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机构地区:[1]武汉大学化学与分子科学学院,武汉430072 [2]武汉大学生命科学学院,武汉430072
出 处:《药物分析杂志》2005年第4期402-405,共4页Chinese Journal of Pharmaceutical Analysis
摘 要:目的:采用大环抗生素游壁菌素键合硅胶手性分离柱 Chirobiotic T 对焦谷氨酸手性对映体进行分离。方法:以 Chirobi-otic T 柱为色谱柱,流动相为甲醇-三乙胺缓冲溶液(醋酸调 pH)体系和甲醇-醋酸-三乙胺极性有机溶剂体系,检测波长为214 nm,考察了焦谷氨酸对映体的分离,并与大环抗生素万古霉素键合硅胶手性分离柱 Chirobiotie V 进行了比较。结果:在甲醇-0.1%三乙胺(80:20,以醋酸调 pH 4.0)为流动相时,焦谷氨酸对映体在 Chirobiotic T 柱上可以实现基线分离,但有系统峰干扰;而甲醇-醋酸-三乙胺极性有机溶剂体系则更利于焦谷氨酸对映体的分离,并可对实际样品进行定量分析,无系统峰干扰。而在这2种条件下,Chirobiotic V 柱无法基线拆分焦谷氨酸对映体。结论:Chirobiotie T 柱对焦谷氨酸手性对映体有很好的拆分能力,可用于实际样品的定量分析。Objective:To establish an HPLC enantioseparation of pyroglutamic acid using teicoplanin bonded silica stationary phase column (Chirobiotic T).Methods:Two mobile phase systems,methanol-triethylamine buffer solu- tion(adjusted pH with acetic acid)and methanol-acetic acid-triethylamine polar organic system were investigated to optimize the separation of D,L-pyroglutamic acid on column Chirobiotic T,with the detection wavelength as 214 nm.The separation was also carried out on the column with vancomycin as the chiral stationary phase for compari- son.Results:Enantiomers of pyroglutamic acid are successfully separated by the column Chirobiotic T under both mobile phase conditions.And the base line enantioseparation was proved to be more easily to be achieved with the methanol-acetic acid-triethylamine polar organic system and quantification could be performed without the inter- ference of the system peak.Baseline separation could not be obtained under these two mobile phase systems with vancomycin as the stationary phase.The quantitative analysis of laboratory-synthesized sample was achieved.Con- clusions:Chirobiotic T is suitable for enantioseparation of pyroglutamic acid and the presented separation method is valuable for sample quantitative analysis.
关 键 词:焦谷氨酸 色谱分离 高效液相 大环抗生素 手性对映体 溶剂体系 定量分析 三乙胺 缓冲溶液 检测波长 万古霉素 基线分离 分离柱 流动相 醋酸 甲醇 色谱柱 硅胶 键合 有机 极性 干扰 系统 样品 拆分
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