两种叶菜中5种典型手性农药对映体的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法研究  

Chiral Resolution of Five Enantiomers of Chiral Pesticides in Two Leaf Vegetables by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Chiral Stationary Phase

作　　者：骆冲 黄聪灵 朱富伟 谢书越 黄健祥 叶倩 邓义才 万凯 LUO Chong;HUANG Cong-ling;ZHU Fu-wei;XIE Shu-yue;HUANG Jian-xiang;YE Qian;DENG Yi-cai;WAN Kai(Public Monitoring Center for Agro-product of Guangdong Academy of Agricultural Science,Guangzhou 510640, China;Key Laboratory of Testing and Evaluation for Agro-product Safety and Quality,Ministry of Agriculture, Guangzhou 510640,China;Agricultural Products Quality and Safety Risk Assessment Laboratory(Guangzhou),Ministry of Agriculture,Guangzhou 510640,China)

机构地区：[1]广东省农业科学院农产品公共监测中心,广东广州510640 [2]农业部农产品质量安全检测与评价重点实验室,广东广州510640 [3]农业部农产品质量安全风险评估实验室(广州),广东广州510640

出　　处：《分析测试学报》2018年第3期294-299,共6页Journal of Instrumental Analysis

基　　金：广东省农业科学院院长基金(201319);农产品质量安全风险评估项目(GJFP201700203)

摘　　要：基于手性固定相/超高效液相色谱-串联质谱技术建立了同时拆分2种叶菜类蔬菜(菜心、油麦菜)中5种典型手性农药(多效唑、腈菌唑、甲霜灵、三唑酮和唑菌酮)对映体的分析方法。样品用乙腈提取,N-丙基乙二胺(PSA)粉和石墨化碳黑(GCB)粉净化,经手性色谱柱CHIRALCEL OD-RH拆分后,超高效液相色谱-串联质谱(UPLC-MS/MS)检测。结果表明,5种手性农药在0.005~1.0 mg·L-1范围内均呈良好线性关系;在0.01、0.1、0.5 mg·kg-1加标水平下的平均回收率为68.8%~104%,相对标准偏差(n=6)为1.0%~13.7%。该方法准确、简单、可靠,可以满足叶菜类蔬菜中多种手性农药残留的检测要求,并为这5种手性农药对映体在蔬菜中的残留及消解规律研究提供技术支持。A method based on ultra performance liquid chromatography-tandem mass spectrometry with chiral stationary phase was developed for the simultaneous analysis of five chiral pesticide residues(paclobutrazo,myclobutanil,metalaxyl,triazolone and famoxadone)in leafy vegetables,including Chinese flowering cabbage and leaf lettuce.The sample was extracted with acetonitrile,then purified with primary secondary amine and graphitized carbon black.The upper clear liquid was filtered after centrifugation.After separated with a CHIRRALCEL OD-RH chiral column,the extract was detected using UPLC-MS/MS.Results indicated that the calibration curves of the five chiral pesticides showed good linear relationships in the concentration range of 0.005-1.0 mg·L-1.The recoveries at three spiked levels of 0.01,0.1,0.5 mg·kg-1 were in the range of 68.8%-104%with relative standard deviations of 1.0%-13.7%.This method is rapid,convenient and reliable,and could meet the requirements for residue analysis,and could provide a technical support for the investigation on five chiral pesticides residues in vegetables and their digestion regularity.

关 键 词：手性拆分 超高效液相色谱-串联质谱 对映体 蔬菜 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]