摘要
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。
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.
引文
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