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Volume 34 Issue 2
Mar.  2015
Article Contents

Citation:

Determination of trichlorobenzenes in sea water by dispersive liquid-liquid microextraction-gas chromatography/mass method

  • Received Date: 2014-02-03
    Accepted Date: 2014-04-14
  • Studies on the determination of trichlorobenzenes (TCBs) in sea water, by dispersive liquid-liquid microextraction (DLLME)-gas chromatography/mass (GC/MS) method, have been carried out. Parameters, such as the kind and volume of extraction solvent, disperser solvent, extraction time and temperature, were intensively studied and optimized. The result showed that the optimized DLLME condition was obtained when 0.5 mL of actone (disperser solvent), containing 10 L chlorobenze (extraction solvent) was used for the treatment of 10 mL synthetic seawater samples with 10 min-ultrasonic extaction at 25℃. Overall recoveries of the present method were 97.8%~102.5%with RSD values at 2.8%~6.6%. The detective limits for 1, 3, 5-, 1, 2, 4- and 1, 2, 3- TCB were 1.5 g/L, 0.5 g/L and 2.0 g/L, respectively. Comparing with traditional sample preparation procedures, e. g. head-space, liquid-liquid extraction and solid phase extraction, the present method was accurate, better enrichment property, better repeatability, easier to be operated with less interference. The present method has been applied for the determination of the TCBs residue concentration of 5 real samples. The result showed that two of them were found to contain 2~3 kinds of these TCBs. The TCBs detected in the studied samples were at concentration of(1.9~6.7)g/L.
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  • [1] 杨 瑾.近海水域的污染危害与防治[J].海洋开发与管理, 2007(6):77-80.[2]杜青平, 黄彩娜, 贾晓珊, 等.1, 2, 4-三氯苯对3种海洋微藻的毒性效应[J].生态环境, 2007, 16(2):352-357.[6]魏复盛.水和废水监测分析方法[M].第四版.北京:中国环境科学出版社, 2002.[7]顾海东.吹扫捕集-气相色谱法测定水中挥发性卤代烃和氯苯[J].环境监测管理与技术, 2002, 14(6):24-25.[8]安 琼, 董元华, 倪 俊, 等.气相色谱法测定禽蛋中微量有机氯农药及多氯联苯的残留[J].色谱, 2002, 20(2):167-171.[9]李 竺, 郜洪文, 陈 玲, 等.固相萃取技术在环境中农药残留分析的研究进展[J].世界科技研究与发展, 2005, 27(5):64-71.[10] U.S.ENVIRONMENTAL PROTECTION AGENCY.EPA Method 504.1:1, 2-dibromoethane (EDB), 1, 2-dibromo-3-chloro-propane (DBCP), and 1, 2, 3-trichlorichlorobenzene(123TCP) in water by microextraction and gas chromatography[S].[12]ZHAO L M, LEE H K.Application of static liquid-phase microextraction to the analysis of organochlorine pesticides in water[J].Journal of Chromatography A, 200l, 919(2):381-388.[15]张成功, 赵 倩, 陈 波, 等.液-液-液三相液相微萃取-高效液相色谱法检测尿样中的安非他明和氯胺酮[J].色谱, 2007, 25(5):641-645.[20]张正斌, 陈振东, 刘莲生, 等.海洋化学原理和应用:中国近海的海洋化学[M].北京:海洋出版社, 1999.[21]沈昊宇, 赵永纲, 怀明敏, 等.分散液-液微萃取-气相色谱/质谱联用法测定机械加工水基切削液及其废水中的三氯苯[J].色谱, 2009, 27(1):63-68.
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Determination of trichlorobenzenes in sea water by dispersive liquid-liquid microextraction-gas chromatography/mass method

  • 1. Ningbo Institute of Technology, Zhejiang University, Zhejiang, Ningbo 315100, China;
  • 2. Marine Environmental Monitoring Center of Ningbo, SOA, Ningbo 315012, China;
  • 3. Hubei Collaborative Innovation Center for Advanced Organochemical Materials, & Ministry-of-Education Key Laboratory for the Synthesis and Applications of Organic Functional Molecules, Hubei University, Wuhan 430062, China

Abstract: Studies on the determination of trichlorobenzenes (TCBs) in sea water, by dispersive liquid-liquid microextraction (DLLME)-gas chromatography/mass (GC/MS) method, have been carried out. Parameters, such as the kind and volume of extraction solvent, disperser solvent, extraction time and temperature, were intensively studied and optimized. The result showed that the optimized DLLME condition was obtained when 0.5 mL of actone (disperser solvent), containing 10 L chlorobenze (extraction solvent) was used for the treatment of 10 mL synthetic seawater samples with 10 min-ultrasonic extaction at 25℃. Overall recoveries of the present method were 97.8%~102.5%with RSD values at 2.8%~6.6%. The detective limits for 1, 3, 5-, 1, 2, 4- and 1, 2, 3- TCB were 1.5 g/L, 0.5 g/L and 2.0 g/L, respectively. Comparing with traditional sample preparation procedures, e. g. head-space, liquid-liquid extraction and solid phase extraction, the present method was accurate, better enrichment property, better repeatability, easier to be operated with less interference. The present method has been applied for the determination of the TCBs residue concentration of 5 real samples. The result showed that two of them were found to contain 2~3 kinds of these TCBs. The TCBs detected in the studied samples were at concentration of(1.9~6.7)g/L.

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