| 苯胺的健康效应研究进展 |
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| 引用本文： | 吴悦，赖永忠，陆国永，等. 顶空/气相色谱-质谱法同时测定印染废水中吡啶、苯胺和硝基苯[J]. 岩矿测试，2023，42（4）：781−792. DOI: 10.15898/j.ykcs.202303280041 |
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| 作者姓名： | 吴悦 赖永忠 陆国永 林晓昇 梁树生 许文帅 |
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| 作者单位： | 1.汕头职业技术学院建设生态学院，广东 汕头 515041;2.汕头大学海洋生物研究所，广东 汕头 515063;3.汕头大学广东省海洋生物技术重点实验室，广东 汕头 515063;4.广东省汕头生态环境监测中心站，广东 汕头 515041 |
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| 基金项目： | 广东省高职院校高水平专业群建设项目（GSPZYQ2021004）；广东省职业技术教育学会第四届理事会2023—2024年度科研规划课题（202212G237）；2023年广东省科技创新战略专项项目（STKJ2023026，STKJ2023027） |
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| 摘 要： | 吡啶、苯胺和硝基苯是重要的化工原料，因其低沸点、易挥发和极性强等特征，极易进入环境水体，并造成污染。基体复杂的印染废水含吡啶、苯胺和硝基苯等多种致癌的含氮有机污染物，排入外环境的印染废水将通过食物链影响人类健康，建立印染废水中三种化合物同时检测的方法对于保障工业外排水质安全至关重要。本文通过优化顶空条件等方法参数，建立了同时检测印染废水中吡啶、苯胺和硝基苯的顶空/气相色谱-质谱法（HS/GC-MS）。取10.0mL样品至预加有4.0g碳酸钠的20mL顶空瓶内，再加入总体积为50µL甲醇，在80℃顶空进样器中平衡60min，最后采用GC-MS检测和外标法定量。结果表明，吡啶（苯胺）和硝基苯的线性范围分别介于1.00～30.0µg/L和0.50～15.0µg/L，相关系数均大于0.992，检出限为0.15～0.93µg/L；对实验室空白和纺织产业园区污水处理厂排放的印染废水进行加标回收检测，平均回收率分别为73.6%～105.8%和67.2%～89.9%，相对标准偏差（RSD）分别为5.9%～14.2%（n=8）和2.2%～11.5%（n=6）。采用本方法检测纺织产业园区印染废水中吡啶、苯胺和硝基苯的浓度分别为1.10～1.13µg/L、1.71～5.36µg/L和未检出～0.19µg/L。该方法提出了有利于提高方法灵敏度的措施，例如加入适量的甲醇和碳酸钠，以及提高样品平衡温度，为印染废水中吡啶、苯胺和硝基苯的同时监控提供技术支撑。
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| 关 键 词： | 顶空/气相色谱-质谱法 吡啶 苯胺 硝基苯 印染废水 |
| 收稿时间： | 2023-03-28 |
| 修稿时间： | 2023-06-02 |
Research progress on health effects of aniline |
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| WU Yue，LAI Yongzhong，LU Guoyong，et al. Simultaneous Determination of Pyridine, Aniline and Nitrobenzene in Printing and Dyeing Wastewater by Headspace Gas Chromatography-Mass Spectrometry[J]. Rock and Mineral Analysis，2023，42（4）：781−792. DOI: 10.15898/j.ykcs.202303280041 |
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| Authors: | WU Yue LAI Yongzhong LU Guoyong LIN Xiaosheng LIANG Shusheng XU Wenshuai |
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| Affiliation: | 1.Department of Ecological Construction, Shantou Polytechnic, Shantou 515041, China;2.Institute of Marine Science, Shantou University, Shantou 515063, China;3.Guangdong Provincial Key Laboratory of Marine Biotechnology, Shantou University, Shantou 515063, China;4.Shantou Ecological and Environment Monitoring Center Station of Guangdong Province, Shantou 515041, China |
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| Abstract: | BACKGROUNDPyridine, aniline, and nitrobenzene are important chemical raw materials with low boiling point and strong polarity. They are highly susceptible to enter environmental water and cause pollution. Printing and dyeing wastewater with a complex matrix contains various carcinogenic nitrogen-containing organic pollutants, such as pyridine, aniline, and nitrobenzene. Printing and dyeing wastewater discharging into the environment is harmful to human health through the food chain. The simultaneous detection method of pyridine, aniline, and nitrobenzene in environmental water is necessary.OBJECTIVESTo establish an analytical method based on headspace gas chromatography-mass spectrometry for the simultaneous determination of pyridine, aniline, and nitrobenzene in water.METHODSThe contents of pyridine, aniline, and nitrobenzene in the effluents from the wastewater treatment plants in the textile industry parks were detected and quantified by the external standard method with headspace gas chromatography-mass spectrometry method. Finally, the experiment conditions were optimized.RESULTSThe results showed that the linear ranges of pyridine and aniline were between 1.00µg/L and 30.0µg/L, and nitrobenzene was in the mass concentration range of 0.50-15.0µg/L, with the correlation coefficient above 0.992. The limits of detection were 0.15-0.93µg/L. The concentrations of pyridine, aniline and nitrobenzene in the effluents of the wastewater treatment plant in the textile industry parks were detected from 1.10µg/L to 1.13µg/L, from 1.71µg/L to 5.36µg/L and from ND to 0.19µg/L, respectively. The average recoveries of samples from laboratory blanks and wastewater treatment plant effluents at three levels of addition were 73.6% to 105.8% and 67.2% to 89.9%, respectively, with relative standard deviations of 5.9% to 14.2% (n=8) and 2.2% to 11.5% (n=6). The process and conditions of headspace are summarized as follows: 10.0mL of sample was placed into a 20mL headspace bottle containing 4.0g Na2CO3, and then 50µL methanol was added; the equilibration time of the headspace sampler was 60 min, and the equilibrium temperature was 80℃.CONCLUSIONSSome measures are conductive to improving the sensitivity of the method, such as addition of methanol and sodium carbonate, and increasing the sample equilibrium temperature, in order to reduce the dissolved concentrations of the targets in the water and improve the precipitation effect of the targets. This method improves the detection efficiency, and is of significance for the simultaneous monitoring of pyridine, aniline, and nitrobenzene in printing and dyeing wastewater. |
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| Keywords: | headspace gas chromatography-mass spectrometry pyridine aniline nitrobenzene printing and dyeing wastewater |
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