摘要:
采用纤维膜保护的三相液相微萃取(HF-LLLME)技术,对偶氮染料在人工汗液和光辐照协同作用下降解产生致癌芳香胺的分析方法进行了研究.选用苯胺、邻甲苯胺、对氯苯胺和对硝基苯胺的汗液混合溶液进行模拟样品预处理,以正辛醇为有机萃取相,在供体相pH值为9,NaCl浓度为200 g·L-1,接收相为pH=1的盐酸水溶液,萃取时间为60 min的萃取条件下,4种芳香胺的富集倍数在410—1250倍之间.将接收相直接进行毛细管电泳(CE)测定,样品相中4种芳香胺质量浓度在10—100 μg·L-1范围内,其质量浓度与电泳峰面积之间呈良好的线性关系.在此基础上,分别对两种偶氮染料,活性艳红X-3B和分散红S-R在人工汗液环境下光致降解实际过程中产生的芳香胺进行三相液相微萃取和毛细管电泳(HF-LLLME-CE)测定,其加标回收率分别在90.8%—93.0%之间和97.8%—115.0%之间.实验结果表明,纤维膜三相液相微萃取对汗液基质中芳香胺具有很好的富集效果,与毛细管电泳联用实现了复杂基质中芳香胺的测定.
Abstract:
A simple and rapid three phase (liquid-liquid-liquid) micro extraction method(LLLME) using hollow fibre membrane (HF) was employed before capillary electrophoresis (CE) analysis. For the pretreatment of aromatic amines which are generated from azo dyes in perspiration matrix by photo-catalysis, aniline, o-toluidine, 4-chloroaniline, 4-nitroaniline as model compounds were extracted from simulative solution of perspiration. Under the optimized conditions, using octanol as organic phase, pH 9 and 200 g·L-1 ion concentration in the donor phase, pH 1 for the receiving phase and 60 min extraction time, enrichment factors ranging from 410 to 1250 were obtained for the four aromatic amines.The receiving phase was analyzed by CE directly. The absorption of aromatic amines had good linear relation with the concentration of aromatic amines in the range of 10—100 μg·L-1 at the given CE condition. The real sample, aromatic amines generated from brilliant X-3B and disperse red S-R in perspiration by photo catalysis, were also successfully detected. The recoveries of aromatic amines generated from brilliant X-3B and disperse red S-R were 90.8%—93.0% and 97.8%—115.0% separately. This HF-LLLME method demostrates good separation and enrichment of aromatic amines in perspiration matrix, HF-LLLME in conjunction with CE can quantitatively determine of aromatic amines in complex matrix.
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