摘要
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 an HPLC method for chiral separation of pinocembrin enantiomers;to monitor the process of separation reaction of pinocembrin and to determine the optical purity of the product.Methods:RP-HPLC with Chiralpak AD-RH chiral column was adopted.The mobile phase was 100% methanol at the flow rate of 1.0 mL·min-1,and the detective wavelength was 290 nm.Results:The resolution of pinocembrin enantiomers was 5.0 under the above conditions.The method was used for determining the optical purity of the separated enantiomers of pinocembrin.The enantiomeric excess percentage(ee%) was over 97%.Conclusion:With good resolution and repeatability,the method can be reliably used for chiral separation of pinocembrin enantiomers,and determination of the optical purity of S- and R-pinocembrin sample.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2010年第1期88-90,共3页
Chinese Journal of Pharmaceutical Analysis
基金
国家重大科技专项(2009ZX09501)
中国医学科学院药物研究所基本科研业务费专项(2006QN23)
卫生公益性行业科研专项(200802038)