分散液液微萃取-GC-MS/MS测定纺织废水中痕量4-氨基偶氮苯  

Determination of trace 4-aminoazobenzene in textile wastewater by dispersive liquid-liquid microextraction-GC-MS/MS

作　　者：丁友超 曹丽华 李姗 钱凯 王晓琼 周佳 汤娟 DING Youchao;CAO Lihua;LI Shan;QIAN Kai;WANG Xiaoqiong;ZHOU Jia;TANG Juan(Nanjing Customs Industrial Products Testing Center,Nanjing 210019,China;China National Accreditation Service for Conformity Assessment,Beijing 100062,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,江苏南京210019 [2]中国合格评定国家认可委员会,北京100062 [3]南京金检检验有限公司,江苏南京210019

出　　处：《印染》2024年第4期61-65,共5页China Dyeing and Finishing

基　　金：海关总署科研项目(2022HK063)。

摘　　要：建立了分散液液微萃取-气相色谱串联质谱法测定纺织废水中偶氮染料释放的痕量4-氨基偶氮苯的新方法。在碱性条件下,用连二亚硫酸钠还原纺织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4-氨基偶氮苯进行分散液液微萃取,之后采用气相色谱-串联质谱法测定,内标法定量。方法优化了废水试样制备、还原反应条件、分散液液微萃取影响条件以及色谱和质谱条件等。优化的检测方法呈现良好的线性关系,线性范围为0.1~10.0μg/L;方法检出限为0.03μg/L,定量限为0.1μg/L;加标回收率为88.0%~97.0%。该方法具有操作简便、检出限低的优势,能够满足纺织废水中痕量4-氨基偶氮苯的检测。A new method for the determination of trace 4-aminoazobenzene released from azo dyes in textile wastewater by dispersive liquid-liquid microextraction coupled with gas chromatography-tandem mass spectrometry(GC-MS/MS)is established.Azo dyes in the wastewater sample are reduced with sodium dithionite under alkaline conditions,then the 4-aminoazobenzene generated by decomposition is microextracted by dispersive liquid-liquid microextraction with acetonitrile as a dispersant and chloroform as an extractant,and then determined by gas chromatography-tandem mass spectrometry,and quantified by internal standard method.The wastewater sample preparation,reduction reaction conditions,dispersive liquid-liquid microextraction conditions,chromatography and mass spectrometry conditions are optimized.The optimized detection method shows a good linear relationship,with a linear range of 0.1-10.0μg/L,a limit of detection of 0.03μg/L,a limit of quantification of 0.1μg/L,and a recovery rate of 88.0%-97.0%.The method has the advantages of simple operation and low detection limit which can meet the detection of trace 4-aminoazobenzene in textile wastewater.

关 键 词：测试 分散液液微萃取 气相色谱串联质谱 纺织废水 4-氨基偶氮苯 

分 类 号：TS197[轻工技术与工程—纺织化学与染整工程]