摘要
建立了一种基于QuEChERS(Quick Easy Cheap Effective Rugged and Safe)前处理技术和超高效液相色谱-串联质谱(UHPLC-MS/MS)以及气相色谱(GC)快速检测玉米中14种草地贪夜蛾应急防治推荐用药残留的方法。通过对色谱质谱条件、提取溶剂、缓冲体系、净化剂、提取温度等进行优化,确定了以甲醇和0.1%甲酸+5 mmol/L乙酸铵作为流动相,0.1%(体积分数)氨水乙腈作为提取溶剂,4 g MgSO_(4)+1.5 g NaCl作为缓冲体系,-20℃冷冻离心等条件。14种杀虫剂线性关系良好,相关系数(r^(2))均不小于0.9917,检出限(S/N=3)为0.08~4.50 g/kg,定量限(N=10)为0.30~13.5μg/kg。3个加标水平下(60、100、400μg/kg)的平均回收率为75.00%~125.68%,相对标准偏差(RSD)为0.00%~14.64%。茚虫威、虫酰肼、虱螨脲等8种待测物表现为中等或强基质效应。该方法简便易操作,具有较好的灵敏度和准确度,适用于玉米中14种草地贪夜蛾应急防治推荐用药残留的快速检测。
A method based on QuEChERS(Quick Easy Cheap Effective Rugged and Safe)pretreatment technique and ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)and gas chromatography(GC)was developed for the simultaneous determination of 14 recommended drugs'residues for emergency control of Spodoptera frugiperda in corn.After optimizing the chromatographic and Mass spectrum conditions,extraction solvents,buffer systems,purification agents and extraction temperatures,methanol and 0.1%formic acid+5 mmol/L ammonium acetate,0.1%ammonium hydroxide acetonitrile,4 g MgSO_(4)+1.5 g NaCl,centrifuge at-20℃were considered as optimal conditions.There were good linear correlations of 14 Insecticides with their coefficients(r^(2))no less than 0.9917,the limit of detections(S/N=3)was 0.08~4.50μg/kg,the limit of quantitations(S/N=10)was 0.30~13.5μg/kg.Average recoveries of 14 Insecticides at three spiked levels(60,100,400μg/kg)ranged from 75.00%~125.68%with their relative standard deviations(RSD)of 0.00%~14.64%.Indoxacarb,Tebufenozide,Tebufenozide and other 5 insecticides showed moderate or strong matrix effects.This method is easy to operate and has good sensitivity and accuracy,which is suitable for rapid determination of 14 recommended drugs'residues for emergency control of Spodoptera frugiperda in corn.
作者
李莹
仲伶俐
李曦
刘炜
陈敏
LI Ying;ZHONG Ling-Li;LI Xi;LIU Wei;CHEN Min(Institute of Quality and Testing Technology for Agro-products,Sichuan Academy of Agricultural SciencesChengdu 610066,China)
出处
《化学研究与应用》
北大核心
2025年第8期2445-2451,共7页
Chemical Research and Application
作者简介
通讯作者:李莹(1990-),女,助理研究员,主要从事农产品质量安全及风险评估。E-mail:Liying0098@126.com。
