正丙醇/硫酸铵双水相萃取-高效液相色谱-串联质谱法测定印染废水中的7种分散染料的含量  

HPLC-MS/MS Determination of 7 Disperse Dyes in Printing and Dyeing Wastewater with Separation by Bi-Aqueous Phase Extraction Using n-Propanol and Ammonium Sulfate as Extraction System

作　　者：叶紫宇 高仕谦[1] 顾海东[2] 张占恩[1,2] YE Ziyu;GAO Shiqian;GU Haidong;ZHANG Zhan'en(School of Environmental Science and Engineering,Suzhou University of Science and Technology,.,Suzhou 215009,China;Jiangsu Key Laboratory of Environmental Science and Engineering, Suzhou University of Science and Technology,Suzhou 215009,China)

机构地区：[1]苏州科技大学环境科学与工程学院,苏州215000 [2]苏州科技大学江苏省环境科学与工程重点实验室,苏州215000

出　　处：《理化检验（化学分册）》2019年第1期46-50,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江苏省高校自然科学研究重大项目(15KJA610003);苏州科技大学青年基金项目(341511201);苏州科技大学人才引进科研项目(331511207)

摘　　要：取含分散染料的废水样品5.00mL,用由正丙醇200μL和硫酸铵2.75g组成的萃取剂体系进行双水相超声提取21min。离心5min后,分取上层有机相50μL,吹氮蒸干。用CH_3CN-H_2O(7+3)混合液100μL溶解残渣。此溶液引入作为固定相的Zorbax Eclipse XDB-CN色谱柱,并用0.1%(体积分数)甲酸溶液和乙腈(3+7)混合液为流动相进行梯度洗脱。用MS/MS测定其中7种分散染料的含量。质谱分析中采用电喷雾离子源及多反应监测模式。所测定的7种分散染料的质量浓度在一定范围内与其峰面积呈线性关系,7种染料的检出限(3S/N)在3.3～57ng·L^(-1)之间。以印染废水样品为基质,按标准加入法进行回收试验,测得回收率在80.0%～116%之间,测定值的相对标准偏差(n=5)在1.2%～10%之间。5.00 mL of the wastewater sample were taken and extracted ultrasonically for 21 min by biaqueous phase extraction with extractant system composed of 200μL of n-propanol and 2.75 g of(NH4)2SO4.After centrifuging for 5 min,50μL of the upper organic phase was taken and evaporated to dryness by N2-blowing.The residue was dissolved with 100μL of CH3CN-H2O(7+3)mixture,and the solution was then separated by HPLC using Zorbax Eclipse XDB-CN column as stationary phase and a mixture of 0.1%(φ)formic acid solution and acetonitrile(3+7)was used as mobile phase for elution.MS/MS with ESI,MRM was adopted for determination of the 7 disperse dyes.As shown by the results,linear relationships between values of peak area and mass concentration of the 7 disperse dyes were found in definite ranges,with detection limits(3 S/N)in the range of 3.3-57 ng·L^-1.Test for recovery by standard addition method was made using wastewater from printing and dyeing process as matrix,giving results in the range of 80.0%-116%,and RSDs(n=5)ranged from 1.2% to10%.

关 键 词：双水相萃取 高效液相色谱-串联质谱法 分散染料 印染废水 

分 类 号：O657.63[理学—分析化学]