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

通讯作者: 牛增元, E-mail:zyniuqd@163.com

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 μ g/L，7种芳香胺的线性范围为0.05~5 μ g/L，2，4-二氨基苯甲醚的线性范围为20~100 μ g/L，相关系数为0.996~0.999。20种芳香胺的检出限可达0.05 μ g/L，2，4-二氨基苯甲醚检出限为20 μ g/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

YE Xiwen ^1, ,
HE Jing ^1, ,
LI Ying ^1, ,
NIU Zengyuan ^{1,
,} ,
ZHANG Tiantian ^1, ,
LUO Xin ^1, ,
ZOU Li ^2, ,
LIAN Sumei ^3,

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

Corresponding author: NIU Zengyuan, zyniuqd@163.com

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 μ g/L for 13 aromatic amines; 0.05-5 μ g/L for 7 aromatic amines; and 20-100 μ g/L for 2,4-diaminoanisole. The correlation coefficients were in the range of 0.996-0.999. The limits of detection reached 0.05 μ g/L for all the 20 aromatic amines, and the detection limit of 2,4-diaminoanisole was 20 μ g/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

1. [1] Inoue K, Aikawa S, Fukushima Y. Polym Int, 2018, 67:755
2. [2] Qin X, Xu Y Y, Hu Z, et al. Progress in Textile Technology, 2018(6):16 秦鑫, 徐韵扬, 胡喆, 等. 纺织科技进展, 2018(6):16
3. [3] Muz M, Dann J P, Jager F, et al. Environ Sci Technol, 2017, 51(8):4681
4. [4] Benigni R, Passerini L. Mutat Res, 2002, 511(3):191
5. [5] Bhaskar M, Aruna P, Jeevan R J G, et al. Anal Chim Acta, 2004, 509(1):39
6. [6] China Environmental Monitoring Research Team. Environmental Priority Pollutant. Beijing:China Environmental Science Press, 1989:9 中国环境监测研究课题组. 环境优先污染物. 北京:中国环境科学出版社, 1989:9
7. [7] Li G, Xu Y Y, Chen J. Arid Environmental Monitoring, 2008, 22(2):73 李刚, 许月英, 陈静. 干旱环境监测, 2008, 22(2):73
8. [8] GB 3838-2002
9. [9] GB 8978-1996
10. [10] EN 14362-1:2012
11. [11] EN 14362-3:2012
12. [12] Long C Y, Mai Z B, Yang X F, et al. Food Chem, 2011, 126(3):1324
13. [13] Jin X L, Jiang G B, Huang G L, et al. Chemosphere, 2004, 56(11):1113
14. [14] Wang H M, Jiang P S, Hou X H, et al. Petrochemical, 2012, 41(3):342 王洪明, 江丕森, 侯晓虹, 等. 石油化工, 2012, 41(3):342
15. [15] Mishra S, Singh V, Jain A, et al. The Analyst, 2001, 126(10):1663
16. [16] Jalilian N, Ebrahimzadeh H, Asgharinezhad A A. J Chromatogr A, 2017, 1499:38
17. [17] Fan J, Fan Y C, Zhang S L, et al. Sep Sci Technol, 2011, 46(7):1172
18. [18] Mousa A, Basheer C, Abdulnaser A, et al. Int J Environ Anal Chem, 2015, 95(8):744
19. [19] Lucaire V, Schwartz J J, Delhomme O, et al. Anal BioanalChem, 2018, 410(7):1955
20. [20] Peng J G, Wang D H, Wu C Y. Journal of Instrumental Analysis, 2004, 23(3):18 彭家钢, 王丹华, 吴采樱. 分析测试学报, 2004, 23(3):18
21. [21] Agudelo Mesa L B, Padró J M, Reta M. Food Chem, 2013, 141(3):1694
22. [22] Khalilian F, Rezaee M. Food Anal Method, 2017, 10(4):885
23. [23] Sun J Q, Qiao B, Sun D S. Advanced Materials Research, 2014, 838/841:2582
24. [24] Fan Y C, Hu Z L, Chen M L, et al. Chinese Chem Lett, 2008, 19(8):985
25. [25] Ding M Z, Peng J, Ma S L, et al. Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2018, 54(10):62 丁明珍, 彭璟, 马少玲, 等. 理化检验(化学分册), 2018, 54(10):62
26. [26] Xu H, Tong H. Journal of Instrumental Analysis, 2000, 19(1):76 许泓, 佟晖. 分析测试学报, 2000, 19(1):76
27. [27] Lirio S, Fu C W, Lin J Y, et al. Anal Chim Acta, 2016, 927:55
28. [28] Zhu L Y, Tay C B, Lee H K. J Chromatogr A, 2002, 963(1):231
29. [29] Feng W, Zhu Y, Ouyang G F. Chinese Journal of Analytical Chemistry, 2015, 43(7):957 冯文, 朱莹, 欧阳钢锋. 分析化学, 2015, 43(7):957
30. [30] Deng H M, Yang F, Li Z Y, et al. J Chromatogr A, 2017, 15(7):37
31. [31] Farajzadeh M A, Djozan D, Bakhtiyari R F. Talanta, 2010, 81(4/5):1360
32. [32] Chiang J S, Huang S D. J Chromatogr A, 2008, 1185(1):19
33. [33] Canales R, Guinez M, Bazán C, et al. Talanta, 2017, 174:548
34. [34] Zhu Y L, Zhang W Y, Li L X, et al. Anal Methods, 2014, 6(7):2102
35. [35] Sun Z Q, Ye Y Y, Yu H Q. China Fiber Inspection, 2018(3):101 孙卓群, 叶雅悠, 虞鹤群. 中国纤检, 2018(3):101
36. [36] Vastag G, Apostolov S, Matijevic B, et al. J Chromatogr B, 2018, 1084:141
37. [37] Zhou Q X, Jiang G B, Liu J F, et al. Anal Chim Acta, 2004, 509:55
38. [38] Psillakis E, Kalogerakis N. TrAC-Trends Anal Chem, 2003, 22(9):565
39. [39] Zhang Y, He Y, Li G A, et al. Chinese Journal of Environmental Engineering, 2016, 10(2):509 张雁, 何咏, 李国傲, 等. 环境工程学报, 2016, 10(2):509
40. [40] Lin Z A, Zhang J H, Cui H M, et al. J Chromatogr A, 2010, 1217(26):4507
41. [41] Sarafraz-Yazdi A, Mofazzeli F, Es'haghi Z. Talanta, 2009, 79:472
42. [42] Wen W, Zhang W F, Zhang Y H. Chinese Journal of Chromatography, 2019, 37(5):491 闻威, 张文芬, 张岩皓. 色谱, 2019, 37(5):491
43. [43] Zhu Y, Zhu Y, Wang L L. Chinese Journal of Chromatography, 2012, 30(4):345 诸寅, 朱岩, 王丽丽. 色谱, 2012, 30(4):345
44. [44] Luo J, Huang L F, Hu N N. Chemical Production and Technology, 2014, 21(5):38 罗嘉, 黄兰芳, 胡念念. 化工生产与技术, 2014, 21(5):38
45. [45] Wang C, Gu C K, Ma Q, et al. Journal of Instrumental Analysis, 2019, 38(3):263 王春, 顾传坤, 马强, 等. 分析测试学报, 2019, 38(3):263
46. [46] Ye X W, Peng Y, Niu Z Y, et al. Chinese Journal of Chromatography, 2014, 32(9):1005 叶曦雯, 彭燕, 牛增元, 等. 色谱, 2014, 32(9):1005
47. [47] Zhong X L, Lu J Y, Hu Y Q. China Fiber Inspection, 2015(24):68 钟雪莲, 陆佳英, 胡燕琴. 中国纤检, 2015(24):68
48. [48] Han J, Yang M, Bai Z Z, et al. China Fiber Inspection, 2014(2):73 韩军, 杨萌, 白子竹, 等. 中国纤检, 2014(2):73
49. [49] Yun H, Liu X, Wang J, et al. Chinese Journal of Chromatography, 2013, 31(9):845 云环, 刘鑫, 王静, 等. 色谱, 2013, 31(9):845
50. [50] Miguel del N S, Cristina P S, José L P P, et al. Anal Bioanal Chem, 2012, 404(6/7):2007
51. [51] Wen Y Y, Chen T, Chen Z H, et al. Environmental Chemistry, 2014, 33(4):670 温裕云, 陈婷, 陈志华, 等. 环境化学, 2014, 33(4):670

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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

通讯作者: 牛增元, E-mail:zyniuqd@163.com

English

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

Corresponding author: NIU Zengyuan, zyniuqd@163.com

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

通讯作者: 牛增元, E-mail:zyniuqd@163.com

English

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

Corresponding author: NIU Zengyuan, zyniuqd@163.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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