QuEChERS EMR-Lipid结合超高效液相色谱-串联质谱法测定动物源食品中16种喹诺酮类药物残留

Determination of 16 quinolones residues in animal food by UPLC-MS/MS with QuEChERSEMR-Lipid

目的:建立一种QuEChERS EMR-Lipid结合超高效液相色谱-串联质谱(UPLC-MS/MS)法同时测定动物源性食品中16种喹诺酮类药物残留的分析方法。方法:前处理利用酸化乙腈实现快速高效的蛋白沉淀萃取,使用增强型脂质去除净化管(QuEChERS EMR-Lipid)和EMR-Lipid反萃管进一步净化,氮吹,用0.1%甲酸水溶液复溶,经C18色谱柱分离后,采用0.2%甲酸水和乙腈作为流动相进行梯度洗脱,在ESI正离子模式下,采用多反应监测(MRM)方式进行扫描。结果:各组分在5~200ng/mL范围内线性关系良好,相关系数均大于0.996。检出限为2.0μg/kg,定量限为5.0μg/kg,在3个添加水平(n=6)的回收率为79.1%~99.3%,相对标准偏差在1.6%~8.7%之间。结论:该方法快速、灵敏、准确,适用于动物源性食品中喹诺酮检测。

Acidified acetonitrile was used to achieve rapid and efficient precipitation and extraction.The enhanced lipid removal purification tube(QuEChERS EMR lipid)and EMR lipid stripping tube were used for further purification,nitrogen blowing to dryness.The mixture was redissolved in 0.1%formic acid water solution.After separation on C18 column,0.2% formic acid water and acetonitrile were used as mobile phase for gradient elution.Mass spectrometry(MS)was used as an ion source(ESI+)and for multi-response monitoring(MRM).The test results showed that the calibration curves of all the components were linear in the concentration ranges of 5—200ng/mL,and the correlation coefficients were more than 0.996;the detection limit was 2.0μg/kg,and the limit of quantification was 5.0μg/kg;the recoveries were 79.1%—99.3 %at three levels(n=6);the relative standard deviation was 1.6%—8.7%.The method is rapid,sensitive and accurate,which is suitable for the determination of quinolones in animal food.