分散液液微萃取-气相色谱串联质谱法测定纺织废水中禁用偶氮染料释放的芳香胺  

Determination of aromatic amines released from banned azo dyes in textile waste-water by dispersive liquid-liquid microextraction-gas chromatography-tandem mass spectrometry

作　　者：曹丽华 丁友超 马立利 钱凯 王香香 周佳 汤娟 CAO Lihua;DING Youchao;MA Lili;QIAN Kai;WANG Xiangxiang;ZHOU Jia;TANG Juan(Nanjing Customs Industrial Products Testing Center,Nanjing 210019,China;Institute of Analysis and Testing,Beijing Academy of Science and Technology(Beijing Center for Physical and Chemical Analysis),Beijing 100089,China;Nanjing Jinjian Inspection Co.,Ltd.,Nanjing 210019,China)

机构地区：[1]南京海关工业产品检测中心,南京210019 [2]北京市科学技术研究院分析测试研究所(北京市理化分析测试中心),北京100089 [3]南京金检检验有限公司,南京210019

出　　处：《分析试验室》2025年第4期487-493,共7页Chinese Journal of Analysis Laboratory

基　　金：海关总署科研项目(2022HK063)资助。

摘　　要：建立了分散液液微萃取-气相色谱串联质谱法(GC-MS/MS)测定纺织废水中禁用偶氮染料释放的芳香胺的新方法。在pH 13条件下,首先用连二亚硫酸钠还原废水试样中的偶氮染料,再以乙腈为分散剂、三氯甲烷为萃取剂,对分解生成的芳香胺进行液液微萃取(DLLME),并采用GC-MS/MS法测定,内标法定量。在优化的实验条件下,各芳香胺均呈良好的线性关系,其中19种芳香胺的线性范围为0.1~10μg/L,2,4-二氨基甲苯的线性范围为5~500μg/L,2,4-二氨基苯甲醚的线性范围为10~1000μg/L。19种芳香胺的方法检出限可达到0.03μg/L,2,4-二氨基甲苯的方法检出限为1.5μg/L,2,4-二氨基苯甲醚的方法检出限为3.0μg/L。各芳香胺在阴性纺织废水样品中的加标回收率为73.0%~102.7%,相对标准偏差(RSDs)为2.9%~8.1%。该方法能够满足纺织废水中禁用偶氮染料所释放的痕量芳香胺的检测。A new method for the determination of aromatic amines released from azo dyes in textile wastewater was established by using dispersive liquid-liquid microextraction(DLLME)coupled with gas chromatography-tandem mass spectrometry(GC-MS/MS).Under pH 13,the azo dyes in the wastewater sample were firstly reduced with sodium dithionite,then DLLME was performed for extraction of aromatic amines with acetonitrile as a dispersant and trichloromethane as an extractant,and finally GC-MS/MS was applied for quantification of aromatic amines with internal standard quantification.Under optimum experimental conditions,all aromatic amines showed good linear relationships,the linear ranges were 0.1-10μg/L for 19 aromatic amines,5-500μg/L for 2,4-diaminotoluene,and 10-1000μg/L for 2,4-diaminoanisole.The detection limits were 0.03μg/L for 19 aromatic amines,1.5μg/L for 2,4-diaminotoluene,and 3.0μg/L for 2,4-diaminoanisole.The spiking experiments in negative textile wastewater samples showed that the recoveries of aromatic amines were 73.0%-102.7%,and the relative standard deviations(RSDs)were 2.9%-8.1%.The method can meet the detection of trace aromatic amines released from banned azo dyes in textile wastewater.

关 键 词：分散液液微萃取(DLLME) 气相色谱串联质谱(GC-MS/MS) 纺织废水 禁用偶氮染料 芳香胺 

分 类 号：TS197[轻工技术与工程—纺织化学与染整工程]