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

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。

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.