分析测试学报2012，Vol.31Issue(10)：1314-1318,5.DOI:10.3969/j.issn.1004-4957.2012.10.018
高效液相色谱-串联质谱法检测羊奶中乙酰孕激素多残留研究
Determination of Acetylgestagens in Ovine Milk by High Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
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 G]8 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Key words
acetylgestagens/ ovine milk/ residue/ high performance liquid chromatography - tandem mass spectrometry (HPLC -MS/MS)分类
化学化工引用本文复制引用
方秋华,黄显会,郭春娜,杨刚,孔祥凯..高效液相色谱-串联质谱法检测羊奶中乙酰孕激素多残留研究[J].分析测试学报,2012,31(10):1314-1318,5.基金项目
2010 农业行业标准制定与修订项目 （）
