基于全自动在线顶空固相微萃取-气相色谱-质谱联用技术测定生活饮用水中4种氯酚  

Determination of four chlorophenols in drinking water based on automatic online headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry

作　　者：江阳[1] 李九龙 袁悦 曹凤梅 李虹霖 雍莉[1] 冯子男[1] 李永新 JIANG Yang;LI Jiulong;YUAN Yue;CAO Fengmei;LI Honglin;YONG Li;FENG Zinan;LI Yongxin(Sichuan Provincial Center for Disease Control and Prevention,Chengdu,610041,China;West China School of Public Health and West China Fourth Hospital,Sichuan University,Chengdu,610041,China)

机构地区：[1]四川省疾病预防控制中心理化检验所,成都610041 [2]四川大学华西公共卫生学院(华西第四医院),成都610041

出　　处：《环境化学》2025年第1期131-139,共9页Environmental Chemistry

摘　　要：建立了全自动在线顶空固相微萃取-气相色谱-质谱联用(HS-SPME-GC-MS)分析法同时测定生活饮用水中2-氯酚、2,4-二氯酚、2,4,6-三氯酚和五氯酚.通过单因素实验设计考察了萃取纤维、萃取温度、萃取时间、加盐量、加酸量、消毒剂余量等对萃取效果的影响.优化后的顶空固相微萃取条件为:取10 mL水样于20 mL顶空瓶中,加入3.6 g NaCl、0.1 mL 1 mol·L^(−1)盐酸溶液,使用65μm DVB/PDMS纤维头,萃取温度60℃,萃取时间60 min,振摇速率450 r·min^(−1),解吸时间5 min,解吸温度280℃.4种氯酚浓度-响应线性关系良好,相关系数r均大于0.9994,方法检出限为0.015—0.060μg·L^(−1),方法定量限为0.050—0.20μg·L^(−1),平均回收率为90.4%—115%,相对标准偏差为0.47%—6.91%.该方法具有准确、便捷、灵敏度高等优点,适用于生活饮用水中多种氯酚的同时测定.An automatic online headspace solid-phase microextraction(HS-SPME)-gas chromatography-mass spectrometry(GC-MS)method has been developed for simultaneous determination of 2-chlorophenol,2,4-dichlorophenol,2,4,6-trichlorophenol,and pentachlorophenol in drinking water.The effects of extraction fiber type,extraction temperature,extraction time,salt concentration,acid concentration and residual chlorine on the extraction efficiencies were investigated by one-way experimental design.The optimized HS-SPME parameters were as follows:A 10 mL water sample was taken in a 20-mL headspace bottle with addition of 3.6 g NaCl and 0.1 mL 1 mol·L^(−1)hydrochloric acid solution.The target chlorophenols were extracted for 60 min with a 65μm DVB/PDMS fiber coating under an extraction temperature of 60℃and with a shaking rate of 450 r·min^(−1),desorbed for 5 min under desorption temperature of 280℃.Good concentration-response linear relationship was obtained for four target chlorophenols with the correlation coefficients(r)greater than 0.9994.The limits of detection(LODs)were from 0.015μg·L^(−1)to 0.060μg·L^(−1),and the limits of quantification(LOQs)were from 0.050μg·L^(−1)to 0.20μg·L^(−1).The average recoveries of the four chlorophenols ranged from 90.4%to 115%,and the relative standard deviations were 0.47%to 6.91%.The established method has the advantages of accuracy,rapidity and high sensitivity,and is suitable for simultaneous determination of multiple chlorophenols in drinking water.

关 键 词：顶空固相微萃取 气相色谱质谱联用 氯酚 生活饮用水 

分 类 号：R123[医药卫生—环境卫生学]