固相萃取-气相色谱-质谱法测定地表水中的氯苯类化合物  

Determination of chlorobenzenes in surface water by solid phase extraction and gas chromatography-mass spectrometry

作　　者：王桂珍 王金花 张飞 蒋宗园 范思艺 宁东峰[3] WANG Guizhen;WANG Jinhua;ZHANG Fei;JIANG Zongyuan;FAN Siyi;NING Dongfeng(Environmental Monitoring Center for the Central Line Project of South-to-North Water Diversion of Henan,Nanyang 473000,China;Henan Nanyang Ecological Environment Monitoring Center,Nanyang 473000,China;Institute of Farmland Irrigation,Chinese Academy of Agricultural Sciences,Xinxiang 453002,China)

机构地区：[1]河南省南水北调渠首生态环境监测应急中心,河南南阳473000 [2]河南省南阳生态环境监测中心,河南南阳473000 [3]中国农业科学院农田灌溉研究所,河南新乡453002

出　　处：《化学分析计量》2024年第2期40-45,共6页Chemical Analysis And Meterage

摘　　要：建立同时测定地表水中7种氯苯类化合物的固相萃取-气相色谱-质谱(GC-MS)法。样品中的氯苯类化合物经HLB固相萃取柱分离,通过5.0 mL乙酸乙酯和7.5 mL二氯甲烷进行洗脱提取,干燥浓缩后,选择DB-5MS毛细管柱作为分离柱,用GC-MS法测定,外标法定量。结果表明,在各自的线性范围内,氯苯类化合物的响应值与其质量浓度的线性关系良好,相关系数均大于0.9995,痕量水平下回收率为79.9%~115.7%,相对标准偏差为2.8%~10.3%(n=6),方法检出限为0.14~0.30μg/L。该方法简便、准确,灵敏度高,可以为地表水中氯苯类化合物的测定提供一定的技术支撑。An analytical method was developed for the determination of seven chlorobenzenes in surface water using solid phase extraction and gas chromatography-mass spectrometry(GC-MS).The chlorobenzene compounds in the samples were separated by HLB solid phase extraction column,eluted and extracted by 5.0 mL ethyl acetate and 7.5 mL dichloromethane.After drying and concentration,DB-5MS capillary column was selected as the separation column,determined by GC-MS,and quantified by external standard method.The results showed that the response values of chlorobenzenes had a good linear relationship with their mass concentrations in their respective linear ranges.The correlation coefficients were all more than 0.9995.The recoveries of seven chlorobenzenes at ultra-trace level were 79.9%-115.7%and the relative standard deviations(RSD)were 2.8%-10.3%(n=6).The detection limit of seven chlorobenzenes were in range of 0.14-0.30μg/L.The method has merits of simplicity,accuracy,sensitivity,which can be used for the test requirements of chlorobenzenes in drinking water.

关 键 词：固相萃取 气相色谱-质谱法 氯苯类化合物 

分 类 号：O657.71[理学—分析化学]