基于超高压液相色谱荧光检测法的空气中苯胺类化合物测定  

Determination of aniline derivatives in the air using ultrahigh-pressure liquid chromatography through fluorescent detection

作　　者：王超[1] 王绍俊[2] 陈烨[1] 吕怡兵[1] 滕恩江[1] 

机构地区：[1]中国环境监测总站,北京100012 [2]新疆生产建设兵团环境监测中心站,乌鲁木齐830002

出　　处：《安全与环境学报》2016年第2期343-346,共4页Journal of Safety and Environment

基　　金：国家高技术研究发展计划"863计划"项目(2013AA06A308)

摘　　要：建立了硅胶吸附管采样-超高压液相色谱荧光检测法测定空气中苯胺、联苯胺和N,N-二甲基苯胺的方法。采用硅胶填料吸附管采集空气中3种苯胺类化合物（ADs）。使用含1%氨水的甲醇对硅胶填料解吸20 min。解吸溶液经0.22μm尼龙滤膜过滤后,采用超高压液相色谱荧光检测法分析,3种ADs的荧光激发/发射波长分别为232 nm/329 nm、292 nm/383 nm和243 nm/383 nm。3种ADs在5min内实现基线分离,在0.05～2.0 mg/L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0.08～0.4μg/m3（采样体积以10 L计）,在0.05μg、0.2μg和2.0μg加标水平（相当于10 L空气中ADs质量浓度为5μg/m3、20μg/m3和200μg/m3）下,回收率分别为100%～110%、96%～110%和87%～102%,相对标准偏差分别为0.8%～2.0%、0.3%～1.3%和2.3%～2.9%。研究表明,该方法适用于空气中3种ADs的同时测定。In this paper,the results of determination of aniline derivatives（ ADs） in the air were shown by using ultrahigh- pressure liquid chromatography through fluorescent detection. The samples were collected using a silica gel tube with 6 mm ID,120 mm length,150 mg /75 mg,and 60- 80 mesh size（ 180- 250 μm）. A method was established for simultaneous analysis of the aniline,benzidine and N,N-dimethylaniline in the air through the optimization of conditions for chromatographic analysis,solution desorption and sample preservation. In accordance with the method,three ADs were dissolved by using 1 m L methanol with 1% ammonia for 20 min in the room temperature,and then filtered and analyzed the solution of desorption through 0. 22 μm microfiltration membrane via the ultrahighpressure liquid chromatography with the fluorescence detection. The ADs were separated and prepared on a BEH C18column（ 2. 1 mm ×50 mm,1. 7 μm） in the gradient elution through a methanol-5mmol / L ammonium acetate at the flowing rate of 0. 4 m L / min. When the three ADs were separated via the baseline for 5 min,the fluorescence detection condition（ λex/ λem） for the three ADs literally were prepared at 232 nm /329 nm,292 nm /383 nm and 243 nm /383 nm,respectively. The calibration curves for the ADs were made linear in a range of 0. 05- 2. 0 mg / L with the correlation coefficient of more than 0. 999. With the method limits of detection（ S / N = 3） being set up at 0. 08- 0. 4 μg / m3 with a sampling volume of 10 L,the three ADs were added as spiked with the levels of 0. 05 μg,0. 2 μg and 2.0 μg（ 5 μg / m3,20 μg/m3 and 200 μg / m3 in the air volume of 10L） by a rate of 100%- 110%,96%- 110% and 87%- 102%,with the relative standard deviation being 0. 8%- 2. 0%,0. 3%- 1.3% and 2. 3%- 2. 9%,respectively. Besides,we have promoted the penetrating capacity of the above-mentioned silica gel tube over0. 3 mg and 0. 4 mg for the aniline in N,N-dimethylaniline. Moreover,we have also successfully prolonged the storage time for th

关 键 词：环境学 苯胺类化合物 超高压液相色谱 硅胶管吸附 空气 荧光检测 

分 类 号：X831[环境科学与工程—环境工程]