生活饮用水中环氧氯丙烷和亚硝基二甲胺的气相色谱-三重四级杆串联质谱检测法  

Determination of epichlorohydrin and dimethylnitrosamine in drinking water by gas chromatography-triple-quadrupole mass spectrometry

作　　者：倪海平 刘祥萍[1] 陈春静 董妍 袁婷婷 陈明聪 李冬宁 朱醇[4] NI Hai-ping;LIU Xiang-ping;CHEN Chun-jing;DONG Yan;YUAN Ting-ting;CHEN Ming-cong;LI Dong-ning;ZHU Chun(Physical and Chemical Laboratory,Nanjing Provincial Center for Disease Prevention and Control,Nanjing,Jiangsu 210003,China;不详)

机构地区：[1]南京市疾病预防控制中心理化检验科,江苏南京210003 [2]南京市疾病预防控制中心环境卫生科 [3]南京市鼓楼区疾病预防控制中心检验科 [4]江苏省疾病预防控制中心理化所,南京210009

出　　处：《环境与健康杂志》2024年第11期1009-1012,共4页Journal of Environment and Health

基　　金：2023年度南京市卫生科技发展专项资金项目(YKK23194)。

摘　　要：目的建立生活饮用水中环氧氯丙烷(ECH)和亚硝基二甲胺(NDMA)的气相色谱-三重四级杆串联质谱(GC-MS/MS)测定方法。方法取500 ml水样经椰壳固相萃取柱萃取,10 ml二氯甲烷洗脱,氮吹浓缩至1 ml,VF-WAXms色谱柱分离,用GC-MS/MS在多反应模式(MRM)下测定,外标法定量。结果在4~200μg/L的范围内,所得ECH的回归方程为y=269.4512x-493.946,r=0.9995,线性关系良好;在2~100μg/L的范围内,所得NDMA的回归方程为y=293.6303x+234.1608,r=0.9997,线性关系良好。该方法对ECH、NDMA的方法检出限分别为0.0005、0.0002μg/L,定量下限分别为0.015、0.006μg/L。该方法对ECH的回收率在79%~110%之间,RSD在4.9%~9.5%之间;NDMA回收率在83%~118%之间,RSD在7.6%~11.3%之间。结论该方法具有检出限低、精密度和准确度高,适用于大批量水样中ECH和NDMA的同时测定。Objective To establish a method for the determination of epichlorohydrin(ECH)and dimethylnitrosamine(NDMA)in drinking water by gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS).Methods Totally 500 ml water sample was extracted by coconut shell solid-phase extraction column,eluted with 10 ml of dichloromethane,and then evaporated by nitrogen into 1.0 ml.After separation by VF-WAXms capillary column,determined by GC-MS/MS under multiple reaction modes(MRM),and quantified by external standard method.Results The regression equation for ECH obtained in the range of 4-200μg/L was y=269.4512x-493.946,r=0.9995,with a good linear relationship.The regression equation for NDMA obtained within the range of 2-100μg/L was y=293.6303x+234.1608,r=0.9997,with a good linear relationship.The limits of detection for ECH and NDMA were 0.0005-0.0002μg/L,respectively,and the lower limits of quantification were 0.015 and 0.006μg/L.The recovery rates of ECH were between 79%-110%,and the RSDs were between 4.9%-9.5%.The NDMA recovery rates were between 83%-118%,and the RSDs were between 7.6%-11.3%.Conclusion The method has low detection limit,high precision and accuracy,and is applicable to simultaneous determination of ECH and NDMA in drinking water.

关 键 词：气相色谱-三重四级杆串联质谱法 环氧氯丙烷 亚硝基二甲胺 生活饮用水 

分 类 号：O657.6[理学—分析化学]