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建立并优化了高效液相色谱手性固定相分离富马酸比索洛尔对映体的方法。使用直链淀粉手性固定相(Chiralpak AD-H柱)在正相条件下拆分了富马酸比索洛尔对映体,考察了达到最佳分离效果时,流动相中极性调节剂的组分、流动相中三乙胺的体积分数以及柱温对富马酸比索洛尔对映体拆分影响。流动相为正己烷/乙醇/三乙胺(90/10/0.1,V/V/V),流速1.0 mL/min,紫外检测波长270 nm,柱温30℃时,两种异构体能达到较好的基线分离,并且不对称合成的(S)-富马酸比索洛尔和(R)-富马酸比索洛尔两种异构体产品,对映体过量(e.e.)均高于99.0%,在此色谱条件下的色谱图峰形良好。方法可广泛用于跟踪手性比索洛尔富马酸盐的合成过程分析和质量控制。
A method for the separation of bisoprolol fumarate enantiomers by high performance liquid chromatography with chiral stationary phase was established and optimized. The enantiomers of bisoprolol fumarate were resolved under normal phase using an amylose chiral stationary phase (Chiralpak AD-H column). When the optimal separation was achieved, the effect of the polar regulator Volume fraction of triethylamine in the mobile phase, and the effect of column temperature on the enantiomeric separation of bisoprolol fumarate. The mobile phase was n-hexane / ethanol / triethylamine (90/10 / 0.1, V / V / V) at a flow rate of 1.0 mL / min and UV detection wavelength was 270 nm. Good baseline separation, and the enantiomeric excess (ee) of asymmetric synthesis of bis (S) -bis (bis (2-tolyl) sulfamate) and bis (R) , The chromatogram peaks under this chromatographic condition are good. The method can be used extensively for tracking synthesis and quality control of chiral bisoprolol fumarate.