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Food Chem. 2013 Jun 1;138(2-3):1042-7. doi: 10.1016/j.foodchem.2012.08.041. Epub 2012 Aug 30.

Vitamin D and 25-hydroxyvitamin D determination in meats by LC-IT-MS.

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National Measurement Institute (NMI), 1/153 Bertie Street, Port Melbourne, Victoria 3207, Australia.


This paper reports a method for the rapid, sensitive and simultaneous analysis of vitamin D (Vit D) and 25-hydroxyvitamin D (25OH-Vit D) in meats. Samples were saponified and underwent solid phase extraction with analysis by normal phase liquid chromatography (LC) with ion trap mass spectroscopy (IT-MS), using positive polarity atmospheric pressure chemical ionisation (APCI). Limits of detection (LOD) and quantification (LOQ) for Vit D and 25OH-Vit D were 0.03 and 0.05 μg/100g respectively. Deuterium labelled Vit D and 25OH-Vit D internal standards were added as surrogates prior to saponification, correcting for extraction inefficiencies and potential MS matrix enhancement or suppression effects. Recoveries using internal/surrogate standard correction ranged from 80% to 100% for all vitamers. Measurement uncertainty ranged from 6% to 15% for all vitamers in this method. This process required only 7.5 g of sample per extraction and a batch of 28 extractions could be completed in six hours.

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