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
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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(NH_4)_2SO_4.After centrifuging for 5 min,50μL of the upper organic phase was taken and evaporated to dryness by N_2-blowing.The residue was dissolved with 100μL of CH_3CN-H_2O(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%.
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(NH_4)_2SO_4.After centrifuging for 5 min,50μL of the upper organic phase was taken and evaporated to dryness by N_2-blowing.The residue was dissolved with 100μL of CH_3CN-H_2O(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%.
引文
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[2]AKSU Z,TEZER S.Biosorption of reactive dyes on the green alga Chlorella vulgaris[J].Process Biochemistry,2005,40(3/4):1347-1361.
[3]NCIBI M C,MAHJOUB B,SEFFEN M.Kinetic and equilibrium studies of methylene blue biosorption by Posidonia oceanica,(L.)fibres[J].Journal of Hazardous Materials,2007,139(2):280-285.
[4]CHARUMATHI D,DAS N.Packed bed column studies for the removal of synthetic dyes from textile wastewater using immobilised dead C.tropicalis[J].Desalination,2012,285:22-30.
[5]ROBINSON T,MCMULLAN G,MARCHANT R,et al.Remediation of dyes in textile effluent:A critical review on current treatment technologies with a proposed alternative[J].Bioresource Technology,2001,77(3):247-255.
[6]陈波,徐明敏,赵永纲,等.分散固相萃取-超快速液相色谱-二极管阵列法同时测定环境水中12种致敏性分散染料[J].中国卫生检验杂志,2016,26(19):2747-2750.
[7]王建平.纺织品致敏性分散染料检测方法的德国标准草案[J].印染,2004,30(8):31-34.
[8]秦嘉恺,张丽君,张占恩.基质固相分散萃取-超高效液相色谱-串联质谱法测定污泥中的分散染料[J].现代化工,2016,36(2):172-175.
[9]牛增元,罗忻,叶曦雯,等.高效液相色谱-线性离子阱/静电场轨道阱质谱快速筛查确证生态纺织品中22种致敏性分散染料[J].色谱,2015,33(10):1104-1109.
[10]CLUDIO A F,FERREIRA A M,SHAHRIARI S,et al.Critical assessment of the formation of ionic-liquid-based aqueous two-phase systems in acidic media[J].Journal of Physical Chemistry B,2011,115(38):11145-11153.
[11]LIU Y,HAN J,WANG Y,et al.Selective separation of flavones and sugars from honeysuckle by alcohol/salt aqueous two-phase system and optimization of extraction process[J].Separation&Purification Technology,2013,118(6):776-783.
[12]刘丽丽,程利明,车红霞,等.双水相萃取技术提取牛乳过氧化物酶[J].中国食品学报,2016,16(10):93-98.
[13]HAN J,WANG Y,YU C L,et al.Extraction and determination of chloramphenicol in feed water,milk,and honey samples using an ionic liquid/sodium citrate aqueous two-phase system coupled with highperformance liquid chromatography[J].Analytical&Bioanalytical Chemistry,2011,399(3):1295-1304.
[14]FERREIRA A M,COUTINHO J A P,FER-NANDES A M,et al.Complete removal of textile dyes from aqueous media using ionic-liquid-based aqueous two-phase systems[J].Separation&Purification Technology,2014,128(325):58-66.
[15]陈荣圻.分散染料60年发展概述(待续)[J].染整技术,2016,38(8):31-35.
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