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relative ionisation and fragmentation efficiencies of vitamin D to pre-vitamin D are not known; (2) the pre-
vitamin D peak may have been subject to different ion suppression from the vitamin D peak, making
accurate quantitation of this form difficult; (3) the pre-vitamin D transition showed a peak area of 1% of the
peak area of vitamin D making reliable integration difficult.
Assuming that pre-vitamin D and vitamin D in the sample after saponification have reached equilibrium, and
that the equilibrium constant and kinetic as are the same for the analyte and isotope labelled forms of
vitamin D, this method does not distinguish between contribution from either form and measures only an
aggregate result for both pre-vitamin D and vitamin D. This satisfies the requirement of the applicability
statement of the SMPR [2].
Acknowledgements
Harvey Indyk, Senior Research Scientist for his advice and technical expertise.
References
(1) Gill, B.D.; Indyk, H.E.; Blake, C.J.; Konings, E.J.M.; Jacobs, W.A.; Sullivan, D. (2015) Evaluation
protocol for the review of method validation data by the AOAC Stakeholder Panel on Infant Formula
and Adult Nutritionals Expert Review Panel.
Journal of AOAC International
98, 112
–
115.
(2) Official Methods of Analysis: AOAC SMPR 2011.004.
(3) Gill, B.D.; Zhu, X.; Indyk, H.E. (2015) A rapid method for the determination of vitamin D3 in milk and
infant formula by liquid chromatography-mass spectrometry.
Journal of AOAC International
98, 431
–
435.
(4) Horwitz, W.; Albert, R. (2006)
Journal of AOAC International
89, 1095
–
1109.
(5) Shimizu, M., Yamada S. (1994)
Vitamins
68,15
–
30 cited in: Ding, S.; Schoenmakers, I.; Jones, K.;
Koulman, A.; Prentice, A.; Volmer, D.A. (2010). Quantitative determination of vitamin D metabolites in
plasma using UHPLC-MS/MS.
Analytical and Bioanalytical Chemistry
398, 779
–
789.
(6) Abernethy, G.A. (2012) A rapid analytical method for cholecalciferol (vitamin D3) in fortified infant
formula, milk and milk powder using Diels
–
Alder derivatisation and liquid chromatography
–
tandem
mass spectrometric detection.
Analytical and Bioanalytical Chemistry
402, 1433
–
1440.
VitD-18 (February 2016)
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