title: Simultaneous determination of vitamins D2 and D3 by LC-MS/MS in infant formula and adult nutritionals: First Action 2011.13.
abstract: 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.
authors: Abbott Nutrition, 3300 Stelzer Rd, Nutritional Research Center, Columbus, OH 43219, USA. don.gilliland@abbott.com
authors: Donald L
authors: DL
authors: Gilliland
authors: Charles K
authors: CK
authors: Black
authors: James E
authors: JE
authors: Denison
authors: Charles T
authors: CT
authors: Seipelt
mesh_terms: D002762:Cholecalciferol / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D004872:Ergocalciferols / Q000032:analysis*; D041943:Infant Formula / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D004872:Ergocalciferols; D002762:Cholecalciferol