在线凝胶色谱-气相色谱-串联质谱法检测稻虾种养水环境中4种酰胺类除草剂残留量  

On-line gel chromatography-gas chromatography-tandem mass spectrometry for the determination of four amide herbicides residues in rice-crayfish integrated culture system

作　　者：卜媛媛[1] 胡珀[1] 尹戈 范军 金华[1] BU Yuanyuan;HU Po;YIN Ge;FAN Jun;JIN Hua(Huaian Institute for Food and Drug Control,Huaian,223300,China;Shimadzu China Co.Ltd,Shanghai,200233,China)

机构地区：[1]淮安市食品药品检验所,淮安223300 [2]岛津企业管理(中国)有限公司上海分公司,上海200233

出　　处：《环境化学》2022年第9期3115-3117,共3页Environmental Chemistry

基　　金：江苏省市场监督管理局科技计划项目(KJ207547)资助。

摘　　要：本文建立了4种酰胺类除草剂残留的GPC-GC-MS/MS检测方法.采集稻虾综合种养系统中的水样,采用乙酸乙酯进行萃取,萃取液浓缩富集后,通过GPC-GC-MS/MS联用仪在线净化和检测,加入外环氧七氯使用内标法定量分析.结果表明,甲草胺、乙草胺、丙草胺和丁草胺等4种化合物在20—300 ng·mL^(-1)浓度范围内线性关系良好,相关系数>0.99;4种酰胺类除草剂的回收率范围为79%—102%,精密度范围为2.5%—6.1%.该方法操作简单,快速准确,能有效去除基质干扰,提高分析灵敏度,满足4种酰胺类除草剂残留定量分析的要求.In the present study, a method was established for the residue determination of four amide herbicides by gel permeation chromatography-gas chromatography-tandem mass spectrometry(GPC-GC-MS/MS). Water samples from rice-crayfish integrated culture systems were extracted with ethyl acetate and then concentrated for online purification and detection by GPC-GC-MS/MS.Heptachloro epoxide(exo) was spiked as internal standard method for quantitative analysis. The results showed that the correlation coefficients of alachlor, acetochlor, pretilachlor and butachlor were over 0.99 in the concentration range of 20—300 ng·mL^(-1). The recoveries of the four amide herbicides were 79%—102%, with RSD in the range from 2.5% to 6.1%. The results indicated that this method was easy, fast and accurate and could effectively avoid the interference and improve analytical sensitivity, which could meet the residue determination requirements of four amide herbicides.

关 键 词：稻虾综合种养 水样 农药残留 GPC-GC-MS/MS 酰胺类除草剂 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]