液相色谱串联质谱法快速测定牛奶与鸡蛋中的维吉霉素M_1残留量  

Quick Determination of Virginiamycin M1 Residue in Milk and Egg Using Liquid Chromatography Tandem Mass Spectrometry

作　　者：陈小霞[1] 岳振峰[2] 叶卫翔[2] 赵凤娟[2] 张建莹[2] 侯乐锡[2] 林黎[2] 

机构地区：[1]深圳大学教务处,广东深圳518060 [2]深圳出入境检验检疫局食品检验检疫技术中心,广东深圳518067

出　　处：《分析测试学报》2009年第11期1328-1331,共4页Journal of Instrumental Analysis

摘　　要：建立了牛奶和鸡蛋样品中维吉霉素M1残留的液质联用确证方法。用乙腈萃取样品中的维吉霉素M1残留，水稀释后，正己烷脱脂，以YMC—Pack Pro C18色谱柱为分离柱，在正离子模式下以电喷雾电离串联质谱仪进行测定。方法的线性范围为2．5～25μg/L，定量下限为50μg／kg。在50、100、200μg/kg 3个浓度水平进行加标回收实验，回收率为72％～99％，相对标准偏差为2．7％～6．1％。该方法简便、快速、准确，各项技术指标满足国内外法规的要求，可用于牛奶和鸡蛋样品中维吉霉素M1残留的快速确证检测。A confirmative method was developed with liquid chromatography tandem mass spectrometry （LC- MS/MS） to detect virginiamycin M1 residue in milk and egg. The sample was extracted with acetonitrile, then diluted with water and cleaned up with hexane. The extract was analyzed by LC - MS/MS under positive mode using a YMC-Pack Pro C18 column as the analytical column. The result indicated that the calibration curve was linear for virginiamycin M1 concentration in the range of 2.5-25 μg/L with quantification limit of 50 μg/kg. The recoveries of virginiamycin M1 from egg and milk matrices at three spiked concentration levels of 50, 100 and 200 μg/kg ranged from 72% to 99% with relative standard deviations of 2.7% -6. 1% . The method was simple, rapid, and accurate, and its performance could meet the requirement of the domestic and international legislation. Therefore, the method was suitable for quickly confirmation of virginiamycin M1 residue in milk and egg samples.

关 键 词：液相色谱串联质谱 牛奶 鸡蛋 维吉霉素M1 残留 

分 类 号：O657.63[理学—分析化学] O652.63[理学—化学]