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《化学分析计量》 2021年第02期
DOI:10.3969/j.issn.1008-6145.2021.02.006
液液萃取-气相色谱-质谱法测定水中19 种苯胺类化合物
李婧,高翔宇,高文旭,康文贵,张利
西安西北有色地质研究院有限公司,西安 710054 
Determination of 19 aniline compounds in water by liquid-liquid extraction-gas chromatography-mass spectrometry
Li Jing, Gao Xiangyu, Gao Wenxu, Kang Wengui, Zhang Li
Xi'an Northwest Geological Institute for Nonferrous Metals Co., LTD., Xi'an 710054, China 
摘要:建立了液液萃取-气相色谱-质谱法测定水中19 种苯胺类化合物的方法。对液液萃取方法、样品pH、浓缩条件、色谱条件进行了优化,探讨了光氧化降解对苯胺类化合物回收率的影响,在避光条件下,以二氯甲烷为萃取剂,所得提取液在水温为30 ℃、氮气流量为4.0 mL/min 的条件下浓缩后供气相色谱-质谱分析测定。19 种苯胺类化合物的质量浓度在0.2~5.0 mg/L 范围内与色谱峰面积线性关系良好,相关系数R2 大于0.995,检出限为0.013~0.051 μg/L 。实际样品平均加标回收率为80.44%~98.79%,相对标准偏差为4.20%~9.41%(n=6)。该方法前处理简便,结果准确,满足水中多种苯胺类化合物的同时测定。 
Abstract:A method for the determination of 19 aniline compounds in water by liquid-liquid extraction-gas chromatography-mass spectrometry was established. The liquid-liquid extraction method, pH, concentration conditions and chromatographic conditions were optimized, the effects of photo oxidative degradation on the recovery of aniline compounds were discussed. Under the condition of avoiding light, dichloromethane was used as extraction agent, and the extraction solution was concentrated at water temperature of 30 ℃ and nitrogen flow rate of 4.0 mL/min, and then analyzed by gas chromatography-mass spectrometry. The linear range of 19 aniline compounds was 0.2-5.0 mg/L. the correlation coefficient R2 was greater than 0.995, and the detection limit was 0.013-0.051 μg/L. The average recoveries were 80.44% -98.79%, and the relative standard deviations were 4.20%-9.41% (n=6). The method is simple, accurate and suitable for the simultaneous determination of aniline compounds in water. 
关键词:苯胺类化合物;液液萃取;气相色谱-质谱法;光氧化降解;水 
Keywords:aniline compounds; liquid-liquid extraction; gas chromatography-mass; photooxidation degeneration; water 
本文引用格式:
李婧,高翔宇,高文旭,等. 液液萃取- 气相色谱- 质谱法测定水中19 种苯胺类化合物[J]. 化学分析计量,2021,30(2):25.
Li Jing,Gao Xiangyu,Gao Wenxu,et al. Determination of 19 aniline compounds in water by liquid-liquid extraction-gas chromatography-mass spectrometry[J]. Chemical Analysis and Meterage,2021,30(2):25. 

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