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‘Dilute‐and‐Shoot’ Method for Vitamin D Analysis in Dietary Supplement Capsules
Author(s) -
Byrdwell William Craig
Publication year - 2011
Publication title -
the faseb journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.709
H-Index - 277
eISSN - 1530-6860
pISSN - 0892-6638
DOI - 10.1096/fasebj.25.1_supplement.996.5
Subject(s) - atmospheric pressure chemical ionization , chemistry , chromatography , chromatography detector , mass spectrometry , vitamin , rice bran oil , electrospray ionization , bran , chemical ionization , high performance liquid chromatography , ionization , biochemistry , ion , organic chemistry , raw material
Three methods are demonstrated for a complete analysis of vitamin D and triacylglycerols (TAGs) in fortified dietary supplements that virtually eliminates all chemical pretreatment prior to analysis. Three mass spectrometers, in parallel, plus a UV detector, an evaporative light scattering detector (ELSD), and a corona charged aerosol detector (CAD), were used simultaneously. The contents of gelcaps labeled as containing 1000 IU (25 mcg) vitamin D 3 in safflower oil and 2000 IU (50 mcg) vitamin D 3 in rice bran oil were analyzed without the need for lengthy saponification and extraction. Three to five gelcaps were analyzed using vitamin D 2 as an internal standard. Vitamin D 3 was analyzed using UV detection, selected ion monitoring (SIM) atmospheric pressure chemical ionization mass spectrometry (APCI‐MS), and two transitions of multiple reaction monitoring (MRM) APCI‐MS. TAGs in the oils were analyzed using full‐scan APCI‐MS, electrospray ionization (ESI) MS, up to MS 4 , plus two auxiliary detectors‐‐‐the ELSD and CAD. TAGs containing fatty acids up to 28 carbons in length were identified. The vitamin D contents of the gelcaps exceeded label values, and additional chromatographic peaks appeared when the source of vitamin D 3 was fish oil (safflower oil gelcap) versus synthetic vitamin D 3 (rice bran oil gelcap).