液相色谱-串联质谱法测定印染废水中的21种禁用染料残留  

Determination of 21 Forbidden Dye Residues in Printing and Dyeing Wastewater by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：胡贝贞 陈勤伟 赵佳胤 陈瑶 董文洪 宋伟华 韩超 HU Beizhen;CHEN Qinwei;ZHAO Jiayin;CHEN Yao;DONG Wenhong;SONG Weihua;HAN Chao(Comprehensive Technical Service Center of Shaoxing Customs,Shaoxing 312000;Nanjing Customs Industrial Products Testing Center,Wuxi 214101;Comprehensive Technical Service Center of Wenzhou Customs,Wenzhou,325027;Key Laboratory of Pollution Exposure and Health Intervention of Zhejiang Province,College of Biology and Environmental Engineering,College of Biology and Environment Engineering,Zhejiang Shuren University,Hangzhou 310015)

机构地区：[1]绍兴海关综合技术服务中心,浙江绍兴312000 [2]南京海关纺织工业产品检测中心,江苏无锡214101 [3]温州海关综合技术服务中心,浙江温州325027 [4]浙江省污染暴露与健康干预重点实验室,浙江树人学院,生物与环境工程学院,浙江杭州310015

出　　处：《分析科学学报》2024年第4期427-434,共8页Journal of Analytical Science

基　　金：浙江省基础公益研究计划项目(LGF18B050001)资助。

摘　　要：建立了印染废水中包括中性染料、碱性染料、酸性染料和直接染料4类共21种染料残留量的液相色谱-串联四极杆质谱联用检测方法。采用基于苯乙烯基-二乙烯基苯为基体并键合N-吡咯烷酮亲水基团的HLB小柱和弱阳离子交换WCX小柱串联富集水样中的染料并实现一步式净化,采用T 3色谱柱分离,串联四极杆质谱在电喷雾电离正、负离子同时扫描模式下,多反应监测模式(MRM)测定。重点研究并优化了质谱条件、液相色谱分离条件和样品净化条件。结果表明,21种染料在10~1000μg/L浓度范围内呈良好的线性,相关系数(R^(2))大于0.9990,方法定量限为1.0μg/L,加标回收率在75.6%~105.0%,相对标准偏差为4.25%~10.34%。该方法简便、快速,抗干扰能力强,适用于基质复杂的印染废水中21种染料的日常定性和定量分析。A liquid chromatography-tandem mass spectrometry method for the determination of 21 forbidden dyes including neutral dyes,alkaline dyes,acidic dyes,and direct dyes in printing and dyeing wastewater was established.A hydrophobic polystyrene-divinylbenzene resin hydrophilic lipophilic balance HLB cartridge and a weak cation exchange WCX cartridge were concatenated to enrich the 21 dyes in water samples,the samples were puried simultaneously.Separation was carried out on a T 3 column and determination was carried out using tandem quadrupole mass spectrometry by simultaneous scanning of positive and negative electrospray ionization in multiple reaction monitoring(MRM)mode.The research focused on the optimization of the chromatographic and mass spectrometric conditions and sample purification.Results indicated that the calibration curves for the 21 dyes were linear in the range of 10-1000μg/L,with correlation coefficients no less than 0.9990,the limit of quantification was 1.0μg/L,the recoveries were 75.6%-105.0%with the relative standard deviations of 4.25%-10.34%.The proposed method is accurate,sensitive and has strong anti-interference ability,which is suitable for confirmation and quantitative analysis of the 21 dyes in printing and dyeing wastewaters with complex matrix.

关 键 词：液相色谱-串联质谱 印染废水 禁用染料 残留 

分 类 号：O657.63[理学—分析化学]