QuEChERS-GC-MS同时测定梨中21种有机磷农药残留  

Simultaneous Determination of 21 Organophosphorus Pesticide Residues in Pears by QuEChERS-GC-MS

作　　者：张艳 李慧冬[1,2,3] 丁蕊艳 郭长英[1,2,3] 毛江胜 陈子雷[1,2,3] ZHANG Yan;LI Huidong;DING Ruiyan;GUO Changying;MAO Jiangsheng;CHEN Zilei(Institute of Agricultural Quality Standards and Testing Technology,Shandong Academy of Agricultural Sciences,Jinan 250100;Agricultural Product Quality and Safety Risk Assessment Laboratory of Ministry of Agriculture and Rural Agriculture,Jinan 250100;Shandong Key Laboratory of Food Quality and Safety Testing Technology,Jinan 250100)

机构地区：[1]山东省农业科学院农业质量标准与检测技术研究所,济南250100 [2]农业农村部农产品质量安全风险评估实验室,济南250100 [3]山东省食品质量与安全检测技术重点实验室,济南250100

出　　处：《食品工业》2019年第11期323-327,共5页The Food Industry

基　　金：国家现代农业产业技术体系(CARS-28-23);山东省农业科学院农业科技创新工程(CXGC2017A03)

摘　　要：利用QuEChERS法结合气相色谱-串联质谱(GC-MS)建立了同时检测梨中21种有机磷农药残留的分析方法。样品经乙腈提取,氯化钠盐析后,采用N-丙基乙二胺(Primary secondary amine, PSA)净化,以气相色谱-串联质谱和选择离子监测(SIM)模式检测,外标法定量。结果表明:21种有机磷农药在0.01~1μg/mL范围内具有良好的线性关系,相关系数均大于0.99;方法检出限在0.2~2.6μg/kg之间;在0.01, 0.1和0.5 mg/kg三个添加水平下,回收率为85.4%~100.4%,相对标准偏差(RSD, n=6)在1.9%~6.8%之间。该方法操作简便快速,回收率、精密度和重现性均较好,可以满足梨中21种有机磷农药的定性与定量分析要求。A method for the simultaneous determination of 21 organophosphorus pesticide residues in pears was established by QuEChERS combined with gas chromatography-mass spectrometry. The sample was extracted with acetonitrile, salting out by sodium chloride, purified by N-propyl ethylenediamine(PSA), and then detected by gas chromatography-tandem mass spectrometry with the method of selective ion monitoring(SIM). The external standard method was used for quantitative analysis. The results showed that the calibration curves of 21 organophosphorus pesticides had a good linear relationship in the range of 0.01-1 μg/m L with correlation coefficients more than 0.99. The limits of detection(LOD) were 0.2-2.6 μg/kg. At the spiked levels of 0.01, 0.1 and 0.5 mg/kg, the recoveries of all compounds were between 85.4% and 100.4%, and the relative standard deviations(RSD, n=6) ranged from 1.9% to 6.8%. The method was simple and fast to operate, and it had good recovery and precision, which was suitable for qualitative and quantitative detection of 21 organophosphorus pesticides in pear.

关 键 词：QUECHERS 气相色谱-串联质谱 梨 21种有机磷 

分 类 号：R28[医药卫生—中药学]