Determination of cholecalciferol (vitamin D3) in selected foodsĭimartino G (2007) Convenient analysis of vitamin D in cheese and other food matrixes by liquid chromatography/mass spectrometry. Significantly for routine laboratories, the method returns results within 2 h, generates minimal waste and minimises health and safety concerns to the analyst.ĪOAC (2002) Official methods of analysis 2002.05. The repeatability standard deviation was 4.23 %. The method has been subjected to a single-laboratory validation and has been found to be linear, highly selective and accurate with respect to National Institute of Standards and Technology Standard Reference Material 1849, analyte spiking experiments and comparison with an LC–UV-based method. An internal standard, deuterium-labelled VD3, was used to correct for losses in extraction and any variation in derivatisation and ionisation efficiencies. Detection was by triple quadrupole mass spectrometer using a selective transition, m/z 560 → 298. The analyte was then re-extracted into a small volume of acetonitrile and analysed by reverse-phase chromatography. A portion of the isooctane layer was then transferred, and an aliquot of 4-phenyl-1,2,4-triazoline-3,5-dione was added to derivatise VD3.
Milk or reconstituted milk powder was solubilised in methanol and extracted in one step into isooctane, which was separated by centrifugation.
This method is rapid and cost effective and is intended for use in quality control in the manufacture of fortified infant formulae and milk powders. A method for analysing vitamin D 3 (VD3, cholecalciferol) has been established and validated.
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