毛细管电泳法检测美普他酚手性.PDF

复旦学报(医学版) Fudan Univ J Med Sci2005 Jan,32(1) 105 毛细管电泳法检测美普他酚手性 拆分中的光学纯度关 陈燕郁韵秋郑优丽仇缀百“ (复旦大学药学院药物化学教研室 上海 200032) [摘要】目的 建立测定二对甲苯甲酞酒石酸美普他酚对映体的毛细管区带电泳法，并检测其光学纯度。方法 采用72 cm x 50 pm未涂层石英毛细管，30 mmol几磷酸缓冲液(州8.05，内含0. 5 % TM-卜CD，乙睛12%)，运 行电压20 kV，毛细管柱温20 r-，压力进样3 kPax3s，检测波长200 nm。结果 在选定的实验条件下二对甲苯 甲酞酒石酸美普他酚对映体达到基线分离。两对映体在0.10--0.80 mg/mL的浓度范围内，浓度与峰面积的响 应均呈良好的线性关系，相关系数分别为:0.9996和0.9998。迁移时间的RSD在3%以内，峰面积的RSD在 10%以内，左旋体的加样回收率为100.26%(n=6)，最低检测浓度为0.02 mg/mLo测定3批样品的光学纯度 分别为84.10%,92.54%,)99.60%。结论 本法适用于实验室中二对甲苯甲酞酒石酸美普他酚光学纯度的常 规测定。 【关键词】毛细管区带电泳法;二对甲苯甲酞酒石酸美普他酚;光学纯度;三甲基一P-环糊精 【中国图书馆分类法分类号】R 927 Determination of the Optical Purity during Separation of Meptazinol by HPCE CHEN Yan, YU Yun-qiu, ZHENG You-Ii, QIU Zhui-bai (Department of Medicinal Chemistry, School of Pharmacy, Fudan Unizaersity, Shanghai 200032, China ) [Abstract]Purpose To establish a high performance capillary electrophoresis (HPCE) method for deter- mining the optical purity of meptazinol di-p-toluoyl tartaric acid.MethodsFused-silica capillary used was 72二x 50 porn I . D. Electrophoretic medium was 30 mmol/L phosphate (pH 8.05) with 0. 5 %(W/V) TM-仔CD and 12 % acetonitrile. Detection was carried out with a UV detector at 200 rum. The separation was performed at 20℃with a positive voltage of 20 kV. Samples were injected into the capillary by pressure at 3 kPa for 3 s.ResultsThe enantiomers of meptazinol di-p-toluo贝tartaric acid was separated well. The linear concentration region was 0. 10-0. 80 mg/n止.The RSD for migratory time and peak response