首页|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

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

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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4~200 µg/L的范围内,所得ECH的回归方程为y=269.451 2x-493.946,r=0.999 5,线性关系良好;在2~100 μg/L的范围内,所得NDMA的回归方程为y=293.630 3x+234.160 8,r=0.999 7,线性关系良好.该方法对ECH、NDMA的方法检出限分别为0.000 5、0.000 2µg/L,定量下限分别为0.015、0.006 µg/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.
Determination of epichlorohydrin and dimethylnitrosamine in drinking water by gas chromatography-triple-quadrupole mass spectrometry
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 4-200 μg/L was y=269.451 2x-493.946,r=0.999 5,with a good linear relationship.The regression equation for NDMA obtained within the range of 2-100 μg/L was y=293.630 3x+234.160 8,r=0.999 7,with a good linear relationship.The limits of detection for ECH and NDMA were 0.0005-0.0002 μg/L,respectively,and the lower limits of quantification were 0.015 and 0.006 μg/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.

Gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS)EpichlorohydrinDimethylnitrosamineDrinking water

倪海平、刘祥萍、陈春静、董妍、袁婷婷、陈明聪、李冬宁、朱醇

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南京市疾病预防控制中心理化检验科,江苏南京 210003

南京市疾病预防控制中心环境卫生科

南京市鼓楼区疾病预防控制中心检验科

江苏省疾病预防控制中心理化所,南京 210009

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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

2024

环境与健康杂志
中华预防医学会,天津市疾病预防控制中心

环境与健康杂志

CSTPCD
影响因子:0.658
ISSN:1001-5914
年,卷(期):2024.41(11)