替考拉宁键合手性固定相高效液相色谱法直接拆分泮托拉唑钠对映体

以替考拉宁为手性选择剂制备了大环抗生素类手性固定相替考拉宁键合手性固定相(T-CSP),建立了T-CSP反相液相色谱直接拆分泮托拉唑钠对映体的方法。考察了流动相中有机改性剂的种类和比例、柱温以及流动相流速对拆分泮托拉唑钠对映体的影响。研究发现,用甲醇作有机改性剂比乙腈更有利于对映体的分离;在研究的温度范围内,随着柱温的升高,对映体的保留时间缩短,同时分离因子和分离度降低;在一定范围内降低流速有利于对映体的分离。采用T-CSP色谱柱(150 mm×4.6 mm i.d.,5 μm),以甲醇-水(体积比为35∶65)为流动相,在流速0.6 mL/min、检测波长290 nm、柱温20 ℃的条件下,泮托拉唑钠对映体获得了近于基线的分离,所建立的方法具有简便快速及重复性好等优点。

Direct Enantioseparation of Pantoprazole Sodium by High Performance Liquid Chromatography on Teicoplanin-Bonded Chiral Stationary Phase

Teicoplanin-bonded chiral stationary phase was prepared and used for the direct chiral separation of racemic pantoprazole sodium by reversed-phase high performance liquid chromatography (HPLC). The influences of organic modifiers, the composition of mobile phase, the flow rate and column temperature on enantioseparation were studied. It was found that methanol was preferred than acetonitrile when used as organic modifier. With the increase of column temperature, chiral solutes were less retained and the separation factor value decreased indicating that lower temperature was better for the enantioseparation. Better resolution was obtained at lower flow rates as a result of minimization of the resistance of mass transfer. Based on these experimental data, the chiral HPLC method for the analysis of pantoprazole sodium on prepared chiral column (150 mm x 4.6 mm i. d., 5 microm) was established with simplicity and good reproducibility, by using methanol-water (35 : 65, v/v) as mobile phase at a flow rate of 0.6 mL/min and 20 degrees C.