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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Comparative modelling study on enantioresolution of structurally unrelated compounds with amylose-based chiral stationary phases in reversed phase liquid chromatography-mass spectrometry conditions
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Comparative modelling study on enantioresolution of structurally unrelated compounds with amylose-based chiral stationary phases in reversed phase liquid chromatography-mass spectrometry conditions

机译：基于三相液相色谱 - 质谱条件下基于直链淀粉基手性固定相的结构不相关化合物对比较模拟研究

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摘要

Polysaccharide-based chiral stationary phases (CSPs) are the most used chiral selectors in HPLC. These CSPs can be used in normal, polar organic and aqueous-organic mobile phases. However, normal and polar organic mobile phases are not adequate for chiral separation of polar compounds, for the analysis of aqueous samples and for MS detection. In these situations, reversed phase conditions, without the usual non-volatile additives incompatible with MS detection, are preferable. Moreover, in most of the reported chiral chromatographic methods, retention is too large for routine work. In this paper, the chiral separation of 53 structurally unrelated compounds is studied using three commercial amylose-based CSPs -coated amylose tris(3,5-dimethylphenylcarbamate) (Am1), coated amylose tris(5-chloro-2-methylphenylcarbamate) (Am2), and immobilised amylose tris(3-chloro-5-methylphenylcarbamate) (Am3)-. Chiral separations are carried out using acetonitrile/ammonium bicarbonate (pH = 8.0) mixtures, reversed mobile phases compatible with MS detection. To provide realistic conditions for routine analysis, maximum retention factors are set to 15. Retention and enantioresolution behaviour of compounds in those CSPs are compared. On the other hand, to compare and describe the resolution ability of these CSPs, 58 structural variables of the compounds are tested to model for the first time a categorical enantioresolution (CRs) for Am1 and Am3 CSPs. Discriminant partial least squares, for one response categorical variable (DPLS1) is used for feature selection, modelling. The final DPLS1 models showed good descriptive ability. (C) 2020 Elsevier B.V. All rights reserved.
机译：基于多糖的手性静止阶段（CSP）是HPLC中最常用的手性选择器。这些CSP可用于正常，极性有机和水性移动相。然而，正常和极性有机流动相对于含水样品的分析和MS检测，不足以进行对极性化合物的手性分离。在这些情况下，优选具有与MS检测不相容的通常的非挥发性添加剂的反相条件，是优选的。此外，在大多数报告的手性色谱方法中，保留太大而不能进行常规工作。在本文中，使用三种基于三种基于三种基于CSP的CSPS包涂层三（3,5-二甲基苯基氨基甲酸酯）（AM1），涂覆的淀粉糖三（5-氯-2-甲基苯基氨基甲酸酯）（AM2）进行手性分离）和固定化的直链淀粉三（3-氯-5-甲基苯基氨基甲酸酯）（AM3） - 。使用乙腈/碳酸氢铵（pH = 8.0）混合物进行手性分离，与MS检测相容的反转的流动相。为了提供常规分析的现实条件，将最大保留因子设定为15.比较这些CSP中化合物的保留和对升压行为。另一方面，为了比较和描述这些CSP的分辨率，将化合物的58个结构变量进行了测试，首次测试AM1和AM3 CSP的分类enalioreSolution（CRS）。一个响应分类变量（DPLS1）用于一个响应分类变量（DPLS1）用于特征选择，建模。最终的DPLS1模型显示出良好的描述性能力。 （c）2020 Elsevier B.v.保留所有权利。

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