超高效液相色谱-三重四极杆/线性离子阱串联质谱法同时快速筛查和检测食物中毒样品中的12种抗凝血杀鼠剂

目的 建立食物中毒样品中12 种抗凝血杀鼠剂的超高效液相色谱-三重四极杆/线性离子阱串联质谱(QTrap LC-MS /MS)的检测方法。方法 样品经快速分散固相萃取法(QuEChERS)提取和净化,ACQUITY UPLC BEH-C18柱(1.7μm,2.1mm×50mm)分离,5mmol/L乙酸铵和乙腈为流动相梯度洗脱,按照多级反应监测(MRM)→信息相关采集(IDA)→增强子离子扫描(EPI)→谱库检索的模式进行分析。结果 12种抗凝血杀鼠剂线性相关系数均大于0.99,平均回收率为78.2%～108.2%,相对标准偏差为1.8%～12.3%,方法的检出限为0.006～0.03μg/kg,定量限为0.02～0.10μg/kg。结论 该法简便快速,灵敏度高、重现性较好,适用于食物中毒样品中12种抗凝血杀鼠剂同时快速测定。

Rapid simultaneous screening and detection of 12 anticoagulant rodenticides in food poisoning samples by ultra-performance liquid chromatography-triple quadrupole/linear ion trap tandem mass spectrometry

Objective To establish a rapid analytical method for the simultaneous screening and detection of 12 anticoagulant rodenticides in food poisoning samples using an ultra-performance liquid chromatography-triple quadrupole/linear ion trap tandem mass spectrometry(UPLC-QTrap-MS/MS). Methods Food poisoning samples were extracted and purified with modified QuEChERS method.The 12 anticoagulant rodenticides and the internal standard(warfarin-D5)were separated using an ACQUITY UPLC BEH-C18 column(1.7μm,2.1 mm×50 mm)and gradient eluent was conducted with a mobile phase consisting of 5 mmol/L ammonium acetate formate buffer and acetonitrile.A multiple reaction monitoring(MRM)scan and an enhanced product ion(EPI)scan were performed in an information dependent acquisition(IDA)experiment. Results The calibration curves were linear(r>0.99)for all the compounds.The mean recoveries for the 12 analytes at three spiked levels were in the range of 78.2%~108.2% with RSDs of 1.8%~12.3%.The limits of detection(LODs)for the 12 rodenticides ranged from 0.006 to 0.03μg/kg.The limits of quantification(LOQs)for the 12 rodenticides were between 0.02 and 0.10 μg/kg. Conclusion The developed method is simple,rapid,sensitive and can be used for screening 12 kinds of anticoagulant rodenticide residues in food poisoning samples.