摘要
目的 :建立一种用高效毛细管电泳法测定酒石酸托特罗定中左旋体含量的方法。方法 :研究了影响对映体拆分的手性选择剂种类和浓度 ,缓冲溶液的组成、浓度和pH ,电泳工作电压 ,温度和检测波长 ,择优选择手性分离的最佳电泳条件 ,用含 2 0mmol·L-1羟丙基 - β -环糊精的 0 1mol·L-1三羟基甲氨基甲烷溶液 (用磷酸调节至 pH =3 0 )作为电泳缓冲液 ,工作电压 2 0kV ,柱盒温度为 15℃ ,检测波长 2 0 4nm ,气压进样 3s。结果 :使右旋 -左旋酒石酸托特罗定对映体基线分离。浓度在 0 0 0 1~ 1 5mg·L-1范围内 ,与峰面积的响应呈良好的线性 ,迁移时间和峰面积的RSD小于 5 % ,左旋体加样回收率为 10 2 1% (n =6 ) ,最低检出浓度为 0 5 μg·mL-1。结论
Objective:To establish a high performance capillary electrophoresis (HPCE) method for determining of the levo-enantiomer of tolterodine tartrate.Methods:Both complexation and resolution were affected by the CD type,CD concentration and the pH of electrolyte.The influence of working voltabe and capillary temperature on the enantiomeric separation was also investigated.Electrophoretic medium was 0 1 mol·L\+\{-1\} trishydroxymethylaminomethane buffer (adjust pH to 3 0 with H\-3PO\-4) containing 20 mmol·L\+\{-1\} HP-β-CD.An uncoated capillary used was 57 cm×50 μm(50 cm to the detector).Detection was carried out with a UV detector at 204 nm.The separation was performed at 15 ℃ with a positive voltage of 20 kV.Samples were injected into the capillary by pressure for 3 s.Results:The enantiomers of tolterodine tartrate was separated well.The linear concentration region was 0 001~1 5 mg·mL\+\{-1\}.The RSD for migratory time and peak response were lower than 4 1% and 4 9%.The recovery for levo-enantiomer was 102 1%( n =6).The lowest detective concentration was 0 5 μg·mL\+\{-1\} for each enantiomer.Conclusion:This method was suitable for check levo-enantiomer in tolterodine tartrate in laboratory.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2001年第5期351-354,共4页
Chinese Journal of Pharmaceutical Analysis