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丙卡特罗在三种刷型手性固定相上的直接拆分 被引量:4

Study on Separation of Drug Procaterol Enantiomers by Using Three Brush Type CSPs
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摘要 以正己烷-异丙醇二元混合溶剂体系为流动相,在Whelk—OI、DNB—PG和DNB—Leucine3种刷型手性固定相上将药物丙卡特罗直接拆分为(R,R/S)和(S,R/S)对映体,分离系数α值达1.4~1.8。考察了流动相组成及固定相分子结构对对映体分离效果的影响,同时对丙卡特罗与3种固定相的手性识别机理进行了探讨。结果表明,当流动相中异丙醇的体积分数(φB)为2%~30%时,Ink’与InφB之间呈现较好的线性关系。因此,在一定范围内可以根据所需色谱分离系数或保留时间估计流动相的组成。以后出峰对映体所表征的3种手性柱的色谱分离效能分别为:n(Whelk-OI)=10816/m,n(DNB-PG)=4532/m,n(DNB-Leucine)=12844/m。DNBPG柱柱效相对较低,谱峰展宽较大,且有轻微拖尾,需改善柱子装填和预处理技术以提高色谱分离柱效。 Two types - ( R, R/S) and ( S, R/S) procaterol enantiomers have been separated on three brush type chiral stationary phases-- ( R, R) -Whelk-O1 CSP, (R) -N- (3,5-dinitrobenzoyl) phenylglycine(DNB-PG) CSP and (R) -N-(3,5-dinitrobenzoyl) leucine (DNB-Leucine) CSP by using the binary mixed solvent of hexane and isopropanol as mobile phase. A good separation factor was obtained with α value from 1.4 to 1.8. Effect of mobile phase composition and CSPs' structure on enantioseparation was investigated, and the chiral recognition mechanism were also discussed. A good relationship between lnk'and lnφB (the volume fraction of isopropanol) for three CSPs was achieved when the φB change from 2% to 30% . The result indicated that proper composition of mobile phase could be conveniently evaluated according to the needed separation factor value or retention time. Furthermore, the chromatographic column efficiency for the three chiral columns have been characterized by the later eluted enantiomer, with n(Whelk-OI)of 10 816/m, n(DNB-PG) of 4 532/m and Ft(DNB-Leucine) of 12 844/m.
出处 《分析测试学报》 CAS CSCD 北大核心 2010年第4期407-410,共4页 Journal of Instrumental Analysis
基金 湖北省教育厅基金资助项目(B20082903) 四川省应用基础研究基金资助项目(04GY029-083-3)
关键词 丙卡特罗 对映体拆分 刷型手性固定相 手性识别机理 procaterol enantiomer separation brush type chiral stationary phase chiral recognition mechanism
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