制备型高效液相色谱在手性分离中的应用研究

目的：考察制备型高效液相色谱在分离手性药物中的实际应用及影响因素。方法采用大赛璐手性色谱柱，以正己烷－异丙醇－冰乙酸溶液（100∶1∶0．1％）为流动相，流速70mL? min －1，检测波长240nm，考察了制备型高效液相色谱的放大以及影响因素。结果布洛芬对映异构体在分析条件下实现了良好的分离，将该方法线性放大到制备分离中，根据硬件设备及样品分离度等具体情况优化各项色谱参数，轻松实现了布洛芬原料1日55 g的分离效果，产品回收率达到90％，光学纯度达到98．5％以上。结论结果表明，制备型高效液相色谱应用于布洛芬对映体分离中，简便、可靠、高效、易于放大，可广泛用于手性药物规模化分离。

AppIication of Preparative high Performance Liquid Chromatography in ChiraI Separation

OBJECTIVE To investigate the preparative high performance liquid chromatography and the influ-ence factors for practical application in the separation of chiral drugs .METHODS Use the Daicel chiral column , with hexane-isopropanol-AceticAcid solution ( 99∶1∶0.1%) as mobile phase ,respectively study the analysis type high efficiency liquid phase chromatographic method of preparation type high-efficiency liquid phase chromatography of amplification and laboratory scale factors effecting preparation .RESULTS Ibuprofen enantiomeric isomers under the conditions of the good separation , the linear amplification to separating and preparing , optimizes the chromato-graphic parameters according to the specific circumstances of the hardware equipment and sample separation degree and easily realize the separation effect of ibuprofen raw materials 55 gper days,the product recovery rate reached 90%,the optical purity reached 98.5%.CONCLUSION The method for the preparation of high-performance liq-uid chromatography in chiral sample provides a reference ,combined with the preparation instrument ,can achieve a certain scale industrial amplification .