A confirmatory method was developed and validated for the simultaneous determination of four acetylgestagens residues,including flurogestone acetate(FGA),melengestrol acetate(MGA),megestrol acetate(MA) and chlormadinone acetate(CMA)in ovine milk using high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS) method.The analytes were extracted from milk with acetonitrile,defatted with freezing-lipid filtration,and then the extract was purified with C18 solid-phase extraction column.The analytes were analyzed by HPLC-MS/MS in positive multiple reaction monitoring(MRM)mode. Two product ions from each of the chosen precursor ions were acquired for confirmation of the acetylgestagens.Good linearities were achieved with correlation coefficients not less than 0.999 6 for all analytes in the concentration of 0.5-20 μg/L.The limits of detection were 0.2,0.2,0.1,0.1 μg/kg for FGA,CMA,MGA,MA,respectively,with limits of quantitation of 0.5 μg/kg.Recoveries for the ovine milk fortified at levels of 0.5,1.0,2.0,10 μg/kg were in the range of 87%-96%,with RSDs of 4.5%-9.1%.The developed method is sensitive and accurate,and is suitable for the simultaneous detection of these acetylgestagens in ovine milk.
关键词
乙酰孕激素羊奶残留高效液相色谱-串联质谱
Keywords
acetylgestagensovine milkresiduehigh performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
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Related Institution
Key Laboratory of Tropical Fruits and Vegetables Quality and Safety for State Market Regulation;Hainan Institute for Food Control
Tea Research Institute,Chinese Academy of Agricultural Sciences
Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables;Key Laboratory of Quality and Safety Control for Subtropical Fruit and Vegetable,Ministry of Agriculture and Rural Affairs;Analysis and Test Center,Chinese Academy of Tropical Agricultural Sciences
College of Horticulture and Landscape,Tianjin Agricultural University