Suppr超能文献

基于多糖衍生物的共价固定化和涂覆型手性固定相用于N-保护的α-氨基酸及其酯衍生物对映体分离的比较研究。

Comparative studies between covalently immobilized and coated chiral stationary phases based on polysaccharide derivatives for enantiomer separation of N-protected alpha-amino acids and their ester derivatives.

作者信息

Jin Jing Yu, Bae Su Kyoung, Lee Wonjae

机构信息

College of Pharmacy, Chosun University, Gwangju, Republic of Korea.

出版信息

Chirality. 2009 Nov;21(10):871-7. doi: 10.1002/chir.20680.

Abstract

Liquid chromatographic enantiomer separation of several N-benzyloxycarbonyl (CBZ) and N-tert-butoxycarbonyl (BOC) alpha-amino acids and their corresponding ethyl esters was performed on covalently immobilized chiral stationary phases (CSPs) (Chiralpak IA and Chiralpak IB) and coated-type CSPs (Chiralpak AD and Chiralcel OD) based on polysaccharide derivatives. The solvent versatility of the covalently immobilized CSPs in enantiomer separation of N-CBZ and BOC-alpha-amino acids and their ester derivatives was shown and the chromatographic parameters of their enantioselectivities and resolution factors were greatly influenced by the nature of the mobile phase. In general, standard mobile phases using 2-propanol and hexane on Chiralpak IA showed fairly good enantioselectivities for resolution of N-CBZ and BOC-alpha-amino acids and their esters. However, 50% MTBE/hexane (v/v) for resolution of N-CBZ-alpha-amino acids ethyl esters and 20% THF/hexane (v/v) for resolution of N-BOC-alpha-amino acids ethyl esters afforded the greatest enantioselectivities on Chiralpak IA. Also, liquid chromatographic comparisons of the enantiomer resolution of these analytes were made on amylose tris(3,5-dimethylphenylcarbamate)-derived CSPs (Chiralpak IA and Chiralpak AD) and cellulose tris(3,5-dimethylphenylcarbamate)-derived CSPs (Chiralpak IB and Chiralcel OD). Chiralpak AD and/or Chiralcel OD showed the highest enantioselectivities for resolution of N-CBZ-alpha-amino acids and esters, while Chiralpak AD or Chiralpak IA showed the highest resolution of N-BOC-alpha-amino acids and esters.

摘要

在基于多糖衍生物的共价固定化手性固定相(CSPs)(Chiralpak IA和Chiralpak IB)以及涂覆型CSPs(Chiralpak AD和Chiralcel OD)上,对几种N-苄氧羰基(CBZ)和N-叔丁氧羰基(BOC)α-氨基酸及其相应的乙酯进行了液相色谱对映体分离。展示了共价固定化CSPs在N-CBZ和BOC-α-氨基酸及其酯衍生物对映体分离中的溶剂通用性,并且它们的对映选择性和分离因子的色谱参数受到流动相性质的极大影响。一般来说,在Chiralpak IA上使用2-丙醇和己烷的标准流动相对N-CBZ和BOC-α-氨基酸及其酯的分离显示出相当好的对映选择性。然而,对于N-CBZ-α-氨基酸乙酯的分离,50%甲基叔丁基醚/己烷(v/v)以及对于N-BOC-α-氨基酸乙酯的分离,20%四氢呋喃/己烷(v/v)在Chiralpak IA上提供了最大的对映选择性。此外,还在直链淀粉三(3,5-二甲基苯基氨基甲酸酯)衍生的CSPs(Chiralpak IA和Chiralpak AD)和纤维素三(3,5-二甲基苯基氨基甲酸酯)衍生的CSPs(Chiralpak IB和Chiralcel OD)上进行了这些分析物对映体分离的液相色谱比较。Chiralpak AD和/或Chiralcel OD对N-CBZ-α-氨基酸和酯的分离显示出最高的对映选择性,而Chiralpak AD或Chiralpak IA对N-BOC-α-氨基酸和酯的分离显示出最高的分离度。

文献AI研究员

20分钟写一篇综述,助力文献阅读效率提升50倍。

立即体验

用中文搜PubMed

大模型驱动的PubMed中文搜索引擎

马上搜索

文档翻译

学术文献翻译模型,支持多种主流文档格式。

立即体验