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

建立了牛奶和鸡蛋样品中维吉霉素M_1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 C_(18)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 ～25 μg/L,定量下限为50 μg/kg.在50、100、200 μg/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.

Quick Determination of Virginiamycin M_1 Residue in Milk and Egg Using Liquid Chromatography Tandem Mass Spectrometry

A confirmative method was developed with liquid chromatography tandem mass spectrome-try (LC -MS/MS) to detect virginiamycin M_1 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 C_(18) column as the analytical column. The result indicated that the calibration curve was linear for virginiamycin M_1 concentration in the range of 2. 5 - 25 μg/L with quantification limit of 50 μg/kg. The recoveries of virginiamycin M_1 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 accu-rate, and its performance could meet the requirement of the domestic and international legislation. Therefore, the method was suitable for quickly confirmation of virginiamycin M_1 residue in milk and egg samples.