Review Team (February 2016)

Fonterra Co-operative Group VitD-18 (February 2016) FOR ERP USE ONLY DO NOT DISTRIBUTE

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.

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