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评价苯甲酰基化环糊精点击手性固定相在反相高效液相色谱中的对映体分离。

Evaluation of perphenylcarbamated cyclodextrin clicked chiral stationary phase for enantioseparations in reversed phase high performance liquid chromatography.

机构信息

Key Laboratory of Soft Chemistry and Functional Materials, Ministry of Education, Nanjing University of Science and Technology, Nanjing 210094, People's Republic of China.

Key Laboratory of Soft Chemistry and Functional Materials, Ministry of Education, Nanjing University of Science and Technology, Nanjing 210094, People's Republic of China.

出版信息

J Chromatogr A. 2014 Oct 10;1363:119-27. doi: 10.1016/j.chroma.2014.08.040. Epub 2014 Aug 17.

Abstract

In this study, perphenylcarbamated cyclodextrin clicked chiral stationary phase (CSP) was developed with high column efficiency. The characteristics of the column were evaluated in terms of linearity, limit of detection and limit of quantification. The enantioselectivity of the as-prepared clicked CSP was explored with 26 recemates including aryl alcohols, flavanoids and adrenergic drugs in reversed phase high-performance liquid chromatography. The effect of separation parameters including flow rate, column temperature, organic modifier and buffer on the enantioselectivity of the clicked CSP was investigated in detail. The correlation study of the analytes structure and their chiral resolution revealed the great influence of analytes' structure on the enantioseparations with cyclodextrin CSP. Methanol with 1% of triethylammonium acetate buffer (pH 4) was proved to be the best choice for the chiral separation of basic enantiomers.

摘要

在这项研究中,开发了一种具有高柱效的全苯基碳化二亚胺点击手性固定相(CSP)。通过线性、检测限和定量限来评估柱的性能。采用反相高效液相色谱法,用 26 种外消旋体(包括芳醇、黄酮类和肾上腺素能药物)研究了所制备的点击 CSP 的对映选择性。详细研究了分离参数(流速、柱温、有机改性剂和缓冲液)对点击 CSP 对映选择性的影响。对分析物结构与其手性拆分的相关性研究表明,分析物结构对环糊精 CSP 的手性拆分有很大影响。甲醇中含有 1%的三乙铵乙酸盐缓冲液(pH4)被证明是手性拆分碱性对映异构体的最佳选择。

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