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超高效液相色谱荧光检测法测定空气中甲基苯胺同分异构体及对氯代苯胺

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王绍俊, 王超, 石庭山, 陈烨, 吕怡兵, 周益民. 超高效液相色谱荧光检测法测定空气中甲基苯胺同分异构体及对氯代苯胺[J]. 环境化学, 2016, 35(3): 460-465. doi: 10.7524/j.issn.0254-6108.2016.03.2015081202
引用本文: 王绍俊, 王超, 石庭山, 陈烨, 吕怡兵, 周益民. 超高效液相色谱荧光检测法测定空气中甲基苯胺同分异构体及对氯代苯胺[J]. 环境化学, 2016, 35(3): 460-465. doi: 10.7524/j.issn.0254-6108.2016.03.2015081202
shu
WANG Shaojun, WANG Chao, SHI Tingshan, CHEN Ye, LYU Yibing, ZHOU Yimin. Analysis of toluidines isomers and p-chloroaniline in air by ultra performance liquid chromatography with fluorescence detection[J]. Environmental Chemistry, 2016, 35(3): 460-465. doi: 10.7524/j.issn.0254-6108.2016.03.2015081202
Citation: WANG Shaojun, WANG Chao, SHI Tingshan, CHEN Ye, LYU Yibing, ZHOU Yimin. Analysis of toluidines isomers and p-chloroaniline in air by ultra performance liquid chromatography with fluorescence detection[J]. Environmental Chemistry, 2016, 35(3): 460-465. doi: 10.7524/j.issn.0254-6108.2016.03.2015081202
shu

超高效液相色谱荧光检测法测定空气中甲基苯胺同分异构体及对氯代苯胺

  • 1.

    新疆生产建设兵团环境监测中心站, 乌鲁木齐, 830011;

  • 2.

    中国环境监测总站, 北京, 100012

  • 基金项目:

    863计划(NO.2013AA06A308)资助.

Analysis of toluidines isomers and p-chloroaniline in air by ultra performance liquid chromatography with fluorescence detection

  • 1.

    Central Station of Environment Monitoring, Xinjiang Production and Construction Corps, Urumqi, 830011, China;

  • 2.

    China National Environmental Monitoring Center, Beijing, 100012, China

  • Fund Project: Supported by the National High-tech R&D Program (863 Program) (2013AA06A308).

  • 摘要: 建立了空气中甲基苯胺同分异构体及对氯代苯胺的硅胶吸附管采样-超高效液相色谱荧光检测分析方法.通过硅胶填料吸附管,采集空气中甲基苯胺和氯代苯胺.采用含1%氨水的甲醇,对硅胶填料解吸20 min.解吸溶液经0.22 μm滤膜过滤,采用超高效液相色谱法分析,选择235 nm和335 nm作为荧光检测的激发和发射波长.4种苯胺类化合物在4.5 min内得到分离,在0.1-2.0 mg·L-1范围内线性关系良好,相关系数均大于0.999,方法检出限(S/N=3)为0.11-0.4 μg·m-3(采样体积以10 L计),在0.5、1.0、2.0 μg加标水平(相当于10 L空气中甲基苯胺和氯代苯胺浓度为50、100、200 μg·m-3)下,回收率分别为95%-98%、94%-103%和95%-102%,RSD分别为1.0%-2.2%、1.6%-3.7%和1.3%-2.1%.结果表明,该方法适用于空气中甲基苯胺同分异构体及对氯代苯胺的同时分析.
    Abstract: A method the for analysis of toluidines isomers and p-chloroaniline in air was established using silica gel tube sampling-ultra performance liquid chromatography with fluorescence detection. Silica gel tube was used to collect toluidines isomers and p-chloroaniline in the air. Then a solution of 1 mL methanol with 1% ammonia was used to desorb toluidines isomers and p-chloroaniline in 20 min at room temperature. The desorption solution was filtered through 0.22 μm microfiltration membrane and analyzed by ultra performance liquid chromatography with fluorescence detection. The detection wavelengths(λex/λem) for toluidines isomers and p-chloroaniline was 235 nm/335 nm. Four aniline derivatives were separated within 4.5 min. The calibration curves were linear in the range of 0.1-2.0 mg·L-1. The correlation coefficients were more than 0.999. The method limits of detection (S/N=3) were 0.11-0.4 μg·m-3 assuming the sampling volume was 10 L. The recoveries of toluidines isomers and p-chloroaniline at spiked levels of 0.5, 1.0 and 2.0 μg(equivalent to 50, 100 and 200 μg·m-3 in the 10 L air) were 95%-98%, 94%-103% and 95%-102%, with the relative standard deviation of 1.0%-2.2%, 1.6%-3.7% and 1.3%-2.1%, respectively. The optimized method is robust and reliable for simultaneous detection of toluidines isomers and p-chloroaniline in the air.
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    WANG T, WANG F, MA W P. Quantifying the anilines in ambient air by HPLC[J]. Anhui Agri.Sci.Bull,2015,2015,21(7):25-26(in Chinese).

    [7] 王超, 吕怡兵, 滕恩江, 等. 超高压液相色谱荧光检测法快速测定水中痕量苯胺与联苯胺[J]. 分析测试学报, 2013, 32(1):32-37.

    WANG C, LYU Y B, TENG E J, et al. Determination of trace aniline and benzidine in environmental water by ultrahigh-pressure liquid chromatography with fluorescence detection[J]. Journal of Instrumental Analysis, 2013, 32(1):32-37(in Chinese).

    [8] 王超, 王绍俊, 陈烨, 等. 硅胶吸附管采样-超高效液相色谱法测定空气中7种苯胺类化合物[J]. 环境化学, 2015, 34(3):584-585.

    WANG C, WANG S J, CHEN Y. et al. Simultaneous analysis of seven aniline derivatives in air by ultra performance liquid chromatography using silica gel tube sampling[J]. Environmental Chemistry, 2015, 34(3):584-585(in Chinese).

    [9] 王超, 彭涛, 吕怡兵, 等. 液相色谱法测定水中16种多环芳烃的方法优化[J]. 环境化学, 2014, 33(1):62-68.

    WANG C, PENG T, LYU Y B, et al. Optimization of liquid chromatography method for detection of 16 polycyclic aromatic hydrocarbons in environmental water[J]. Environmental Chemistry, 2014, 33(1):62-68(in Chinese).

    [10] 王超, 彭涛, 高愈霄,等. 混合型固相萃取/超高压液相色谱法测定废水中苯胺类化合物[J]. 分析测试学报, 2013, 32(12):1415-1420.

    WANG C, PENG T, GAO Y X, et al. Determination of aniline derivatives in waste water by ultrahigh-pressure liquid chromatography using mixed-mode solid phase extraction[J]. Journal of Instrumental Analysis, 2013, 32(12):1415-1420(in Chinese).

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  • 收稿日期:  2015-08-12
  • 刊出日期:  2016-03-15
王绍俊, 王超, 石庭山, 陈烨, 吕怡兵, 周益民. 超高效液相色谱荧光检测法测定空气中甲基苯胺同分异构体及对氯代苯胺[J]. 环境化学, 2016, 35(3): 460-465. doi: 10.7524/j.issn.0254-6108.2016.03.2015081202
引用本文: 王绍俊, 王超, 石庭山, 陈烨, 吕怡兵, 周益民. 超高效液相色谱荧光检测法测定空气中甲基苯胺同分异构体及对氯代苯胺[J]. 环境化学, 2016, 35(3): 460-465. doi: 10.7524/j.issn.0254-6108.2016.03.2015081202
shu
WANG Shaojun, WANG Chao, SHI Tingshan, CHEN Ye, LYU Yibing, ZHOU Yimin. Analysis of toluidines isomers and p-chloroaniline in air by ultra performance liquid chromatography with fluorescence detection[J]. Environmental Chemistry, 2016, 35(3): 460-465. doi: 10.7524/j.issn.0254-6108.2016.03.2015081202
Citation: WANG Shaojun, WANG Chao, SHI Tingshan, CHEN Ye, LYU Yibing, ZHOU Yimin. Analysis of toluidines isomers and p-chloroaniline in air by ultra performance liquid chromatography with fluorescence detection[J]. Environmental Chemistry, 2016, 35(3): 460-465. doi: 10.7524/j.issn.0254-6108.2016.03.2015081202
shu

超高效液相色谱荧光检测法测定空气中甲基苯胺同分异构体及对氯代苯胺

  • 1.  新疆生产建设兵团环境监测中心站, 乌鲁木齐, 830011;
  • 2.  中国环境监测总站, 北京, 100012
  • 收稿日期:  2015-08-12
基金项目:

863计划(NO.2013AA06A308)资助.

摘要: 建立了空气中甲基苯胺同分异构体及对氯代苯胺的硅胶吸附管采样-超高效液相色谱荧光检测分析方法.通过硅胶填料吸附管,采集空气中甲基苯胺和氯代苯胺.采用含1%氨水的甲醇,对硅胶填料解吸20 min.解吸溶液经0.22 μm滤膜过滤,采用超高效液相色谱法分析,选择235 nm和335 nm作为荧光检测的激发和发射波长.4种苯胺类化合物在4.5 min内得到分离,在0.1-2.0 mg·L-1范围内线性关系良好,相关系数均大于0.999,方法检出限(S/N=3)为0.11-0.4 μg·m-3(采样体积以10 L计),在0.5、1.0、2.0 μg加标水平(相当于10 L空气中甲基苯胺和氯代苯胺浓度为50、100、200 μg·m-3)下,回收率分别为95%-98%、94%-103%和95%-102%,RSD分别为1.0%-2.2%、1.6%-3.7%和1.3%-2.1%.结果表明,该方法适用于空气中甲基苯胺同分异构体及对氯代苯胺的同时分析.

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