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  

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

作　　者：王绍俊[1] 王超[2] 石庭山 陈烨[2] 吕怡兵[2] 周益民[1] 

机构地区：[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

出　　处：《环境化学》2016年第3期460-465,共6页Environmental Chemistry

基　　金：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0.22μm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—0.4μg·m^(-3)(采样体积以10 L计),在0.5、1.0、2.0μg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、200μg·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.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 of1 m L methanol with 1% ammonia was used to desorb toluidines isomers and p-chloroaniline in20 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% and95%—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.

关 键 词：甲基苯胺 氯代苯胺 超高效液相色谱法 同分异构体 空气 荧光检测 

分 类 号：X831[环境科学与工程—环境工程]