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目的:建立匹诺塞林的手性分析方法,用于拆分产物光学纯度的分析测定,并对手性拆分反应进行监测。方法:采用高效液相色谱法。使用Chiralpak AD-RH淀粉类手性柱,流动相为100%甲醇,流速1.0 mL.min-1,检测波长290 nm。结果:匹诺塞林消旋体在此条件下的分离度为5.0。将该方法实际应用于手性拆分反应得到的光学异构体的光学纯度测定,结果对映体过量百分比(ee%)在97%以上。结论:本方法分离度与重现性好,可用于匹诺塞林光学纯度的分析测定,并对拆分反应进行监测,结果可靠。
OBJECTIVE: To establish a chiral analytical method of pinoxirelin, which can be used for the analysis and determination of the optical purity of the split product. The chiral resolution reaction was monitored. Methods: Using high performance liquid chromatography. The Chiralpak AD-RH starch chiral column was used. The mobile phase consisted of 100% methanol and the flow rate was 1.0 mL · min-1. The detection wavelength was 290 nm. Results: The resolution of Pinocinlin racemate under this condition was 5.0. The method was applied to the optical purity determination of the optical isomers obtained by chiral resolution, and the result showed that the percentage ee% of the enantiomeric excess was above 97%. Conclusion: The method has good resolution and reproducibility, which can be used for the determination of optical purity of pinoxillin. The resolution of the reaction is monitored and the results are reliable.