高效液相色谱-质谱法测定废水中芳香胺类化合物  

Determination of Aromatic Amines in Wastewater Samples by High Performance Liquid Chromatography/Mass Spectrometry

作　　者：黄丽芳[1] 李来生[1] 刘超[1] 

机构地区：[1]南昌大学分析测试中心,南昌330047

出　　处：《分析科学学报》2008年第3期265-269,共5页Journal of Analytical Science

基　　金：江西省教育厅基金(JJ2007-18)

摘　　要：本文建立了一种高效液相色谱-质谱联用方法，用于测定废水中联苯胺、苯胺、对甲苯胺、对硝基苯胺、甲萘胺等芳香胺类化合物的含量。色谱柱为Kromasil C18柱（250×4．6mm i．d．，5μm），以甲醇-5mmol／L甲酸铵缓冲溶液（PH=3．0）为流动相，流速为1．0mL／min，采用梯度洗脱，分流选样。质谱采用电啧雾电离源正离子模式，以各种化合物的选择离子[M＋H]^＋监测模式进行定量分析。实验发现，联苯胺、苯胺、对甲苯胺、对硝基苯胺、甲萘胺有良好的线性关系，它们的线性范围分别为：7．03～281．30μg／L、10．65～213．10μg／L、11．91～238．20μg／L、12．39～247．90μg／L和14．55-291．10μg／L。回收率为92．7％～101．4％。方法检出限为1．7～3．2μg／L。该分析方法灵敏度高、前处理简便、所测浓度范围宽，适用于废水中芳香胺环境污染物的快速测定。A new method for the determination of aromatic amines, including benzidine, aniline, p-toluidine, p-nitroaniline, and α-naphthylamme, in wastewater was developed by high performance liquid chromatography/mass spectrometry. The chromatographic separation was carried on a Kromasil C18 column by using methanol-5 mmol/L ammonium formate buffer （pH=3.0） as mobile phase at a flow rate of 1 mL/min with a gradient elution mode and split sampling. The mass spectrometric quantitative analysis based on selective ionic measurement [M＋H]^＋ by electro-spray ionization in positive mode. The calibration curves for the above aromatic amines were linear within the range of 7.03-281.30μg/ L,10.65-213. 10μg/L, 11. 91-238. 20μg/L ,12. 39-247. 90μg/L and 14.55-291. 10 μg/L, respectively. The average recoveries were 92.7%-101.4% for the spiked samples. The detection limits （S/N=2） varied from 1.7 μg/L to 3.2μg/L. The results show that the method has high sensitivity, simple pretreatment and wide linear range. It can be used as a fast and sensitive analysis method for the above aromatic amines in wastewater samples.

关 键 词：高效液相色谱-质谱法 芳香胺类化合物 环境污染物 废水 

分 类 号：O657.63[理学—分析化学]