赵海涛 王磊 王帅 刘会会 戚继存 王雅静 张亮 郑百芹 刘洋

摘要 [目的]建立液相色谱-串联质谱法（LC/MS）测定果蔬（番茄、黄瓜、韭菜、马铃薯、西瓜、苹果和橙子）中涕灭威及其代谢物的分析方法。[方法]样品经组织捣碎，乙腈提取，经氨基柱和二氯甲烷+甲醇（95∶5）净化洗脱处理，2 mL甲醇定容，采用Phenomenex H18色谱柱分离。[结果]涕灭威及其代谢物在0.01和0.02 mg/kg 2个添加水平下回收率均为84.667%～104.333%，RSD均为0～5.37%，试验方法检出限为0.01 mg/kg，相关系数均大于0.999 3。[结论]该方法操作简便、快捷，安全性高，只通过一种检测方法便可同时测定果蔬中涕灭威及其代谢物的残留量，准确度和灵敏度高，定量下限低于或等于国家农药残留限量标准。

关键词 液相色谱-串联质谱;涕灭威及其代谢物;果蔬

中图分类号 TS.207.5+3文献标识码 A文章编号 0517-6611（2021）02-0196-05

doi：10.3969/j.issn.0517-6611.2021.02.053

開放科学（资源服务）标识码（OSID）：

Determination of Aldicarb and Its Metabolites in Fruits and Vegetables by Liquid ChromatographyTandem Mass Spectrometry

ZHAO Haitao1，2，3， WANG Lei1，2，3，WANG Shuai1，2，3 et al

（1.Tangshan Food and Drug Comprehensive Testing Center， Tangshan，Hebei 063000;2. Hebei Agricultural Products Quality and Safety Testing Innovation Center， Tangshan，Hebei 063000;3. Tangshan Institute of Industrial Technology for Functional Agricultural Products， Tangshan，Hebei 063000）

Abstract [Objective]To establish a method for the aldicarb and its metabolites detection of 7 vegetables and fruits （tomato， cucumber， leek， potato， watermelon， apple， and orange） by liquid chromatographytandem mass spectrometry. [Method]The samples were mashed， and then extracted with acetonitrile， the extraction was purified by the amino column and dichloromethane + methanol （95∶5）. After constant volume with 2 mL methanol， the target analytes were separated on a Phenomenex H18 column. [Result]The recovery rates of aldicarb and its metabolites were 84.667%-104.333%， RSD were 0-5.37% at two added levels of 0.01 and 0.02 mg/kg. The detection limit of the experimental method was 0.01 mg/kg. The correlation coefficients were all greater than 0.999 3. [Conclusion]The method is simple， fast and safe. It can simultaneously determine aldicarb and its metabolites in vegetables and fruits with only one detection method. The accuracy and sensitivity are high， and the lower limit of quantification is less than or equal to national pesticide residue limit standards.

Key words Liquid chromatographytandem mass spectrometry;Aldicarb and its metabolites;Fruits and vegetables

涕灭威（C7H14N2O2S）具有触杀、胃毒和内吸作用，能被植物根系吸收，传导到植物地上部各组织器官，速效性好，持效期长。然而农药检测已经不仅仅局限于农药本体，其代谢物产生的毒性作用逐渐成为热点[1-8]。通常可通过超高效液相色谱串联质谱仪检测蔬菜中涕灭威及其代谢物[9]，也可通过固相萃取液相色谱串联质谱法测定生姜中涕灭威及其代谢物[10]。

《蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定》中涉及到涕灭威及其代谢物的测定方法是将试样中氨基甲酸酯类农药及其代谢物用乙腈提取，经过滤、浓缩后，采用固相萃取技术分离、净化、浓缩后，使用带荧光检测器和柱后衍生系统的高效液相色谱进行检测，保留时间定性，外标法定量[11]。……