手性金属-有机骨架材料[Zn2(D-Cam)2(4,4′ -bpy)]n薄层色谱对苯磺酸氨氯地平外消旋体的分离研究
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篇名: 手性金属-有机骨架材料[Zn2(D-Cam)2(4,4′ -bpy)]n薄层色谱对苯磺酸氨氯地平外消旋体的分离研究
TITLE:
摘要: 目的:建立一种分离苯磺酸氨氯地平外消旋体的方法。方法:先合成手性金属-有机骨架材料[Zn2(D-Cam)2(4,4′ -bpy)]n(简称为Zn-MOF)并对其进行X射线粉末衍射表征,由其与GF254硅胶混合制备薄层色谱固定相后用于分离苯磺酸氨氯地平外消旋体;以两个对映体的比移值和分离度为指标优选分离条件(展开剂组成及比例、手性Zn-MOF的用量等)并进行方法的重现性试验。结果:成功合成了手性Zn-MOF材料并经表征证实;优选的分离条件为取0.10 g手性Zn-MOF混合1.5 g GF254硅胶制备薄层色谱板、展开剂为乙腈-仲丁醇(30 ∶ 70,V/V)。在此条件下,苯磺酸氨氯地平外消旋体实现了有效分离,所得斑点大小均一,比移值>0.27,分离度约为2(RSD=3.8%,n=3)。结论:由手性Zn-MOF制备的薄层色谱固定相对苯磺酸氨氯地平外消旋体具有较好的手性识别能力,且其分离方法操作简单,结果直观、准确、重现性好。
ABSTRACT: OBJECTIVE: To establish a method for the resolution of Amlodipine benzenesulfonate racemates. METHODS: The chiral metal-organic frameworks [Zn2(D-Cam)2(4,4′ -bpy)]n (called Zn-MOF for short) were synthetized, and X ray powder  diffraction characterization was also performed. Chiral Zn-MOF was mixed with GF254 silica gel to prepare TLC solid phase and separate Amlodipine benzenesulfonate racemates. Using specific shift value and resolution degree of 2 enantiomers as index, resolution condition (composition and proportion of developing agent, amount of chiral Zn-MOF) were optimized and reproducibility test of method was also conducted. RESULTS: Chiral Zn-MOF material was successfully synthesized and confirmed after characterization. The optimal resolution condition was as follows as 0.10 g chiral Zn-MOF mixed with 1.5 g GF254 silica gel TLC plate, acetonitrile-butanol as developing agent (30 ∶ 70, V/V). Under the condition, Amlodipine benzenesulfonate racemates was separated effectively; obtained spots were uniform in size with specific shift value>0.27 and resolution rate of 2 (RSD=3.8%, n=3). CONCLUSIONS: The stationary phase of TLC which is prepared by chiral Zn-MOF shows excellent chiral recognition, and resolution method is simple in operation. The result is intuitionistic, accurate and reproducible. The method is suitable for the chiral resolution of Amlodipine benzenesulfonate racemates.
期刊: 2018年第29卷第13期
作者: 张美,钟帅,刘涵,杨宽林,饶高雄
AUTHORS: ZHANG Mei,ZHONG Shuai,LIU Han,YANG Kuanlin,RAO Gaoxiong
关键字: 手性固定相;[Zn2(D-Cam)2(4,4′ -bpy)]n;薄层色谱;苯磺酸氨氯地平外消旋体;分离
KEYWORDS: Chiral stationary phase; [Zn2(D-Cam)2(4,4′ -bpy)]n; TLC; Amlodipine benzenesulfonate racemates; Resolution
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