气相色谱联合三重四级杆串联质谱法检测地表水中苯达松、乙草胺、异丙隆等7种常用除草剂残留  

Determination of 7 common herbicides in surface water by gas chromatography combined with triple quadrupole tandem mass spectrometry

作　　者：张文锦 李志华 陈晓琴 盖建功 后小龙 李学科 ZHANG Wenjin;LI Zhihua;CHEN Xiaoqin;GAI Jiangong;HOU Xiaolong;LI Xueke(Gansu Dingxi Ecological Environment Monitoring Center,Dingxi 743000,China)

机构地区：[1]甘肃省定西生态环境监测中心,甘肃定西743000

出　　处：《中国测试》2022年第10期36-40,共5页China Measurement & Test

基　　金：甘肃省科技计划资助(自然科学基金)项目(21JR7RA692)。

摘　　要：建立一种气相色谱联合三重四级杆串联质谱法检测地表水中苯达松、乙草胺、异丙隆等7种常用除草剂残留的分析方法。将地表水样品进行预处理后,以全自动固相萃取法选择HLB固相萃取柱对样品进行提取。然后用10 mL的正己烷将吸附在萃取柱上的农药洗脱下来,于45℃水浴中氮气吹至近干,用正己烷定容至1 mL,进样气相色谱串联质谱(GC-MS/MS)分析系统,外标法定量。结果表明,苯达松、乙草胺、异丙隆、丁草胺、嗪草酮、扑草净和禾草灵在质量浓度0.02~5.0μg/mL范围内线性关系良好,相关系数均大于0.995。检出限如下:苯达松:0.062μg/L,乙草胺:0.063μg/L,异丙隆:0.058μg/L,丁草胺:0.050μg/L,嗪草酮:0.046μg/L,扑草净:0.087μg/L和禾草灵:0.071μg/L。平均加标回收率均在90.2%~102.3%之间,精密度6次测定结果的相对标准偏差在1.58%~4.18%之间。该方法具有简单、快速,自动化程度高,定性定量结果准确等优点,为水样中农药残留的监测提供一种新的分析方法。An analytical method was developed for the determination of 7 common herbicides(such as bendasone, acetochlor and isoproderone.etc) in surface water by gas chromatography combined with triple quadrupole tandem mass spectrometry. After the surface water samples were pre-treated, the HLB solid phase extraction column was used to extract the samples according to automatic solid phase extraction method.10 mL n-hexane was used to elution the pesticides adsorbed on the extraction column, and nitrogen was blown to near dry in a 45℃ water bath. N-hexane was used to constant volume to 1 mL, and the samples were injected into the gas chromatography-tandem mass spectrometry(GC-MS/MS) analysis system, and quantified by external standard method. Results show that, bentazone, acetochlor, isoproturon, butachlor, metribuzin,prometryn and diclofop-methyl showed good linear relationships in the concentration ranges of 0.02-5.0 μg/L,with correlation coefficients(r) all greater than 0.995. Detection limits were as follows: bentazone: 0.062 μg/L,acetochlor: 0.063 μg/L,isoproturon: 0.058 μg/L,butachlor: 0.050 μg/L,metribuzin: 0.046 μg/L, prometryn:0.087 μg/L and diclofop-methyl: 0.071 μg/L, respectively. Average recoveries were in the range 90.2%-102.3%;Relative standard deviation(RSD) of precision(n=6) were 1.58%-4.18 %. The method has the advantages of simple, rapid, high degree of automation, accurate qualitative and quantitative results, providing a new analytical method for the monitoring of pesticide residues in water samples.

关 键 词：固相萃取 GC-MS/MS 地表水 除草剂 苯达松 

分 类 号：TB9[一般工业技术—计量学]