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高等学校化学研究 ›› 2011, Vol. 27 ›› Issue (6): 939-943.

• Articles • 上一篇    下一篇

Liquid-liquid Microextraction Based on Solidification of Floating Organic Drops Coupled with Gas Chromatography for Analyzing Trace Benzene, Toluene and Xylene in Water Samples

ZHANG Mao-sheng1*, HUANG Jia-rong2, ZHENG Xiang-hua3 and XIE Qiong-fang1   

  1. 1. Department of Chemistry and Environmental Science, Zhangzhou Normal University, Zhangzhou 363000, P. R. China;
    2. Zhangzhou Entry-Exit Inspection and Quarantine Bureau, Zhangzhou 363000, P. R. China;
    3. Inspection and Quarantine Technical Center, Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361012, P. R. China
  • 收稿日期:2010-12-22 修回日期:2011-03-28 出版日期:2011-11-25 发布日期:2011-11-07
  • 通讯作者: ZHANG Mao-sheng E-mail:maoshengzhang@fjzs.edu.cn
  • 基金资助:

    Supported by the National Natural Science Foundation of China(No.21105088) and the Program for Science and Technology Projects of the Education Department of Fujian Province, China (No.JA10211).

Liquid-liquid Microextraction Based on Solidification of Floating Organic Drops Coupled with Gas Chromatography for Analyzing Trace Benzene, Toluene and Xylene in Water Samples

ZHANG Mao-sheng1*, HUANG Jia-rong2, ZHENG Xiang-hua3 and XIE Qiong-fang1   

  1. 1. Department of Chemistry and Environmental Science, Zhangzhou Normal University, Zhangzhou 363000, P. R. China;
    2. Zhangzhou Entry-Exit Inspection and Quarantine Bureau, Zhangzhou 363000, P. R. China;
    3. Inspection and Quarantine Technical Center, Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361012, P. R. China
  • Received:2010-12-22 Revised:2011-03-28 Online:2011-11-25 Published:2011-11-07
  • Contact: ZHANG Mao-sheng E-mail:maoshengzhang@fjzs.edu.cn
  • Supported by:

    Supported by the National Natural Science Foundation of China(No.21105088) and the Program for Science and Technology Projects of the Education Department of Fujian Province, China (No.JA10211).

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摘要： A new liquid-liquid microextraction method based on the solidification of floating organic drops coupled with gas chromatography was developed for the determination of trace benzene, toluene and xylene(BTX) in water samples. In the microextraction procedure, a microdrop of n-decanol was delivered to the surface of the analytes’ solution, and stirred for a desired time. Following the absolute extraction, the sample vial was cooled in an ice bath for 10 min. The solidified n-decanol was then transferred into a plastic tube and melted naturally; and 1 μL of it was injected into gas chromatography for analysis. Factors relevant to the extraction efficiency were studied and optimized. The optimal experimental conditions were: 15 μL of n-decanol as extractive solvent, 30 mL of solution containing analytes, no salt, the stirring rate 400 r/min, the extraction temperature 30 °C, and the extraction time 30 min. Under those optimized conditions, the detection limit(LOD) of analytes was in a range of 0.05―0.10 ng/mL by the developed method. A good linearity(r>0.99) in a calibration range of 0.01―100 μg/mL was obtained. The recoveries of the real samples at different spiked levels of BTX were in the range from 92.2% to 103.4%.

关键词: Gas chromatography, Liquid-liquid microextraction, Solidified floating organic drop, n-Decanol

Abstract: A new liquid-liquid microextraction method based on the solidification of floating organic drops coupled with gas chromatography was developed for the determination of trace benzene, toluene and xylene(BTX) in water samples. In the microextraction procedure, a microdrop of n-decanol was delivered to the surface of the analytes’ solution, and stirred for a desired time. Following the absolute extraction, the sample vial was cooled in an ice bath for 10 min. The solidified n-decanol was then transferred into a plastic tube and melted naturally; and 1 μL of it was injected into gas chromatography for analysis. Factors relevant to the extraction efficiency were studied and optimized. The optimal experimental conditions were: 15 μL of n-decanol as extractive solvent, 30 mL of solution containing analytes, no salt, the stirring rate 400 r/min, the extraction temperature 30 °C, and the extraction time 30 min. Under those optimized conditions, the detection limit(LOD) of analytes was in a range of 0.05―0.10 ng/mL by the developed method. A good linearity(r>0.99) in a calibration range of 0.01―100 μg/mL was obtained. The recoveries of the real samples at different spiked levels of BTX were in the range from 92.2% to 103.4%.

Key words: Gas chromatography, Liquid-liquid microextraction, Solidified floating organic drop, n-Decanol