分散固相萃取结合HPLC法测定张杂谷中新烟碱类杀虫剂的残留  

Determination of Neonicotinoid Insecticides in Hybrid Millet Using Dispersive Solid-phase Extraction and HPLC

作　　者：卢海博 魏东 王素利 黄智鸿 高宝嘉[1] LU Hai-bo;WEI Dong;WANG Su-li;HUANG Zhi-hong;GAO Bao-jia(Forestry College,Hebei Agriculture University,Banding 071000,Hebei,China;Hebei North University,Hebei Key Laboratory of Quality ＆ Safety Analysis-Testing for Agro-Products and Food,Zhangjiakou 075000,Hebei,China)

机构地区：[1]河北农业大学林学院,河北保定071000 [2]河北北方学院河北省农产品食品质量安全分析检测重点实验室,河北张家口075000

出　　处：《农药》2018年第7期511-515,共5页Agrochemicals

基　　金：河北省教育厅项目(QN2016264)

摘　　要：[目的]研究适合谷子中8种新烟碱类杀虫剂的多残留快速检测方法。[方法]试验以乙腈为提取溶剂,PSA、GCB和C18吸附剂净化,0.3%甲酸水-乙腈梯度洗脱,基质匹配标准曲线外标法定量。[结果]在0.01~2.4 mg/L水平范围内,不同基质中的新烟碱类药剂线性相关系数均大于0.991,在0.05、0.20、0.8 mg/kg添加水平下,谷米、谷糠中新烟碱类杀虫剂的平均回收率为75%~105%,RSD为1.9%~14.4%。[结论]分散固相萃取-高效液相检测方法简便、快速、准确、灵敏、节省样品和有机溶剂,可满足谷米和谷糠中8种新烟碱类杀虫剂残留检测的需要。[Aims] In order to research the method for rapid determination of eight neonicotinoid insecticides in hybrid millet using dispersive solid-phase extraction and high performance liquid chromatography.[Methods] The sample was extracted with acetonitrile and cleaned up with PSA,GCB and C18,and then separated using an gradient elution program of 0.3% aqueous formic acid and acetonitrile.Matrix-matched calibrations were used to quantify the residue concentrations.[Results] In the concentration range of 0.01-2.4 mg/L,the matrix-matched calibration curves showed good linearity with correlation coefficients of ≥0.991.At the addition levels of 0.05,0.20 and 0.8 mg/kg,mean recoveries of neonicotinoid insecticides in different matrices were 75-105% with relative standard deviations（RSD） of1.9-14.4%.[Conclusions] The method is simple,rapid,sensitive and accurate,which can meet the detection requirements of neonicotinoid insecticides in grain and bran of hybrid millet.

关 键 词：新烟碱类杀虫剂 多残留分析 张杂谷 高效液相色谱 

分 类 号：TQ450.2[化学工程—农药化工]