超高效液相色谱法测定果蔬中4种双酰肼类农药残留  

UHPLC determination of four diacylhydrazide pesticides residues in fruits and vegetables

作　　者：李常雄 邹海民[1] 胡晓科[1] 杨晓松[1] 文君[1] LI Changxiong;ZOU Haimin;HU Xiaoke;YANG Xiaosong;WEN Jun(Chengdu Center for Disease Control and Prevention,Chengdu 610041,China)

机构地区：[1]成都市疾病预防控制中心,四川成都610041

出　　处：《中国测试》2020年第3期59-63,共5页China Measurement & Test

基　　金：成都市疾病预防控制中心2018年普及应用项目(20180208)。

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,1.8μm)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0.05~10μg/mL范围内具有良好的线性关系,相关系数R在0.9986~0.9998之间,方法定量为12.94~17.32μg/kg,方法检出限为3.882~5.196μg/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。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 0.05-10μg/mL,the correlation coefficients were 0.9986 and 0.9998.The limit of quantification for the method was 12.94-17.32μg/kg.The limit of detection was 3.882-5.196μg/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.

关 键 词：超高效液相色谱法 双酰肼类 果蔬 农药残留 

分 类 号：R155.5[医药卫生—营养与食品卫生学]