液相色谱–串联质谱法测定蔬菜中6种极性农药残留量  

Determination of Six Kinds of Polar Pesticide Residue in Vegetables by Liquid Chromatography–Tandem Mass Spectrometry

作　　者：郭平[1] 万建春[1] 祝建新[1] 占春瑞[1] 左海根[1] 

机构地区：[1]江西出入境检验检疫局检验检疫综合技术中心,南昌330038

出　　处：《化学分析计量》2016年第2期23-26,共4页Chemical Analysis And Meterage

基　　金：江西省科技厅科研项目(20141BBG70096)

摘　　要：建立了百草枯、敌草快、矮壮素、缩节胺、单甲脒、灭蝇胺6 种极性农药的液相色谱– 串联质谱测定方法.采用SCX 和C18 复合填料（质量比为1∶20）的Shiseido CAPCELL PAK CR 色谱柱分离,用超高压液相色谱– 串联质谱仪测定.利用响应面法优化得到样品的前处理条件,蔬菜样品用甲酸– 乙腈溶液均质提取,三氯甲烷液– 液萃取净化,在定量限的1,2,10 倍浓度水平,回收率在61.7%～116.8% 之间,测定结果的相对标准偏差不大于13.6%（n=6）.该法适用于蔬菜中百草枯、敌草快、矮壮素、缩节胺、单甲脒、灭蝇胺残留量的测定.A HPLC–MS/MS method was established for determination of polar pesticides residues of paraquat, diquat, chlormequat, mepiquat, semiamitraz, cyromazine. The chromatographic separation was achieved by ultra high pressure liquid chromatography–tandem mass spectrometry, using a CAPCELL PAK CR column with SCX and C18 mixing proportion of 1∶20. The sample pretreatment conditions was optimized by response surface method, vegetable samples were extracted with formic acid–acetonitrile solution, andpurified by liquid–liquid extraction with chloroform. The recoveries were 61.7%–116.8% with the relative standard deviation not more than 13.6%(n=6) in the level of 1, 2, 10 times concentration of the limit quantification (LOQ). The method is suitable for the determination of paraquat, diquat, chlormequat, mepiquat, semiamitraz, cyromazine residues in vegitables.

关 键 词：百草枯 敌草快 矮壮素 缩节胺 单甲脒 灭蝇胺 蔬菜 残留量 液相色谱–串联质谱法 

分 类 号：O657.63[理学—分析化学]