液液萃取-分散液液微萃取-气相色谱-质谱联用测定纺织废水中痕量禁用偶氮染料

引用本文: 叶曦雯, 何静, 李莹, 牛增元, 张甜甜, 罗忻, 邹立, 连素梅. 液液萃取-分散液液微萃取-气相色谱-质谱联用测定纺织废水中痕量禁用偶氮染料[J]. 色谱, 2020, 38(2): 255-263. doi: 10.3724/SP.J.1123.2019.07012 shu

Citation: YE Xiwen, HE Jing, LI Ying, NIU Zengyuan, ZHANG Tiantian, LUO Xin, ZOU Li, LIAN Sumei. Determination of trace azo dyes in textile wastewater by liquid-liquid extraction and dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(2): 255-263. doi: 10.3724/SP.J.1123.2019.07012 shu

液液萃取-分散液液微萃取-气相色谱-质谱联用测定纺织废水中痕量禁用偶氮染料

叶曦雯 ^1, ,
何静 ^1, ,
李莹 ^1, ,
牛增元 ^1, ,
张甜甜 ^1, ,
罗忻 ^1, ,
邹立 ^2, ,
连素梅 ^3,

1.
青岛海关技术中心, 山东青岛 266003;
2.
中国海洋大学环境科学与工程学院, 山东青岛 266100;
3.
石家庄海关技术中心, 河北石家庄 050051
基金项目:
国家重点研发计划（NQI 2016YFF0203702）；海关总署科研项目（2019HK070）.

摘要: 建立了液液萃取-分散液液微萃取-气相色谱-质谱联用技术测定纺织废水中痕量偶氮染料的方法。废水中的偶氮染料在碱性条件下经连二亚硫酸钠还原成芳香胺后，先用叔丁基甲醚液液萃取、盐酸反萃进行预浓缩及净化；再以乙腈-氯苯体系进行分散液液微萃取，气相色谱-质谱测定。对前处理条件进行了优化，考察了酸碱度及盐效应对芳香胺萃取效率的影响，结果表明：液液萃取过程中加入30 g NaCl，分散液液微萃取过程中加入1 mL 5 mol/L的NaOH调节体系至碱性才能达到较好的萃取效率。在优化的实验条件下，21种目标物均呈现良好的线性关系，其中13种芳香胺的线性范围为0.05~10 μg/L，7种芳香胺的线性范围为0.05~5 μg/L，2，4-二氨基苯甲醚的线性范围为20~100 μg/L，相关系数为0.996~0.999。20种芳香胺的检出限可达0.05 μg/L，2，4-二氨基苯甲醚检出限为20 μg/L。印染、机织、印花等实际废水加标试验表明，方法的回收率为75.6%~115.1%。该方法富集倍数高，检出限低，适用于纺织废水中痕量禁用偶氮染料的检测。

关键词:

English

Determination of trace azo dyes in textile wastewater by liquid-liquid extraction and dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry

1.
Technology Center of Qingdao Customs, Qingdao 266003, China;
2.
College of Environmental Science and Engineering, Ocean University of China, Qingdao 266100, China;
3.
Technology Center of Shijiazhuang Customs, Shijiazhuang 050051, China
Received Date: 08 July 2019
Fund Project:
Key Project of National and Development Plan (No. NQI 2016YFF0203702)

Abstract: An efficient method based on liquid-liquid extraction and dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry was developed for the determination of trace azo dyes in textile wastewater. The azo dyes were reduced to aromatic amines by sodium dithionite under alkaline conditions. The main pretreatment conditions that affected the extraction efficiency were optimized. Under the optimized experimental conditions, the linear ranges of this method were as follows:0.05-10 μg/L for 13 aromatic amines; 0.05-5 μg/L for 7 aromatic amines; and 20-100 μg/L for 2,4-diaminoanisole. The correlation coefficients were in the range of 0.996-0.999. The limits of detection reached 0.05 μg/L for all the 20 aromatic amines, and the detection limit of 2,4-diaminoanisole was 20 μg/L. Actual wastewater-spiked experiments involving printing, dyeing, and weaving showed that the average recoveries of the amines were in the range of 75.6%-115.1%. The developed method has high enrichment multiples and low detection limits, and it is suitable for the detection of trace levels of banned azo dyes in textile wastewater.

Key words:

dispersion liquid-liquid microextraction (DLLME)
/ gas chromatography-mass spectrometry (GC-MS)
/ azo dye
/ aromatic amine
/ textile wastewater

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液液萃取-分散液液微萃取-气相色谱-质谱联用测定纺织废水中痕量禁用偶氮染料

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Determination of trace azo dyes in textile wastewater by liquid-liquid extraction and dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry

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