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用于在“清洁”水系统中同时预富集和分离有机及无机硒物种的多孔石墨化碳固定相的评估。

Evaluation of porous graphitic carbon stationary phase for simultaneous preconcentration and separation of organic and inorganic selenium species in "clean" water systems.

作者信息

Dauthieu Maxime, Bueno Maïté, Darrouzes Jérôme, Gilon Nicole, Potin-Gautier Martine

机构信息

Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Université de Pau et des Pays de l'Adour, UMR 5034, Helioparc Pau Pyrénées, 2 avenue du Président Angot, 64000 Pau, France.

出版信息

J Chromatogr A. 2006 May 5;1114(1):34-9. doi: 10.1016/j.chroma.2006.02.018. Epub 2006 Feb 21.

DOI:10.1016/j.chroma.2006.02.018
PMID:16494887
Abstract

A high performance liquid chromatography procedure, based on porous graphitic carbon stationary phase, was evaluated for simultaneous on-line preconcentration and separation of organic and inorganic selenium species. Detection was achieved by inductively coupled plasma mass spectrometry with collision/reaction cell (ICP-CRC-MS). Different concentrations of formic acid were tested as mobile phase. A 240 mmol L(-1) concentration with pH adjusted to 2.6, allowed the separation of five species, i.e. selenite, selenate, selenomethionine, selenocystine and selenoethionine. On-line preconcentration of these five species was achieved when heptafluorobutyric acid was used as injection medium, inducing an enrichment of solutes at the top of the column which allowed large volumes (up to 1 mL) to be injected. Combining these injection conditions and 80Se monitoring with ICP-CRC-MS, detection limits between 2 and 8 ng (Se)L(-1), depending on the species, were obtained. Because of the extremely low detection limits obtained, the method was successfully applied to mineral waters.

摘要

基于多孔石墨化碳固定相的高效液相色谱法,用于同时在线预富集和分离有机及无机硒物种。采用电感耦合等离子体质谱仪结合碰撞/反应池(ICP-CRC-MS)进行检测。测试了不同浓度的甲酸作为流动相。浓度为240 mmol L(-1)且pH值调至2.6时,可分离出五种物种,即亚硒酸盐、硒酸盐、硒代蛋氨酸、硒代胱氨酸和硒代乙硫氨酸。当使用七氟丁酸作为进样介质时,可实现这五种物种的在线预富集,使溶质在柱顶富集,从而允许进样大体积(高达1 mL)的样品。将这些进样条件与ICP-CRC-MS对80Se的监测相结合,根据物种不同,检测限在2至8 ng (Se)L(-1)之间。由于获得了极低的检测限,该方法成功应用于矿泉水中。

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