Chiral Separation of β-Receptor Blockers and Analogs on Novel Norvancomycin-Bonded Chiral Stationary Phase
去甲万古霉素键合手性固定相拆分β-受体阻滞剂类药物及其结构类似物的研究

Enantiomeric separation of racemates of 8 beta-receptor blockers and analogs was performed on a novel norvancomycin-bonded chiral stationary phase (NVC-CSP) in polar organic mode using high performance liquid chromatography. The influences of mobile phase composition, acetic acid and triethylamine contents, temperature and flow rate on enantiomeric separation were studied. It was found experimentally that with the increase of the fraction of methanol in the mobile phase, the same tendency was found for all the chiral solutes studied, i. e., the decrease in retention factor (kappa) and the increase in the enantioselectivity factor (alpha). With the increase of column temperature, most solutes were less retained and the alpha value decreased accordingly. Better resolutions were obtained at lower flow rates as a result of the minimization of the resistance to mass-transfer. Better separation results and suitable retentions for most solutes were obtained when a mixture of acetonitrile-methanol-acetic acid-triethylamine (60: 40: 0.4: 0.2, v/v) was used as mobile phase at a flow rate of 0.6 mL/min, and the column temperature was set at 25 degrees C. Conclusions can be drawn from the experimental data that pi-pi complexation, dipole-stacking interactions were engaged in the process of enantiomeric separation, while hydrogen bonding interaction between solutes and CSP was commonly non-enantioselective, although it was mainly responsible for the increased retention in the acetonitrile-predominant mobile phases.