康俊杰 王雪松 董李学 崔亚楠 周鑫 郑百芹 刘洋 项爱丽

摘要 [目的]利用超高效液相色谱-四极杆飞行时间质谱技术建立虾中38种农药残留的快速筛查方法。[方法]采用50%乙腈水溶液作溶剂、QuEChERS提取盐包和Oasis PRiME HLB固相萃取载体作吸附剂，实现了虾肉样品中38种目标物的同时提取和有效净化。目标药物经ACQUITY UPLC HSS T3（1.8 μm，21 mm×50 mm）色谱柱分离，以10  mmol/L乙酸铵-甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱，使用电喷雾离子源，在正离子模式下进行全扫描，可在10  min内实现38种农药的良好分离。[结果]虾中38种农药的定量限（LOQ）为0.5～1.5 μg/kg;3个加标水平的平均回收率为71.4%～97.9%，相对标准偏差（RSD）为4.1%～7.6%。[结论]该方法简便快速、灵敏度较高，可用于虾中38种农药的快速筛查。

关键词 超高效液相色谱-四极杆飞行时间质谱;农药残留;虾;快速筛查

中图分类号 TS 254.7  文献标识码 A

文章編号 0517-6611（2021）16-0193-03

doi：10.3969/j.issn.0517-6611.2021.16.052   开放科学（资源服务）标识码（OSID）：

Rapid Screening of 38 Pesticide Residues in Shrimp by Ultra Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry

KANG Jun-jie1，2，WANG Xue-song1，2，DONG Li-xue1，2 et al （1.Tangshan City Food and Drug Comprehensive Inspection and Testing Center，Tangshan，Hebei 063000;2.Hebei Agricultural Product Quality and Safety Testing Technology Innovation Center， Tangshan，Hebei 063000）

Abstract [Objective] An analytical method was established for the simultaneous determination of 38 pesticide residues in shrimp by ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry.[Method] Using 50% acetonitrile aqueous solution as the solvent， QuEChERS extraction salt packet and Oasis PRiME HLB solid-phase extraction carrier as the adsorbent， the simultaneous extraction and effective purification of 38 target substances in shrimp samples were achieved.The target drug was separated by ACQUITY UPLC HSS T3 （1.8 μm， 21 mm×50 mm） chromatographic column， and 10  mmol/L ammonium acetate-methanol and 0.1% formic acid aqueous solution were used as mobile phases for gradient elution.The electrospray ion source was used for a full scan in positive ion mode could achieve good separation of 38 pesticides within 10  minutes.[Result] The limit of quantification （LOQ） of 38 pesticides in shrimp was 0.5-1.5 μg/kg; the average recovery of the three spiked levels was 71.4%-97.9%， and the relative standard deviation （RSD） was 4.1%-7.6%.[Conclusion] The method is simple， rapid and highly sensitive， and can be used for rapid screening of 38 pesticides in shrimp.

Key words Ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry;Pesticides residues;Shrimp;Rapid screening

随着人们生活水平的提高，虾已经成为日常生活的营养品之一，其安全性问题受到越来越多的关注。虾的安全问题的主要表现是水体环境的污染，有机磷类农药由于杀虫效果好、价格低、范围广等特点，使其成为农业生产中主要的农药品种。农药在水生生物体中富集，对人类的健康造成很大的隐患，亟需对其进行监控[1-3]。人类长期进食含农药残留的虾肉，会对身体造成不良影响，如急性中毒、慢性中毒、干扰内分泌系统、毒害全身多脏器等危害，对身体健康的危害不容忽视[4-6]。农药一直以来是蔬菜水果中检测的重点参数，但近几年根据报道虾肉中农药有检出的现象。……