基于滤过型净化的液相色谱-串联质谱法测定畜禽肉中89种兽药残留

Determination of 89 veterinary drugs in livestock and poultry meat by ultra-high performance liquid chromatography-tandem mass spectrometry based on pass-through solid phase extraction purification

建立了一种采用滤过型净化柱对畜禽肉样品进行前处理、同时测定89种兽药残留的液相色谱-串联质谱(UPLC-MS/MS)检测方法。畜禽肉用10 mL含1%(V/V)乙酸的乙腈提取,FaVEx-NM柱净化,ACQUITY BEH C18(2.1 mm×100 mm, 1.7μm)柱分离,电喷雾正、负离子模式下多反应监测方式(MRM)采集数据,外标法定量。89种被测物,包括磺胺类、喹诺酮类、硝基咪唑类及其代谢物、苯并咪唑类及其代谢物、 β2-兴奋剂类、 β-阻滞剂类、利尿剂类共7类化合物,在一定浓度范围内线性关系良好(R2>0.99),在鸡肉、牛肉和猪肉中的加标回收率范围为52.3%~119.8%,相对标准偏差(RSD)均小于20%。利尿剂类的5个化合物,检出限(LODs)范围为0.86~4.51μg/kg,定量限(LOQs)范围为2.87~15.0μg/kg,其余84个化合物的LODs范围为0.02~0.44μg/kg, LOQs范围为0.07~1.48μg/kg;LODs均满足GB 31650-2019的要求。该方法适用于畜禽肉类中兽药残留的高通量快速筛查。

A pass-through solid phase extraction(SPE)purification was used to establish an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of 89 veterinary drug residues in livestock and poultry meat simultaneously.The meat was extracted with 10 mL acetonitrile containing 1%(V/V)acetic acid,purified by FaVEx-NM solid phase extraction column.The target analytes were separated on ACQUITY BEH C18(2.1 mm×100 mm,1.7μm)column,detected with electrospray ionization in the positive or negative ion mode using multiple reaction monitoring(MRM),quantified by external standard method.The results showed that 89 kinds of veterinary drugs,including sulfonamides,quinolones,nitroimidazoles and their metabolites,benzimidazoles and their metabolitesβ2-stimulants,β-blockers and diuretics,had good linear relationships,with the correlation coefficients(R2)higher than 0.99.The recoveries of the compounds were in the range of 52.3%-119.8%in the three matrices of chicken,pork and beef.The relative standard deviations(RSDs)were less than 20%.The limits of detections(LODs)of 5 compounds belonging to the class diuretics were 0.86-4.51μg/kg,and the limits of quantitation(LOQs)were 2.87-15.0μg/kg.While the LODs of the others 84 compounds were 0.02-0.44μg/kg,and the LOQs were 0.07-1.48μg/kg.All the LODs of the target analytes were lower than the requirements of GB 31650-2019.This method is suitable for high-throughput screening of the veterinary drug residues in livestock and poultry meat.