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采用蒸发光散射检测的超临界流体色谱法同时测定无机阴离子和阳离子。

Simultaneous determination of inorganic anions and cations by supercritical fluid chromatography using evaporative light scattering detection.

作者信息

Foulon Catherine, Di Giulio Pauline, Lecoeur Marie

机构信息

Univ Lille, EA 7365 - GRITA - Groupe de Recherche sur les Formes Injectables et les Technologies Asssociées, F-59000 Lille, France.

Univ Lille, EA 7365 - GRITA - Groupe de Recherche sur les Formes Injectables et les Technologies Asssociées, F-59000 Lille, France.

出版信息

J Chromatogr A. 2018 Jan 26;1534:139-149. doi: 10.1016/j.chroma.2017.12.047. Epub 2017 Dec 18.

Abstract

Supercritical fluid chromatography (SFC) is commonly used for the analysis of non-polar compounds, but remains poorly explored for the separation of polar and ionized molecules. In this paper, SFC has been investigated for the separation of 14 inorganic ions sampled in aqueous solutions. Four polar stationary phases were first screened using CO-methanol-based mobile phases containing water or different acidic or basic additives, in order to select the most efficient conditions for the simultaneous retention of inorganic cations and anions and to favor their detection using evaporative light scattering detector (ELSD). Orthogonal selectivity was obtained depending on the stationary phase used: whereas anions are less retained on HILIC stationary phase, 2-ethylpyridine (2-EP) stationary phase exhibits strong interaction for anions. Best results were obtained under gradient elution mode using a 2-EP stationary phase and by adding 0.2% triethylamine in the CO-methanol-based mobile phase. The composition of the injection solvent was also investigated. The results showed that a methanolic sample containing a percentage of water not exceeding 20% does not affect the analytical performances obtained on 2-EP. Moreover, the presence of triethylamine in the injection solvent contributes to eliminate peaks shoulders. Among the 14 inorganic ions tested, three cations (Li, Ca and Mg) and five anions (Cl, Br, NO, I, SCN) were totally resolved in 15 min. NO and NO still coeluted in the final optimized conditions. The other investigated ions were either strongly retained on the stationary phase or not detected by the ELSD.

摘要

超临界流体色谱法(SFC)通常用于分析非极性化合物,但在分离极性和离子化分子方面的研究仍较少。本文研究了SFC用于分离水溶液中采样的14种无机离子。首先使用含有水或不同酸性或碱性添加剂的基于CO-甲醇的流动相筛选了四种极性固定相,以选择同时保留无机阳离子和阴离子的最有效条件,并有利于使用蒸发光散射检测器(ELSD)进行检测。根据所使用的固定相获得了正交选择性:阴离子在亲水作用色谱(HILIC)固定相上保留较少,而2-乙基吡啶(2-EP)固定相对阴离子表现出强烈的相互作用。在梯度洗脱模式下,使用2-EP固定相并在基于CO-甲醇的流动相中添加0.2%三乙胺可获得最佳结果。还研究了进样溶剂的组成。结果表明,含水量不超过20%的甲醇样品不会影响在2-EP上获得的分析性能。此外,进样溶剂中三乙胺的存在有助于消除峰肩。在所测试的14种无机离子中,三种阳离子(Li、Ca和Mg)和五种阴离子(Cl、Br、NO、I、SCN)在15分钟内完全分离。在最终优化条件下,NO和NO仍会共洗脱。其他研究的离子要么在固定相上强烈保留,要么未被ELSD检测到。

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