Abstract

A new chiral stationary phase based on homochiral crystals of α-NiSO₄∙6H₂O obtained under the condition of Viedma ripening is proposed for the separation of 2-pentanol racemate. The retention times and separation parameters are determined from chromatograms of the separation of 2-pentanol racemate. Separation occurs in the concentration range 4–11.3 mg/mL (eluent is a mixture of n-heptane and chloroform). The reliability of the separation is confirmed by polarimetry and the gas-chromatographic analysis of the fractions of each peak with mass-spectrometric detection. It is shown that the separation parameters do not depend on the elution rate. With an increase in the volume fraction of chloroform, the eluting force increases, and the separation criterion and the selectivity coefficient decrease. The latter range from 1.09 to 1.32. The maximum separation efficiency was 2000 tp/m. The proposed stationary phase can be used for the semi-preparative separation of ennatiomers.

中文翻译：

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基于 Viedma 成熟获得的同手性 NiSO4·6H2O 晶体在手性固定相上分离 2-戊醇外消旋体

摘要

提出了一种基于在Viedma 熟化条件下获得的 α-NiSO ₄ ∙6H ₂ O 同手性晶体的新型手性固定相，用于 2-戊醇外消旋物的分离。保留时间和分离参数由分离 2-戊醇外消旋物的色谱图确定。分离发生在 4–11.3 mg/mL 的浓度范围内（洗脱液是n-庚烷和氯仿）。分离的可靠性通过旋光测定法和用质谱检测每个峰的馏分的气相色谱分析来证实。结果表明，分离参数不依赖于洗脱速率。随着氯仿体积分数的增加，洗脱力增加，分离标准和选择性系数降低。后者的范围从 1.09 到 1.32。最大分离效率为2000 tp/m。建议的固定相可用于对映异构体的半制备分离。