Simultaneous Determination of Vitamins D2 and D3 by LC-MS/MS in Infant Formula and Adult Nutritionals: First Action 2011.13

Autor: Donald L Gilliland, Charles K Black, James E Denison, Charles T Seipelt, Dawn Dowell
Rok vydání: 2012
Předmět:
Zdroj: Journal of AOAC INTERNATIONAL. 95:583-587
ISSN: 1944-7922
1060-3271
DOI: 10.5740/jaoacint.cs2011_13
Popis: During the “Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting” held on June 29, 2011, an Expert Review Panel (ERP) on behalf of AOAC INTERNATIONAL adopted the method “Simultaneous Determination of Vitamins D2 and D3 by LC-MS/MS in Infant Formula and Adult Nutritionals” as an AOAC Official First Action method. Vitamins D2 and D3 are extracted from the sample using pentane–ether; the extract is collected and dried under nitrogen. Vitamin D is separated from interfering compounds using UPLC, and quantitated using tandem mass spectrometry (MS/MS). Preliminary data showed the intermediate precision ranged from 3.34–8.05% and an accuracy range of 98.5–111% over the samples tested for vitamin D3. For vitamin D2, the intermediate precision ranged from 2.37–5.45% and accuracy ranged from 96.4–104% over the four matrixes evaluated. The analytical range for the method is bounded by the concentrations of the working standards, 21–270 ng/mL, and is equivalent to 0.168–2.16 mcg/100 g in ready-to-feed product. The practical method quantitation limit is 0.168 mcg/100 g product with method detection limit of 60 ng/100 g product. The ERP reviewed the data and determined that the performance characteristics of the method met the standard method performance requirements, and therefore the method was granted First Action status.
Databáze: OpenAIRE