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使用大环糖肽抗生素键合固定相高效液相色谱法直接拆分卡巴拉汀

Enantioseparation of Rivastigmine by High Performance Liquid Chromatography Using Vancomycin Chiral Stationary Phase

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【作者】 许哲周宁许旭许杏祥

【Author】 Xu Zhe1,2, Zhou Ning1, Xu Xu1, Xu Xing-Xiang1 1(Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai 200032) 2(Graduate School of Chinese Academy of Sciences, Beijing 100039)

【机构】 中国科学院上海有机化学研究所中国科学院上海有机化学研究所 上海200032中国科学院研究生院北京100039上海200032

【摘要】 采用高效液相色谱法在大环糖肽抗生素键合固定相手性柱上拆分了卡巴拉汀(Rivastigmine)对映体。考察了甲醇∶乙酸∶三乙胺流动相体系中乙酸和三乙胺的浓度和比例、有机酸的种类、分离温度及流动相流速对拆分结果的影响。选定的色谱条件为:Chirobiotic V手性柱(250mm×4.6mmi.d.,5μm),流动相为V(甲醇)∶V(乙酸)∶V(三乙胺)=100∶0.02∶0.01,柱温5℃,流速0.5mL/min,检测波长274nm。在柱温5~30℃范围内测定lnα与1/T呈线性关系:lnα=ΔΔH0/RT+ΔΔR0/R。

【Abstract】 Direct enantioseparation of rivastigmine was achieved by high performance liquid chromatography using a vancomycin bound chiral stationary phase. The effects of the content and ratio of acetic acid/triethylamine in the mobile phase, acid additive, column temperature and flow rate of mobile phase on the enantioseparation of rivastigmine were studied. By using the Chirobiotic V column (250 mm × 4.6 mm i.d., 5 μm), and methanol:acetic acid: triethylamine (100∶0.02∶0.01, V/V) as mobile phase, flow rate of 0.5 mL/min, detection wavelength of 274 nm, enantioseparation of rivastigmine was achieved. The relationship between lnα and 1/T was investigated in the range of 5-30℃. The linear equation is lnα=ΔΔH0/RT+ΔΔS0/R.

  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2007年07期
  • 【分类号】R917
  • 【被引频次】6
  • 【下载频次】210
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