畜禽肉及鸡蛋等动物源性食品中44种多兽药残留检测超高效液相色谱-串联质谱法

Simultaneous Determination of 44 Veterinary Drug Residues of in Animal Products Such as Livestock and Poultry Meat and Eggs Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了一种快速、准确测定畜禽肉及鸡蛋等动物源性食品中44种兽药残留检测的超高效液相色谱-质谱法(UPLC-MS/MS)定性定量检测方法。选取猪肉、鸡肉、鸡蛋3种代表性基质,样品经80%乙腈溶液(含0.2%甲酸)提取,采用Prime HLB固相萃取柱净化、C_(18)色谱柱分离,以0.1%甲酸水和乙腈为流动相进行梯度洗脱,电喷雾电离(ESI^(+)、ESI^(-)),多反应监测模式扫描(MRM)。37种兽药采用基质外标法定量,7种兽药采用基质内标法定量。结果表明,44种兽药的线性范围为0.50~100 ng/mL,相关系数均大于0.9950,检出限范围为1.0~10.0μg/kg,定量限为3.0~30.0μg/kg。3种基质3个水平的添加回收率分别为64.9%~108.0%,62.5%~107.0%,66.4%~111.0%,相对标准偏差(RSD)(n=6)均小于15%;该方法可高效率提取多种兽药,去除干扰杂质,具有简单、快速、灵敏、准确等优点,适用于快速畜禽肉及鸡蛋等动物源性食品多兽药残留的检测。

A rapid and accurate ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS)method was established for qualitative and quantitative determination of 44 kinds of veterinary drugs residues in animal products such as livestock and poultry meat and eggs.The method selected the pork,chicken,eggs as three kinds of typical matrix.The analytes were extracted from the samples by 0.2%formic acid in80%acetonitrile,then purified by Prime HLB.The analytes were seperated on a C_(18) chromatographic column by gradient elution with 0.1%formic acid water and acetonitrile as the mobile phases.Mass spectrometry was conducted by electrospray ionization(ESI^(-)and ESI^(+))and multi response monitoring mode(MRM).37 kinds of veterinary drugs were quantified by matrix external standard method and 7 drugs were quantified by matrix internal standard method.The results showed that there were good linear relationships for 44 veterinary drugs in the range of 0.5~100 ng/mL with the correlation coefficients not less than 0.9950.The limits of detection were 1.0~10.0μg/kg,the limits of quantification were 3.0~30.0μg/kg.The recoveries of pork,chicken and egg for three levels were 64.9%~108.0%,62.5%~107.0%,66.4%~111.0%respectively and the relative standard deviations(RSD)(n=6)was less than 15%.The established method was easy to operate,senstive with good purification effct and was suitable for rapid screening and determination of veterinary drug residues in animal products such as livestock and poultry meat and eggs.