液液萃取-衍生化/气相色谱-质谱法测定水中6种苯氧羧酸类除草剂  

Determination of Six Types of Phenoxy Acid Herbicides in Water by Gas Chromatography-Mass Spectrometry with Liquid-Liquid Extraction and Derivatization

作　　者：王媛媛 梁晶 王玲玲 赖晓姗 WANG Yuanyuan;LIANG Jing;WANG Lingling;LAI Xiaoshan(Henan Ecological Environment Monitoring and Safety Center,Zhengzhou 450000;Hami Ecological Environment Monitoring Station in Xinjiang Uygur Autonomous Region,Hami,Xinjiang 839000)

机构地区：[1]河南省生态环境监测和安全中心,郑州450000 [2]新疆维吾尔自治区哈密生态环境监测站,新疆哈密839000

出　　处：《中国农学通报》2025年第11期159-164,共6页Chinese Agricultural Science Bulletin

基　　金：环境标准制修订项目“水质氯代苯氧酸类除草剂的测定气相色谱-质谱法”(2014-48)。

摘　　要：本研究建立了一种可同时测定水中6种苯氧羧酸类除草剂的气相色谱-质谱法。水样经二氯甲烷液液萃取、脱水浓缩后,在碳酸钾催化下经五氟苄基溴衍生,衍生物进气相色谱-质谱分析。样品经Rtx-5ms毛细管色谱柱分离,采用选择离子扫描模式检测,内标法定量。结果表明:在最优实验条件下,6种苯氧羧酸类除草剂在质量浓度0.5~20.0μg/mL范围内线性关系良好,相关系数不低于0.999。方法检出限为0.2μg/L,精密度范围2.2%~6.9%。采用该方法对地下水、地表水、海水、生活污水和工业废水样品进行加标回收试验,基体加标回收率在83.0%~113%之间。该方法精密度较好、回收率稳定,为水中苯氧羧酸类除草剂的检测提供了一种有效的解决方案。A method for determination of 6 phenoxy acid herbicides in water by gas chromatography-mass spectrometry was established.After liquid-liquid extraction with dichloromethane,the extract was dehydrated and concentrated,then derivatized with PFBBR under the catalysis of potassium carbonate.The derivatives were analyzed by gas chromatography-mass spectrometry.Samples were separated by Rtx-5ms capillary chromatography column,detected by SIM mode,and quantified by internal standard.The results showed that under the optimal experimental conditions,6 phenoxy acid herbicides showed good linear relationships in the concentration range of 0.5 to 20.0μg/mL,the correlation coefficient was not less than 0.999.The detection limit was 0.2μg/L,and the precision range was 2.2%-6.9%.The spiked tests were conducted on groundwater,surface water,seawater,domestic sewage,and industrial wastewater samples,and the recovery range was 83.0%-113%.Results showed that this method had good precision and stable recovery,providing an effective solution for the detection of phenoxy acid herbicides in water.

关 键 词：液液萃取 衍生化 气相色谱-质谱法 苯氧羧酸类除草剂 分析方法 

分 类 号：X832[环境科学与工程—环境工程]