大体积全自动固相萃取-气相色谱-质谱法同时测定饮用水中43种半挥发性有机物  

Simultaneous determination of 43 compounds of semi-volatile organic compounds in drinking water by gas chromatography-mass spectrometry with automatic bulk solid phase extraction

作　　者：梁素丹 陈剑刚[1] 林丽玲[1] 张艳[1] 冯翠霞[1] LIANG Sudan;CHEN Jiangang;LIN Liling;ZHANG Yan;FENG Cuixia(Zhuhai Center for Disease Control and Prevention,Guangdong Zhuhai 519000,China)

机构地区：[1]珠海市疾病预防控制中心

出　　处：《中国食品卫生杂志》2019年第6期533-540,共8页Chinese Journal of Food Hygiene

基　　金：珠海市科技计划项目(20171009E030065)

摘　　要：目的建立大体积全自动固相萃取-气相色谱-质谱(SPE-GC-MS)法同时测定饮用水中43种半挥发性有机物(SVOCs)。方法 1.0 L饮用水样品经HLB固相萃取柱富集、净化后,分别以2 ml乙酸乙酯、4 ml二氯甲烷洗脱,洗脱液氮吹浓缩至0.5 ml,用乙酸乙酯定容至1.0 ml,经HP-5 ms UI超高惰性毛细管柱(30 m×250μm,0.25μm)分离,采用GC-MS的选择离子扫描模式(SIM)分析,以保留时间和特征离子定性,内标法定量。结果 43种SVOCs均得到有效分离,方法的线性关系良好,相关系数r^2≥0.995,方法检出限为0.000 13~0.008 2μg/L,定量限为0.000 42~0.027μg/L,平均回收率为70.0%~138%,精密度为0.3%~12.1%。应用该方法测定16份不同水质样品,结果共检出六氯苯、五氯硝基苯和萘等10种SVOCs。结论本方法灵敏、高效,适用于饮用水中多种SVOCs的同时检测,可为突发公共卫生事件提供依据。Objective To establish a method for the simultaneous determination of 43 compounds of semi-volatile organic compounds(SVOCs) in drinking water by gas chromatography-mass spectrometry with automatic bulk solid phase extraction(SPE-GC-MS). Methods SVOCs in 1.0 L drinking water sample were enriched and purified by HLB solid phase extraction column, eluted by 2 ml ethyl acetate and 4 ml dichloromethane, purged and concentrated to 0.5 ml and volumed to 1.0 ml by ethyl acetate, separated by HP-5 ms ultra-inert capillary column(30 m×250 μm,0.25 μm), and then analyzed by selective ion scanning mode(SIM) coupled with GC-MS. Qualitative analysis was performed by retention time and characteristic ions, and quantitative analysis was performed by the internal standard method. Results Forty-three compounds of SVOCs were effectively separated and showed good linear relationship(r^2≥0.995). The detection limits and quantitative limits of the method were 0.000 13-0.008 2 μg/L and 0.000 42-0.027 μg/L. The recoveries and precisions were 70.0%-138% and 0.3%-12.1%. Sixteen samples of different water were determined by the method, and ten compounds of SVOCs such as hexachlorobenzene, pentachloronitrobenzene and naphthalene were detected. Conclusion The method was sensitive and efficient, it was suitable for simultaneous detection of SVOCs in drinking water and provide a basis for public health emergencies.

关 键 词：气相色谱-质谱 饮用水 半挥发性有机物 全自动固相萃取 

分 类 号：R155[医药卫生—营养与食品卫生学]