QuEChERS-气相色谱-质谱法检测果品中41种有机磷类农药残留  

Determination of 41 organophosphorus pesticide residues in fruits by QuEChERS and gas chromatography-mass spectrometry

作　　者：段夏菲[1] 曾雅[1] 李映霞[1] 李沙沙[2] 凌东辉[1] DUAN Xia-fei;ZENG Ya;LI Ying-xia;LI Sha-sha;LING Dong-hui(Haizhu District Center for Disease Control and Prevention,Guangzhou,Guangdong 510288,China)

机构地区：[1]广州市海珠区疾病预防控制中心,广东广州510288 [2]暨南大学附属第一医院,广东广州510632

出　　处：《中国卫生检验杂志》2018年第15期1797-1802,共6页Chinese Journal of Health Laboratory Technology

基　　金：广州市医药卫生科技项目(20171A011337);广州市海珠区科技计划项目(海科工商信计2017-36)

摘　　要：目的建立果品中41种有机磷农药残留的QuEChERS-气相色谱-质谱联用分析方法。方法改进了样品前处理中的提取溶剂、分散固相萃取净化剂的种类和加入量。筛选了不同类型的硫酸镁、N-丙基乙二胺(PSA)、石墨化炭黑(GCB)及C_(18)吸附剂,根据对农药的吸附作用和净化效果,得到了最优配比的净化剂。果品中有机磷残留经过乙腈提取,QuEChERS净化,氮吹浓缩后乙腈定容,气相色谱-质谱法测定,选择离子模式定量。结果 41种组分的线性范围为0.010μg/ml^10.0μg/ml,相关系数均≥0.995 1,方法检出限为0.22μg/kg^10.9μg/kg,定量限为0.72μg/kg^36.2μg/kg。各组分的平均回收率为74.0%~102%,相对标准偏差均≤12%。结论该方法具有前处理简便快捷、净化效果佳、灵敏度高、成本低等特点,适用于果品中有机磷农药残留的快速确认及定量检测。Objective To establish an analytical method for the determination of 41 organophosphorus pesticide residues in fruits by QuEChERS and gas chromatography-mass spectrometry（GC-MS）. Methods The procedure of pretreatment was improved,such as types and volume of extraction solvent and dispersive solid-phase extraction cleanup agent. Different types of adsorbing materials were optimized,including Mg SO4,PSA,GCB and C_（18）. According to the adsorption and purification effect,the optimal ratio of purificant was obtained. The pesticides were extracted from fruit samples with acetonitrile,and the extract was cleaned-up by QuEChERS reagent. After dried-up under nitrogen flow,the residue was dissolved in acetonitrile,and then the target pesticides were detected by GC-MS. Selective ion monitoring mode was used for quantitative analysis.Results The linear range of the method was 0. 010 μg/ml-10. 0 μg/ml,with the correlative coefficents ≥0. 995 1. The limits of detection（LODs） of the method were within 0. 22 μg/kg-10. 9 μg/kg,and the limits of quantification（LOQs） were within 0. 72 μg/kg-36. 2 μg/kg. The recoveries of the method were from 74. 0% to 102%. The relative standard deviations（RSD） were no more than 12%. Conclusion The method was suitable for the identification and quantitative detection of organophosphorus pesticides in fruits due to its simplicity,good purification,high sensitivity and low cost.

关 键 词：QUECHERS 气相色谱-质谱法 有机磷 农药残留 果品 

分 类 号：O657.63[理学—分析化学]