摘要
建立了花生仁、葵花籽、核桃仁和杏仁中185种农药多残留的气相色谱-串联质谱(GC-MS/MS)检测方法。样品经乙腈(含1%乙酸)均质提取,ENVI-18串联PSA固相萃取柱净化,在多重反应监测(MRM)模式下进行气相色谱-串联质谱法测定。185种农药在坚果样品中的检出限(S/N=5)为0.02～526.4μg/kg,定量下限(LOQ,S/N=10)均低于最大残留限量(MRLs),其中检出限在10μg/kg以下的农药数占被检农药总数的81%。185种农药在1～83倍LOQ浓度范围内的线性关系良好(r>0.99)。以4种坚果类样品为基质,在1、2、4倍LOQ加标水平下,185种农药的平均回收率在70%～110%范围的占86.0%;平均回收率在60%～120%范围的占90.5%;相对标准偏差(RSD)小于10%的占82.3%。该方法准确、灵敏、简便,可用于坚果中农药残留的日常检测。
A multi-residue analytical method was developed for the determination of 185 pesticides in nuts（peanuts,sunflower seeds,walnuts and amonds） by gas chromatography tandem mass spectrometry（GC-MS/MS）.The pesticide residues were extracted twice with homogenizer using acetonitrile containing 1% acetic acid.The extract was cleaned up with ENVI-18 tandem PSA solid-phase extractor and analyzed by GC-MS/MS under multiple reaction monitoring（MRM） mode.The limits of detection（LOD,S/N=5） were between 0.02 μg/kg and 526.4 μg/kg,in which the LODs of 81% of the tested pesticides were lower than 10 μg/kg.The limits of quantitation（LOQs,S/N=10） of 185 pesticides were less than the maximum residue limits（MRL）.All of the tested pesticides showed good linear relationship（r〉0.99） between 1 and 83 times of LOQs.The four samples were determined at three spiked levels of 1,2,4 times LOQ.The average recoveries of 86.0% pesticides were between 70% and 110%,and 90.5% pesticides were between 60% and 120%.The RSDs of 82.3% pesticides were less than 10%.This method was simple,sensitive and accurate,and could be used for the routine analysis of pesticide residues in nuts.
出处
《分析测试学报》
CAS
CSCD
北大核心
2011年第5期513-521,共9页
Journal of Instrumental Analysis
