顶空固相微萃取-GC-MS/MS法监测地表水中7种有机溶剂  

Monitoring of seven organic solvents in surface water using headspace solid-phase microextraction GC-MS/MS method

作　　者：姚洋 杨汤燕 张庆鹏 张胜平 刘晓芳 YAO Yang;YANG Yan;ZHANG Qing-peng;ZHANG Sheng-ping;LIU Xiao-fang(Shandong Linyi Ecological Environment Monitoring Center,Linyi 276000,China;Yihe New Area Branch of Linyi Ecological Environment Bureau,Linyi 276000,China)

机构地区：[1]山东省临沂生态环境监测中心,山东临沂276000 [2]临沂市生态环境局沂河新区分局,山东临沂276000

出　　处：《化学研究与应用》2025年第4期1014-1018,共5页Chemical Research and Application

摘　　要：建立顶空固相微萃取技术联合气相色谱三重四级杆质谱(GC-MS/MS)测定地表水中硝基苯、苯胺、甲基叔丁基醚、溴甲烷、溴乙烷、联苯和1,1,1-三氯乙烷7种常见溶剂残留检测方法的检测方法。采用顶空固相微萃取技术,选择聚丙烯酸酯涂层纤维地表水样进行提取。提取液进样色谱质谱系统,外标法定量。硝基苯、苯胺、甲基叔丁基醚、溴甲烷、溴乙烷、联苯和1,1,1-三氯乙烷7种溶剂在质量浓度0.005~0.5μg·mL^(-1)范围内与相应的定量离子峰面积呈良好的线性关系,相关系数均大于0.995。检出限如下:硝基苯:0.00342μg·mL^(-1)、苯胺:0.00435μg·mL^(-1)、甲基叔丁基醚:0.00452μg·mL^(-1)、溴甲烷:0.00476μg·mL^(-1)、溴乙烷:0.00453μg·mL^(-1)、联苯:0.00456μg·mL^(-1)、1,1,1-三氯乙烷:0.00480μg·mL^(-1)。样品在不同水平浓度点的回收率在90.5%~110.3%之间,相对标准偏差在1.78%~4.58%之间(n=6)。该方法操作简单、快速,定性定量准确,适用于地表水中硝基苯等7种有机溶剂残留的监测,为保护地表水环境提供技术参考。Establish a detection method for seven common solvent residues in surface water,including nitrobenzene,aniline,methyl tert butyl ether,bromomethane,bromoethane,biphenyl,and 1,1,1-trichloroethane,using headspace solid-phase microextraction technology combined with gas chromatography triple quadrupole mass spectrometry(GC-MS/MS).Using headspace solid-phase microextraction technology,surface water samples coated with polyacrylate fibers were selected for extraction.Extraction solution injection into chromatography-mass spectrometry system,quantification by external standard method.Nitrobenzene,aniline,methyl tertbutyl ether,bromomethane,bromoethane,biphenyl and 1,1,1-trichloroethane had good linear relationships with quantitative ion peak area in the range 0.005~0.5μg·mL^(-1),correlation coefficients(r^(2))were all above 0.995.Their detection limits were as follows:nitrobenzene::0.00342μg·mL^(-1)、aniline:0.00435μg·mL^(-1)、methyl tert-butyl ether:0.00452μg·mL^(-1)、bromomethane:0.00476μg·mL^(-1)、bromomethane:0.00453μg·mL^(-1)、biphenyl:0.00456μg·mL^(-1)、1,1,1-trichloroethane:0.00480μg·mL^(-1).Recoveries of this method in 3 concentration levels were ranged from 90.5%~110.3%.The results of RSD were 1.78%~4.58%(n=6).This method is easy to operate,fast,and accurate in qualitative and quantitative analysis.It is suitable for monitoring the residues of seven organic solvents,including nitrobenzene,in surface water and provides technical reference for protecting the surface water environment.

关 键 词：顶空固相微萃取 GC-MS/MS 地表水 溶剂残留 

分 类 号：O657.7[理学—分析化学]