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.
作者
江阳
李九龙
袁悦
曹凤梅
李虹霖
雍莉
冯子男
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)
出处
《环境化学》
北大核心
2025年第1期131-139,共9页
Environmental Chemistry
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
headspace solid phase microextraction
gas chromatography-mass spectrometry
chlorophenols
drinking water
