作者：李常雄, 邹海民, 胡晓科, 杨晓松, 文君

作者单位：成都市疾病预防控制中心，四川 成都 610041

关键词：超高效液相色谱法;双酰肼类;果蔬;农药残留

摘要：

建立同时测定果蔬中抑食肼、甲氧虫酰肼、环虫酰肼、虫酰肼4种双酰肼类农药残留的超高效液相色谱法。方法用含1%氨水的甲醇溶液对样品进行提取，提取液经过乙二胺-N-丙基硅烷（PSA）和十八烷基硅烷键合相（C18）基质分散净化后，采用Agilent RRHD SB-C18柱(2.1 mm×50 mm，1.8 μm)分离，Agilent 1290 Infinity超高效液相色谱仪DAD检测器进行检测。可在4 min内完成对4种双酰肼类农药的检测，且在0.05~10 μg/mL范围内具有良好的线性关系，相关系数R在0.998 6~0.999 8之间，方法定量为12.94~17.32 μg/kg，方法检出限为3.882~5.196 μg/kg。在0.05~2.5 mg/kg范围内，平均加标回收率为72.4%~100.4%，相对标准偏差为2.1%~6.1%。该方法灵敏度高、选择性好、操作简单，适用于果蔬中4种双酰肼类农药残留的同时快速分析。

UHPLC determination of four diacylhydrazide pesticides residues in fruits and vegetables
LI Changxiong, ZOU Haimin, HU Xiaoke, YANG Xiaosong, WEN Jun
Chengdu Center for Disease Control and Prevention, Chengdu 610041, China
Abstract: To establish a method for the simultaneous determination of four dihydrazides pesticide residues in fruits and vegetables by ultra high performance liquid chromatography (UHPLC). Samples were extracted by solution of 1% ammonia water in methanol, and purified by dispersion solid phase extration using PSA and C18 as solid phase, then separated by Agilent RRHD SB-C18(2.1 mm×50 mm, 1.8μm) and detected by DAD detector of Agilent 1290 Infinity ultra highperformance liquid chromatography. The detection of four dihydrazides pesticides can be completed within 4 minutes, and agood linearity was obtained within the concentration range of 0.05-10 μg/mL, the correlation coefficients were 0.998 6 and 0.999 8.The limit of quantification for the method was 12.94-17.32 μg/kg. The limit of detection was 3.882-5.196 μg/kg. Average recoveries for six new insecticides in four samples at spiked levels of 0.05-2.5 mg/kg were between 74.2% and 100.4%, with a relative standard deviations between 2.1% and 6.1%. The method is of good selection, high sensitivity, and it is simple and fast, it is suitable for simultaneous and rapid analysis of four diacylhydrazides pesticide residues in fruits and vegetables.
Keywords: UHPLC;diacylhydrazides;fruits and vegetables;pesticides residues
2020, 46(3):59-63  收稿日期: 2019-09-02;收到修改稿日期: 2019-10-27
基金项目: 成都市疾病预防控制中心2018年普及应用项目（20180208）
作者简介: 李常雄(1985-),男,重庆市人,硕士,主要从事理化检验分析工作
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