液相色谱三级四极杆质谱法快速测定动物组织中维吉霉素M_1残留量

Rapid Determination of Virginiamycin M_1 Residue in Animal Tissue Using Liquid Chromatography/Tandem Mass Spectrometry

建立了鸡肉、鸡肝、鸡肾、猪肾和牛肾样品中维吉霉素M1残留的液质联用确证方法。用乙腈萃取样品中维吉霉素M1残留,然后用水稀释和正己烷脱脂后,进样分析。采用YMC-PackProC18色谱柱进行分离,在正离子模式下采用电喷雾电离串联质谱仪进行测定。方法的定量限分别为:鸡肉25μg/kg、鸡肝100μg/kg、鸡肾100μg/kg、猪肾150μg/kg、牛肾100μg/kg。方法的回收率为:鸡肉86.8%-108%,鸡肝81.8%-109%,鸡肾85.5%-102%,猪肾82.7%-102%,牛肾80.7%-103%;室内相对标准偏差为:鸡肉4.3%-6.7%,鸡肝3.3%-7.3%,鸡肾2.8%-4.6%,猪肾1.9%-4.1%,牛肾3.4%-6.9%。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,可用于动物组织样品中维吉霉素M1残留量的快速确证检测。

A rapid method was developed for determination and confirmation of virginiamycin M1 residue in chicken muscle, chicken liver, chicken kidney, swine kidney, and bovine kidney using liquid chromatography/ tandem mass spectrometry （LC-MS/MS）. The virginiamycin M1 residues in samples were extracted with acetonitrile, then diluted with water and cleaned up with hexane. The sample was analyzed by LC-MS/MS in positive mode, with a YMC-Pack Pro C18 column as the analytical column. The limit quantitation （LOQ） was 25 μg/kg for chicken muscle, 100 μg/kg for chicken liver, 100 μg/kg for chicken kidney, 150 μg/kg for swine kidney, and 100 μg/kg for bovine kidney respectively. The recoveries were 86.8% - 108 % for chicken muscle, 81.8% - 109% for chicken liver, 85.5% - 102% for chicken kidney, 82.7% - 102% for swine kidney, and 80.7% - 103% for bovine with the relative standard deviations of 4.3% - 6.7 % for chicken muscle, 3.3% - 7.3% for chicken liver, 2.8% - 4.6% for chicken kidney, 1.9% -4.1% for swine kidney, and 3.4% -6.9% for bovine kidney . The method is simple, rapid, and accurate, and its performance meets the requirements of the domestic and international food safety regulations. The method is applicable for determination and confirmation of virginiamycin M1 residue in animal tissues.