QuEChERS/超高效液相色谱-串联质谱法测定禽蛋中90种禁用药物残留

Determination of 90 Prohibited Drugs Residues in Poultry Eggs by QuEChERS/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了禽蛋中90种禁用药物的QuEChERS/超高效液相色谱-三重四极杆串联质谱(UPLC-QqQ-MS)检测方法。样品以0.2%甲酸-乙腈水溶液(3∶1,体积比)超声提取,加入25 mg Na2EDTA螯合基质中的金属离子,用EMR-lipid填料净化后采用ACQUITY UPLC HSS T3柱(2.1 mm×100 mm,1.8µm)分离,正离子模式以0.1%甲酸水-甲醇为流动相,负离子模式以水-乙腈为流动相进行梯度分离,以多反应监测(MRM)方式扫描,标准曲线内标法定量。结果表明:目标物在各自质量浓度范围内呈良好的线性关系,相关系数(r^(2))不小于0.99,检出限(LOD)和定量下限分别为0.05~1µg/kg和0.1~3µg/kg,鸡蛋的回收率为60.8%~111%,相对标准偏差为1.6%~18%,106件实际样品共检出7种药物。该方法操作简捷、准确性高,可实现禽蛋中违禁药物残留的高通量快速检测。

To establish a method for the determination of prohibited drugs in poultry eggs by ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry(UPLC-QqQ-MS),samples were extracted and purified using QuEChERS method.The drugs were extracted with 0.2%formic acid-acetonitrile solution(3∶1,by volume),and 25 mg of Na2EDTA was added to chelate the metal ions in the matrix,and the separation was performed on an ACQUITY UPLC HSS T3 col-umn(2.1 mm×100 mm,1.8µm)after cleanup with EMR-lipid packing.The separation was car-ried out by gradient separation with 0.1%formic acid aqueous solution-methanol as mobile phase in positive ion mode and water-acetonitrile as mobile phase in negative ion mode,which was scanned by multi-reaction monitoring(MRM)mode and quantified by the standard curve internal standard method.The results showed that target compounds obtained good linear relationship in their respec-tive mass concentration ranges,with correlation coefficients(r^(2))not less than 0.99.The limits of de-tection(LODs)and the limits of quantitations(LOQs)for the 90 compounds were determined to be 0.05-1µg/kg and 0.1-3µg/kg,respectively.Average recoveries of these compounds in eggs were 60.8%-111%,and the relative standard deviations were 1.6%-18%,which met the requirements of multiple veterinary drug residues.A total of 7 prohibited drugs were detected in 106 samples.This method can be used for the high-throughput rapid detection of prohibited drug residues in poultry eggs with a simple,accurate and low-cost procedure.