摘要
采用以离子液体为萃取剂的液相微萃取,对纺织品检测国家标准方法(GB/T 17592—2006)中纺织品样品前处理方法进行了改进,建立了纺织品中源于偶氮染料的芳香胺的提取新方法。比较了直接浸入式微萃取和溶刺棒微萃取模式的萃取效果,确定以溶剂捧微萃取为微萃取模式。并优化了液相微萃取条件:以正辛醇为有机萃取溶剂,离子液体为接收相,给出相pH值为10并添加饱和NaCl溶液,搅拌速率为1000r/min,萃取时间为40min。参照纺织品检测国家标准方法,采用高效液相色谱法对所公布的22种致癌芳香胺进行了定性、定量测定。结果表明,该方法的线性范围宽,相关系数r〉0.9951,检出限(S/N=3)为0.01~2.13μg/L,相对标准偏差小于4.5%(n=8);回收率为82%~94%,8种芳香胺的富集倍数为5.7~270.0。与纺织品检测国家标准方法相比,该方法简单、快速,并显示了较好的富集效果和高的回收率。
A ionic liquid-based liquid phase microextraction method has been developed for the extraction of 22 cancer-causing aromatic amines from the forbidden azo dyes in textiles, which was announced by the national standard method for textiles(GB/T 17592 -2006). The extraction efficiencies of the two models, direct immersion microextraction and solvent bar microextraction was investigated. The solvent bar microextraction were selected as the experimental model of microextraction for its better performance. The influences of extraction parameters were investigated, and the optimum experimental conditions were as follows: organic solvent: n-octanol, acceptor phase: 1-butyl-3-methylimidazolium hexafluorophosphate, pH value of donor phase: 10, stirring rate: 1000 r/min, extraction time: 40 min. Under the optimal conditions, 22 cancer-causing aromatic amines were analyzed by the extraction method combination with high performance liquid chromatography. The resuits showed that the proposed method provided a wide linear range with correlation coefficients more than 0. 995 1. The detection limits(S/N =3) ranged from 0.01 to 2. 13 μg/L, and the recoveries were 82% - 94% with RSDs less than 4.5% ( n = 8 ). The enrichment folds of 22 aromatic amines were in the range of 5.7 - 270. 0. Compared with the national standard method, this method was simple and fast in operation, and also showed high sensitivity and extraction efficiency.
出处
《分析测试学报》
CAS
CSCD
北大核心
2009年第6期671-676,共6页
Journal of Instrumental Analysis
基金
江西省教育厅科研基金资助项目(GJJ08303)
江西省教育厅青年基金资助项目(GJJ09523)
作者简介
张慧(1981-),女,湖南娄底人,硕士研究生
通讯作者:丁健桦,Tel:0794-8258320,E-mail:dingjianh2004@126.com