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顶空固相微萃取-气相色谱-质谱联用测定黑臭水体中的4种主要异味物质

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夏雪, 陈倩茹, 王川, 陈迪松, 张丽萍, 武俊梅, 周巧红, 吴振斌. 顶空固相微萃取-气相色谱-质谱联用测定黑臭水体中的4种主要异味物质[J]. 环境化学, 2019, (12): 2789-2796. doi: 10.7524/j.issn.0254-6108.2019011601
引用本文: 夏雪, 陈倩茹, 王川, 陈迪松, 张丽萍, 武俊梅, 周巧红, 吴振斌.

顶空固相微萃取-气相色谱-质谱联用测定黑臭水体中的4种主要异味物质

[J]. 环境化学, 2019, (12): 2789-2796. doi: 10.7524/j.issn.0254-6108.2019011601
shu
XIA Xue, CHEN Qianru, WANG Chuan, CHEN Disong, ZHANG Liping, WU Junmei, ZHOU Qiaohong, WU Zhenbin. Determination of four major odor compounds in black and odorous water by headspace solid phase microextraction combined with gas chromatography-mass spectrometry[J]. Environmental Chemistry, 2019, (12): 2789-2796. doi: 10.7524/j.issn.0254-6108.2019011601
Citation: XIA Xue, CHEN Qianru, WANG Chuan, CHEN Disong, ZHANG Liping, WU Junmei, ZHOU Qiaohong, WU Zhenbin.

Determination of four major odor compounds in black and odorous water by headspace solid phase microextraction combined with gas chromatography-mass spectrometry

[J]. Environmental Chemistry, 2019, (12): 2789-2796. doi: 10.7524/j.issn.0254-6108.2019011601
shu

顶空固相微萃取-气相色谱-质谱联用测定黑臭水体中的4种主要异味物质

  • 1. 中国科学院水生生物研究所, 淡水生态与生物技术国家重点实验室, 武汉, 430072;

  • 2. 中国科学院大学, 北京, 100049;

  • 3. 武汉理工大学资源与环境工程学院, 武汉, 430070

    • 通讯作者: 武俊梅, E-mail: wujunmei@ihb.ac.cn ; 
  • 基金项目:

    国家"十三五"水专项（2017ZX07602002-004）资助.

Determination of four major odor compounds in black and odorous water by headspace solid phase microextraction combined with gas chromatography-mass spectrometry

  • 1. State Key Laboratory of Freshwater Ecology and Biotechnology, Institute of Hydrobiology, Chinese Academy of Sciences, Wuhan, 430072, China;

  • 2. University of Chinese Academy of Sciences, Beijing, 100049, China;

  • 3. School of Resource & Environmental Engineering, Wuhan University of Technology, Wuhan, 430070, China

    • Corresponding author: WU Junmei, wujunmei@ihb.ac.cn ; 
  • Fund Project: Supported by Major Science and Technology Program for Water Pollution Control and Treatment of China 13th Five-Year Plan (2017ZX07602002-004).

  • 摘要:

    采用顶空固相微萃取-气相色谱-质谱联用测定黑臭水体中的4种主要异味物质，即土腥素、2-甲基异茨醇、β-环柠檬醛、β-紫罗兰酮.从萃取纤维、萃取温度、离子浓度、萃取时间、搅拌速率、解吸时间和解吸温度等7个方面对方法进行优化.结果表明，当选用85 μm CAR/PDMS萃取纤维，萃取温度60℃，20%（NaCl/水），1250 r·min-1搅拌速率条件下萃取40 min，并于GC进样口250℃高温下解吸4 min时效果最佳.4种异味物质在5-1000 ng·L-1范围内线性良好，检出限在0.73-1.14 ng·L-1之间，加标回收率在92.3%-109%之间.基于上述方法，对安徽省阜阳境内黑臭水体检测，4种目标物质均有检出.实验证明，此方法可用于黑臭水体中异味物质的分析检测.

    Abstract:

    Four major odor compounds in black and odorous water including geosmin, 2-methylisobomeol, β-cyclocitral and β-ionone were determined by headspace solid phase microextraction combined with gas chromatography-mass spectrometry. The method was optimized with regards to extraction fiber, extraction temperature, ionic strength, extraction time, stirring rate, desorption time and desorption temperature. The results showed that the optimal conditions of extraction fiber, extraction temperature, ionic strength, extraction time, stirring rate, desorption time and desorption temperature were 85 μm CAR/PDMS, 60℃, 20%, 40 min, 1250 r·min-1, 4 min and 250℃, respectively. The method had linear response within the range of 5-1000 ng·L-1, and the detection limits were between 0.73 and 1.14 ng·L-1. The recoveries of the four odor compounds in pure water were in range of 92.3%-109%. Based on the above method, four target compounds were detected in black and odorous water in Fuyang, Anhui Province. The experiment proved that this method can be used for the analysis and detection of odorous substances in black and odorous water.

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  • 收稿日期:  2019-01-16
  • 刊出日期:  2019-12-10

顶空固相微萃取-气相色谱-质谱联用测定黑臭水体中的4种主要异味物质

    通讯作者: 武俊梅, E-mail: wujunmei@ihb.ac.cn ; 
  • 1. 中国科学院水生生物研究所, 淡水生态与生物技术国家重点实验室, 武汉, 430072;
  • 2. 中国科学院大学, 北京, 100049;
  • 3. 武汉理工大学资源与环境工程学院, 武汉, 430070
  • 收稿日期:  2019-01-16
  • 网络出版日期:  2019-12-10
基金项目:

国家"十三五"水专项（2017ZX07602002-004）资助.

摘要: 

采用顶空固相微萃取-气相色谱-质谱联用测定黑臭水体中的4种主要异味物质，即土腥素、2-甲基异茨醇、β-环柠檬醛、β-紫罗兰酮.从萃取纤维、萃取温度、离子浓度、萃取时间、搅拌速率、解吸时间和解吸温度等7个方面对方法进行优化.结果表明，当选用85 μm CAR/PDMS萃取纤维，萃取温度60℃，20%（NaCl/水），1250 r·min-1搅拌速率条件下萃取40 min，并于GC进样口250℃高温下解吸4 min时效果最佳.4种异味物质在5-1000 ng·L-1范围内线性良好，检出限在0.73-1.14 ng·L-1之间，加标回收率在92.3%-109%之间.基于上述方法，对安徽省阜阳境内黑臭水体检测，4种目标物质均有检出.实验证明，此方法可用于黑臭水体中异味物质的分析检测.

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