固相萃取-气相色谱-串联质谱法测定生活饮用水中21种除草剂  

Solid phase extraction-gas chromatography-tandem mass spectrometry method for determining 21 types of herbicides in drinking water

作　　者：丁宇[1] 周睿[1] 张博[1] 宋黎黎[1] DING Yu;ZHOU Rui;ZHANG Bo;SONG Li-li(Shanghai Huangpu District Center for Disease Prevention and Control,Shanghai 200023,China)

机构地区：[1]上海市黄浦区疾病预防控制中心,上海200023

出　　处：《现代预防医学》2025年第1期149-154,共6页Modern Preventive Medicine

基　　金：上海市黄浦区医学优势专科(2023PYZK04);上海市黄浦区科学委员会课题(HLM202224)。

摘　　要：目的 基于固相萃取前处理技术,建立生活饮用水中21种除草剂的气相色谱-串联质谱检测方法。方法 抽取500 ml水样,经C18固相萃取小柱萃取、5 ml乙酸乙酯-二氯甲烷(1∶1)混合液洗脱。收集洗脱液,真空离心浓缩至近干,用1 ml乙酸乙酯定容后,进样气相色谱质谱仪检测、多反应监测模式(MRM)定量。结果 在5.0~200.0μg/L范围内,各除草剂呈现良好的线性,相关系数在0.995 4~0.999 8之间,检出限(LOD)在0.11~1.21μg/L之间,定量限(LOQ)在0.33~3.64μg/L之间,精密度(RSD)在1.6%~6.3%范围内,回收率在74.3%~112.7%之间。结论 该方法线性范围宽、准确、可靠,适合于水中多种除草剂的检测。Objective To establish a gas chromatography-tandem mass spectrometry(GC-MS/MS)method for detecting 21 types of herbicides in drinking water based on solid phase extraction(SPE)pre-treatment technology.Methods A 500 ml water sample was extracted using a C18 solid phase extraction column,followed by elution with a 5 ml mixture of ethyl acetate and dichloromethane(1:1).The eluent was collected and concentrated near dryness using vacuum centrifugation,and then reconstituted with 1 ml of ethyl acetate for analysis by gas chromatography-mass spectrometry in multiple reaction monitoring(MRM)mode.Results Within the concentration range of 5.0μg/L to 200.0μg/L,the herbicides exhibited good linearity,with correlation coefficients ranging from 0.9954 to 0.9998.The limits of detection(LOD)ranged from 0.11μg/L to 1.21μg/L,while the limits of quantification(LOQ)ranged from 0.33μg/L to 3.64μg/L.Precision(RSD)was found to be between 1.6%and 6.3%,and the recovery rates ranged from 74.3%to 112.7%.Conclusion This method demonstrates a wide linear range,accuracy,and reliability,making it suitable for the detection of multiple herbicides in water.

关 键 词：固相萃取 气相色谱-串联质谱法 生活饮用水 除草剂 

分 类 号：O657.71[理学—分析化学]