高效液相色谱-串联质谱联用测定脂肪中乙酰孕激素残留

Analysis of Acetylgestagens Residues in Animal Fat by Liquid Chromatography Tandem Mass Spectrometry

建立了脂肪中5种乙酰孕激素,包括醋酸甲羟孕酮(MPA)、醋酸氯地孕酮(CMA)、醋酸甲地孕酮(MEGA)、甲烯雌醇醋酸酯(MLA)及17α-羟基孕酮醋酸酯(HPA)的液相色谱-串联质谱(LC-MS/MS)检测方法。考察了脂肪样品溶剂提取、固相萃取净化对样品分析的影响,确定样品各前处理过程的条件。采用电喷雾(ESI)阳离子,在选择反应监测模式(SRM)下,本方法对5种乙酰孕激素的检出限为0.2～0.3μg/kg,定量限为0.5μg/kg。在空白猪脂肪样品中以0.5、1.0和5.0μg/kg3个水平添加时,5种乙酰孕激素的回收率范围在60.5%～84.1%,RSD为8.9%～16.8%。

A sensitive method was developed for quantitative detection of 5 acetylgestagens residues in animal fat tissues. The effects of solvent extraction and clean-up by solid phase extraction column on the fat sample analysis were investigated. The acetylgestagens were confirmed and quantified using a liquid chromatography tandem mass spectrometry in the selective reaction monitoring mode via positive electrospray ionization. The limits of detection ranged from 0.2 to 0.3 μg/kg and the limits of quantification were 0.5 μg/kg. When fat samples were fortified acetylgestagens at 0.5, 1.0 and 5.0 μg/kg levels, the mean recoveries were in the range of 60.5% -84.1% and the relative standard deviation （RSD） were in the range of 8.9% -16.8%.