当前位置: X-MOL 学术J. Chromatogr. A › 论文详情
Our official English website, www.x-mol.net, welcomes your feedback! (Note: you will need to create a separate account there.)
Development of an analytical method for urocanic acid isomers in fish based on reactive extraction cleanup and chaotropic chromatography techniques
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2018-03-14 , DOI: 10.1016/j.chroma.2018.03.023
Jian-Jun Zhong , Ningbo Liao , Mingfeng He , Yunfeng Pu , Donghong Liu

Urocanic acid (UA), existing in trans- or cis-isoform, is of fairly recent interest to food researchers because of its potential public health hazards of scombrotoxicity and immunotoxicity, as well as associating with fish spoilage. This work is among the first efforts to study the analytical chemistry of UA in fish. With 0.6 M perchloric acid UA was extracted, and co-extracted fish matrix components were efficiently removed through a reactive extraction of UA. The optimum conditions for the reactive extraction, which allowed an 80% recovery of UA, were sample pH adjustment to 9, twice extractions with 32% (w/w) di (2-ethylhexyl) phosphate in hexanol, and a back-extraction with 0.1 M hydrochloric acid at 1:1 phase ratio. A chaotropic hexafluorophosphate salt was added to acidic water-acetonitrile mobile phases to improve the reversed-phase chromatography of UA, which otherwise was poorly retained. Optimum separation conditions were obtained for fish samples and enabled a fast (10 min), convenient-to-use chromatography that clearly outperforms cumbersome legacy ion-pair chromatography. Intended for routine use in our laboratory, the proposed method passed an in-house validation test for linearity, matrix effect (on reactive extraction), accuracy, precision, and detectability.



中文翻译:

基于反应萃取净化和离液色谱技术的鱼类尿酸异构体分析方法的开发

尿酸(UA),以反式顺式形式存在-亚型对食品研究人员来说是最近才引起关注的,因为它具有潜在的公共卫生危害,包括中毒和免疫毒性,以及与鱼类变质相关的危害。这项工作是研究鱼类中UA的分析化学的首批工作之一。用0.6 M高氯酸提取UA,并通过反应性UA高效去除共提取的鱼基质成分。允许UA回收率达到80%的反应性萃取的最佳条件是将样品的pH值调节至9,两次用32%(w / w)的磷酸二(2-乙基己基)己醇萃取,然后用反萃取进行萃取。 1:1比例的0.1 M盐酸。向酸性水-乙腈流动相中添加离液六氟磷酸盐,以改善UA的反相色谱,否则保留得不好。获得了鱼类样品的最佳分离条件,并可以进行快速(10分钟),易于使用的色谱,明显优于笨重的传统离子对色谱。为了在我们实验室中常规使用,该方法通过了线性,基质效应(对反应萃取的影响),准确性,精密度和可检测性的内部验证测试。

更新日期:2018-03-14
down
wechat
bug