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万古霉素手性固定相分离曼尼希碱类化合物对映体

Chiral Separation of Some Mannich Compounds by High Performance Liquid Chromatography on Vancomycin-based Stationary Phase

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【作者】 毕玉金杨晶江坤关瑾李发美

【Author】 Bi Yu-Jin1, Yang Jing1, Jiang Kun1, Guan Jin1, 2, Li Fa-Mei*11(School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016)2(School of Applied Chemistry, Shengyang Institute of Chemical Technology, Shenyang 110124)

【机构】 沈阳药科大学药学院沈阳药科大学药学院 沈阳110016沈阳110016沈阳化工学院应用化学学院沈阳110124

【摘要】 采用大环抗生素类万古霉素手性固定相高效液相色谱法研究了一系列曼尼希碱类化合物的手性分离情况,并讨论了流动相中有机相的种类和比例、缓冲盐的种类和浓度、pH和柱温对该类化合物手性分离的影响。最佳实验条件为:乙腈:硝酸铵(35mmol/L,pH3.8)=15∶85(V/V),柱温15℃,流速0.6mL/min,检测波长300nm;四氢呋喃:硝酸铵(20mmol/L,pH4)=15∶85(V/V),柱温15℃,流速0.6mL/min,检测波长350nm。通过对比研究8种曼尼希碱类化合物的色谱行为,从结构上讨论了化合物中各种官能团对手性分离的影响,并探讨了手性分离的内在机制。

【Abstract】 Chiral separation of some Mannich compounds by high performance liquid chromatography (HPLC) on vancomycin-based stationary phase was studied. Effects of the type and concentration of organic modifier, the pH, the type and concentration of buffer solution, and column temperature on the retention time and enantiomeric resolution were investigated and discussed. The separation conditions were as follows: acetonitrile, ammonium nitrate (35 mmol/L, pH 3.8)=15∶85(V/V) as the mobile phase, at a flow rate of 0.6 mL/min, column temperature of 15℃, detection wavelength of 300 nm; tetrahydrofuran, ammonium nitrate (20 mmol/L, pH 4)=15∶85(V/V) as the mobile phase, at a flow rate of 0.6 mL/min, column temperature of 15℃, detection wavelength of 350 nm. The chromatographic behavior of Mannich compounds enantiomers with very similar structure was studied comparatively, and the structural factors affecting chiral separation as well as the mechanism of chiral separation were discussed.

  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2007年06期
  • 【分类号】R917
  • 【被引频次】8
  • 【下载频次】251
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