study represent the most comprehensive comparison of LC-MS/MS assay performance for serum total 25(OH)D and document the significant impact of the lack of separation of 3-epi-25(OH)D(3) and 25(OH)D(3) on assay performance, particularly with regard to mean % bias.
Disciplines :
Laboratory medicine & medical technology
Author, co-author :
Wise, Stephen A.
Camara, Johanna E.
Burdette, Carolyn Q.
Hahm, Grace
Nalin, Federica
Kuszak, Adam J.
Merkel, Joyce
Durazo-Arvizu, Ramón A.
Williams, Emma L.
Hoofnagle, Andrew N.
Ivison, Fiona
Fischer, Ralf
van den Ouweland, Jody M. W.
Ho, Chung S.
Law, Emmett W. K.
Simard, Jean-Nicolas
Gonthier, Renaud
Holmquist, Brett
Meadows, Sarah
Cox, Lorna
Robyak, Kimberly
Creer, Michael H.
Fitzgerald, Robert
Clarke, Michael W.
Breen, Norma
LUKAS, Pierre ; Centre Hospitalier Universitaire de Liège - CHU > Unilab > Bone and cartilage markers laboratory
Cavalier, Etienne ; Université de Liège - ULiège > Département de pharmacie > Chimie médicale
Interlaboratory comparison of 25-hydroxyvitamin D assays: Vitamin D Standardization Program (VDSP) Intercomparison Study 2 - Part 1 liquid chromatography - tandem mass spectrometry (LC-MS/MS) assays - impact of 3-epi-25-hydroxyvitamin D(3) on assay performance.
Binkley N, Dawson-Hughes B, Durazo-Arvizu R, Thamm M, Tian L, Merkel JM, et al. Vitamin D measurement standardization: the way out of the chaos. J Steroid Biochem Mol Biol. 2017;173:117–21. 10.1016/j.jsbmb.2016.12.002. DOI: 10.1016/j.jsbmb.2016.12.002
Binkley N, Krueger D, Cowgill CS, Plum L, Lake E, Hansen KE, et al. Assay variation confounds the diagnosis of hypovitaminosis D: a call for standardization. J Clin Endocrinol Metab. 2004;89(7):3152–7. 10.1210/jc.2003-031979. DOI: 10.1210/jc.2003-031979
Wise SA, Phinney KW, Tai SSC, Camara JE, Myers GL, Durazo-Arvizu R, et al. Baseline assessment of 25-hydroxyvitamin D assay performance: a Vitamin D Standardization Program (VDSP) interlaboratory comparison study. J AOAC Int. 2017;100(5):1244–52. 10.5740/jaoacint.17-0258. DOI: 10.5740/jaoacint.17-0258
Sempos CT, Binkley N. 25-Hydroxvitamin D assay standardization and vitamin D guidelines paralysis. Public Health Nutrition. 2020;23(7):1153–64. 10.1017/S1368980019005251. DOI: 10.1017/S1368980019005251
Barake M, Daher RT, Salti I, Cortas NK, Al-Shaar L, Habib RH, et al. 25-Hydroxyvitamin D assay variations and impact on clinical decision making. J Clin Endocrinol Metab. 2012;97(3):835–43. 10.1210/jc.2011-2584. DOI: 10.1210/jc.2011-2584
Black LJ, Anderson D, Clarke MW, Ponsonby AL, Lucas RM, Ausimmune Investigator Group. Analytical bias in the measurement of serum 25-hydroxyvitamin D concentrations impairs assessment of vitamin D status in clinical and research settings. PLoS One. 2015;10(8):14. 10.1371/journal.pone.0135478. DOI: 10.1371/journal.pone.0135478
Altieri B, Cavalier E, Bhattoa HP, Perez-Lopez FR, Lopez-Baena MT, Perez-Roncero GR, et al. Vitamin D testing: advantages and limits of the current assays. European Journal of Clinical Nutrition. 2020;74(2):231–47. 10.1038/s41430-019-0553-3. DOI: 10.1038/s41430-019-0553-3
Bivona G, Lo Sasso B, Iacolino G, Gambino CM, Scazzone C, Agnello L, et al. Standardized measurement of circulating vitamin D 25(OH)D and its putative role as a serum biomarker in Alzheimer's disease and Parkinson's disease. Clin Chim Acta. 2019;497:82–7. 10.1016/j.cca.2019.07.022. DOI: 10.1016/j.cca.2019.07.022
Bjerg LN, Halgreen JR, Hansen SH, Morris HA, Jorgensen NR. An evaluation of total 25-hydroxyvitamin D assay standardization: Where are we today? J Steroid Biochem Mol Biol. 2019;190:224–33. 10.1016/j.jsbmb.2019.03.015. DOI: 10.1016/j.jsbmb.2019.03.015
Dirks NF, Martens F, Vanderschueren D, Billen J, Pauwels S, Ackermans MT, et al. Determination of human reference values for serum total 1,25-dihydroxyvitamin D using an extensively validated 2D ID-UPLC-MS/MS method. J Steroid Biochem Mol Biol. 2016;164:127–33. 10.1016/j.jsbmb.2015.12.003. DOI: 10.1016/j.jsbmb.2015.12.003
Fraser WD, Tang JCY, Dutton JJ, Schoenmakers I. Vitamin D measurement, the debates continue, new analytes have emerged, developments have variable outcomes. Calcified Tissue International. 2020;106(1):3–13. 10.1007/s00223-019-00620-2. DOI: 10.1007/s00223-019-00620-2
Herrmann M, Farrell CJL, Pusceddu I, Fabregat-Cabello N, Cavalier E. Assessment of vitamin D status - a changing landscape. Clin Chem Lab Med. 2017;55(1):3–26. 10.1515/cclm-2016-0264. DOI: 10.1515/cclm-2016-0264
Makris K, Sempos C, Cavalier E. The measurement of vitamin D metabolites: part I-metabolism of vitamin D and the measurement of 25-hydroxyvitamin D. Horm-Int J Endocrinol Metab. 2020;19(2):81–96. 10.1007/s42000-019-00169-7. DOI: 10.1007/s42000-019-00169-7
Makris K, Sempos C, Cavalier E. The measurement of vitamin D metabolites part II-the measurement of the various vitamin D metabolites. Horm-Int J Endocrinol Metab. 2020;19(2):97–107. 10.1007/s42000-020-00188-9. DOI: 10.1007/s42000-020-00188-9
Stokes CS, Lammert F, Volmer DA. Analytical methods for quantification of vitamin D and implications for research and clinical practice. Anticancer Res. 2018;38(2):1137–44. 10.21873/anticanres.12332. DOI: 10.21873/anticanres.12332
Sempos CT, Vesper HW, Phinney KW, Thienpont LM, Coates PM, VDSP. Vitamin D status as an international issue: national surveys and the problem of standardization. Scand J Clin Lab Invest. 2012;72:32–40. 10.3109/00365513.2012.681935. DOI: 10.3109/00365513.2012.681935
Wise SA, Tai SSC, Burdette CQ, Camara JE, Bedner M, Lippa KA, et al. Role of the National Institute of Standards and Technology (NIST) in support of the vitamin D initiative of the National Institutes of Health, Office of Dietary Supplements. J AOAC Int. 2017;100(5):1260–76. 10.5740/jaoacint.17-0305. DOI: 10.5740/jaoacint.17-0305
Tai SSC, Bedner M, Phinney KW. Development of a candidate reference measurement procedure for the determination of 25-hydroxyvitamin D3 and 25-hydroxyvitamin D2 in human serum using isotope-dilution liquid chromatography-tandem mass spectrometry. Anal Chem. 2010;82(5):1942–8. 10.1021/ac9026862. DOI: 10.1021/ac9026862
Tai SSC, Nelson MA. Candidate reference measurement procedure for the determination of (24R),25-dihydroxyvitamin D3 in human serum using isotope-dilution liquid chromatography-tandem mass spectrometry. Anal Chem. 2015;87(15):7964–70. 10.1021/acs.analchem.5b01861. DOI: 10.1021/acs.analchem.5b01861
Stepman HCM, Vanderroost A, Van Uytfanghe K, Thienpont LM. Candidate reference measurement procedures for serum 25-hydroxyvitamin D-3 and 25-hydroxyvitamin D-2 by using isotope-dilution liquid chromatography-tandem mass spectrometry. Clin Chem. 2011;57(3):441–8. 10.1373/clinchem.2010.152553. DOI: 10.1373/clinchem.2010.152553
Mineva EM, Schleicher RL, Chaudhary-Webb M, Maw KL, Botelho JC, Vesper HW, et al. A candidate reference measurement procedure for quantifying serum concentrations of 25-hydroxyvitamin D3 and 25-hydroxyvitamin D2 using isotope-dilution liquid chromatography-tandem mass spectrometry. Anal Bioanal Chem. 2015;407(19):5615–24. 10.1007/s00216-015-8733-z. DOI: 10.1007/s00216-015-8733-z
Phinney KW, Bedner M, Tai SSC, Vamathevan VV, Sander LC, Sharpless KE, et al. Development and certification of a Standard Reference Material for vitamin D metabolites in human serum. Anal Chem. 2012;84(2):956–62. 10.1021/ac202047n. DOI: 10.1021/ac202047n
Phinney KW, Tai SSC, Bedner M, Camara JE, Chia RRC, Sander LC, et al. Development of an improved Standard Reference Material for vitamin D metabolites in human serum. Anal Chem. 2017;89(9):4907–13. 10.1021/acs.analchem.6b05168. DOI: 10.1021/acs.analchem.6b05168
Tai SSC, Nelson MA, Bedner M, Lang BE, Phinney KW, Sander LC, et al. Development of Standard Reference Material (SRM) 2973 vitamin D metabolites in frozen human serum (high level). J AOAC Int. 2017;100(5):1294–303. 10.5740/jaoacint.17-0182. DOI: 10.5740/jaoacint.17-0182
CDC Vitamin D Standardization — Certification Program https://www.cdc.gov/labstandards/vdscp.html Accessed 13 Jul 2021
Erdman P, Palmer-Toy DE, Horowitz G, Hoofnagle A. Accuracy-based vitamin D survey six years of quality improvement guided by proficiency testing. Arch Pathol Lab Med. 2019;143(12):1531–8. 10.5858/arpa.2018-0625-CP. DOI: 10.5858/arpa.2018-0625-CP
Carter GD, Berry J, Durazo-Arvizu R, Gunter E, Jones G, Jones J, et al. Hydroxyvitamin D assays: an historical perspective from DEQAS. J Steroid Biochem Mol Biol. 2018;177:30–5. 10.1016/j.jsbmb.2017.07.018. DOI: 10.1016/j.jsbmb.2017.07.018
Burdette CQ, Camara JE, Nalin F, Pritchett J, Sander LC, Carter, et al. Establishing an accuracy basis for the Vitamin D External Quality Assessment Scheme (DEQAS). J AOAC Int. 2017;100(5):1277–87. 10.5740/jaoacint.17-0306. DOI: 10.5740/jaoacint.17-0306
Binkley N, Sempos CT, VDSP. Standardizing vitamin D assays: the way forward. J Bone Miner Res. 2014;29(8):1709–14. 10.1002/jbmr.2252. DOI: 10.1002/jbmr.2252
Stockl D, Sluss PM, Thienpont LM. Specifications for trueness and precision of a reference measurement system for serum/plasma 25-hydroxyvitamin D analysis. Clin Chim Acta. 2009;408(1-2):8–13. 10.1016/j.cca.2009.06.027. DOI: 10.1016/j.cca.2009.06.027
Phinney KW, Sempos CT, Tai SSC, Camara JE, Wise SA, Eckfeldt JH, et al. Baseline assessment of 25-hydroxyvitamin D reference material and proficiency testing/external quality assurance material commutability: A Vitamin D Standardization Program Study. J AOAC Int. 2017;100(5):1288–93. 10.5740/jaoacint.17-0291. DOI: 10.5740/jaoacint.17-0291
Annema W, Nowak A, von Eckardstein A, Saleh L. Evaluation of the new restandardized Abbott Architect 25-OH Vitamin D assay in vitamin D-insufficient and vitamin D-supplemented individuals. J Clin Lab Anal. 2018;32(4):5. 10.1002/jcla.22328. DOI: 10.1002/jcla.22328
Cavalier E, Delanaye P, Lukas P, Carlisi A, Gadisseur R, Souberbielle JC. Standardization of DiaSorin and Roche automated third generation PTH assays with an International Standard: impact on clinical populations. Clin Chem Lab Med. 2014;52(8):1137–41. 10.1515/cclm-2013-1027. DOI: 10.1515/cclm-2013-1027
Cavalier E, Lukas P, Bekaert AC, Carlisi A, Le Goff C, Delanaye P, et al. Analytical and clinical validation of the new Abbot Architect 25(OH) D assay: fit for purpose? Clin Chem Lab Med. 2017;55(3):378–84. 10.1515/cclm-2016-0566. DOI: 10.1515/cclm-2016-0566
Cavalier E, Lukas P, Bekaert AC, Peeters S, Le Goff C, Yayo E, et al. Analytical and clinical evaluation of the new Fujirebio Lumipulse (R) G non-competitive assay for 25(OH)-vitamin D and three immunoassays for 25(OH) D in healthy subjects, osteoporotic patients, third trimester pregnant women, healthy African subjects, hemodialyzed and intensive care patients. Clin Chem Lab Med. 2016;54(8):1347–55. 10.1515/cclm-2015-0923. DOI: 10.1515/cclm-2015-0923
Cavalier E, Lukas P, Crine Y, Peeters S, Carlisi A, Le Goff C, et al. Evaluation of automated immunoassays for 25(OH)-vitamin D determination in different critical populations before and after standardization of the assays. Clin Chim Acta. 2014;431:60–5. 10.1016/j.cca.2014.01.026. DOI: 10.1016/j.cca.2014.01.026
Depreter B, Heijboer AC, Langlois MR. Accuracy of three automated 25-hydroxyvitamin D assays in hemodialysis patients. Clin Chim Acta. 2013;415:255–60. 10.1016/j.cca.2012.10.056. DOI: 10.1016/j.cca.2012.10.056
Elsenberg E, ten Boekel E, Huijgen H, Heijboer AC. Standardization of automated 25-hydroxyvitamin D assays: how successful is it? Clin Biochem. 2017;50(18):1126–30. 10.1016/j.clinbiochem.2017.06.011. DOI: 10.1016/j.clinbiochem.2017.06.011
Heijboer AC, Blankenstein MA, Kema IP, Buijs MM. Accuracy of 6 routine 25-hydroxyvitamin D assays: influence of vitamin D binding protein concentration. Clin Chem. 2012;58(3):543–8. 10.1373/clinchem.2011.176545. DOI: 10.1373/clinchem.2011.176545
Hutchinson K, Healy M, Crowley V, Louw M, Rochev Y. Verification of Abbott 25-OH-vitamin D assay on the architect system. Pract Lab Med. 2017;7:27–35. 10.1016/j.plabm.2017.01.001. DOI: 10.1016/j.plabm.2017.01.001
Lim YK, Park AJ, Kweon OJ, Choi JH. Performance evaluation and measurement uncertainty determination of the new version of the Abbott Architect 25-OH Vitamin D 5P02 Assay. Am J Clin Pathol. 2019;151(2):209–16. 10.1093/ajcp/aqy131. DOI: 10.1093/ajcp/aqy131
Moreau E, Bacher S, Mery S, Le Goff C, Piga N, Vogeser M, et al. Performance characteristics of the VIDAS (R) 25-OH Vitamin D Total assay - comparison with four immunoassays and two liquid chromatography-tandem mass spectrometry methods in a multicentric study. Clin Chem Lab Med. 2016;54(1):45–53. 10.1515/cclm-2014-1249. DOI: 10.1515/cclm-2014-1249
Wise SA, Camara JE, Sempos CT, Burdette CQ, Hahm G, Nalin F, et al. (2022) Interlaboratory comparison of 25-hydroxyvitamin D assays: Vitamin D Standardization Program (VDSP) intercomparison study 2 - Part 2 Ligand binding assays – Impact of 25-hydroxyvitamin D2 and 24R,25-dihydroxyvitamin D3 on assay performance. Anal Bioanal Chem. https://doi.org/10.1007/s00216-021-03577-0
Wise SA, Camara JE, Sempos CT, Lukas P, Le Goff C, Peeters, et al. Vitamin D Standardization Program (VDSP) Intralaboratory study for the assessment of 25-hydroxyvitamin D assay performance. J Steroid Biochem Mol Biol. 2021;212:105917. 10.1016/j.jsbmb.2021.105917. DOI: 10.1016/j.jsbmb.2021.105917
Camara JE, Wise SA, Hoofnagle AN, Williams EL, Carter GD, Jones J, et al. Assessment of serum total 25-hydroxyvitamin D assay commutability of Standard Reference Materials, College of American Pathologists Accuracy-Based Vitamin D (ABVD) Scheme and Vitamin D External Quality Assessment Scheme (DEQAS) materials: Vitamin D Standardization Program (VDSP) commutability study 2. Anal Bioanal Chem. 2021. https://doi.org/10.1007/s00216-021-03470-w.
Camara J, Hoofnagle A, Carter G, Sempos C (2015) Take Two: Gearing up for the next vitamin D commutability study. Clinical Laboratory News (February 1, 2015)
Schleicher RL, Sternberg MR, Lacher DA, Sempos CT, Looker AC, Durazo-Arvizu RA, et al. The vitamin D status of the US population from 1988 to 2010 using standardized serum concentrations of 25-hydroxyvitamin D shows recent modest increases. Am J Clin Nutr. 2016;104(2):454–61. 10.3945/ajcn.115.127985. DOI: 10.3945/ajcn.115.127985
Schleicher RL, Sternberg MR, Looker AC, Yetley EA, Lacher DA, Sempos CT, et al. National estimates of serum total 25-hydroxyvitamin D and metabolite concentrations measured by liquid chromatography-tandem mass spectrometry in the US population during 2007-2010. J Nutr. 2016;146(5):1051–61. 10.3945/jn.115.227728. DOI: 10.3945/jn.115.227728
CLSI (1999) Preparation and Validation of Commutable Frozen Human Serum Pools as Secondary Reference Materials for Cholesterol Measurement Procedures. CLSI Document C37-A. Clinical and Laboratory Standards Institute, Wayne, PA
Danilenko U, Vesper HW, Myers GL, Clapshaw PA, Camara JE, Miller WG. An updated protocol based on CLSI document C37 for preparation of off-the-clot serum from individual units for use alone or to prepare commutable pooled serum reference materials. Clin Chem Lab Med. 2020;58(3):368–74. 10.1515/cclm-2019-0732. DOI: 10.1515/cclm-2019-0732
Phinney KW, Camara JE, Tai SSC, Sander LC, Wise SA, De Grande LAC, et al. Value assignment of vitamin D metabolites in Vitamin D Standardization Program serum samples. J AOAC Int. 2017;100(5):1253–9. 10.5740/jaoacint.17-0204. DOI: 10.5740/jaoacint.17-0204
Wise SA, Tai SSC, Nelson MA, Burdette CQ, Camara JE, Hoofnagle AN, et al. Interlaboratory comparison for the determination of 24R,25-dihydroxyvitamin D-3 in human serum using liquid chromatography with tandem mass spectrometry. J AOAC Int. 2017;100(5):1308–17. 10.5740/jaoacint.17-0183. DOI: 10.5740/jaoacint.17-0183
