论文部分内容阅读
目的:研究拆分外消旋药物氯胺酮的新工艺。方法:在 HPLC 上通过同时采用手性固定相和手性流动相的方式进行双相复合识别拆分外消旋手性药物对映体,结合热力学参数探讨 HPLC 的双相识别拆分机理。结果:在γ-氨丙基硅胶上涂覆质量分数为15%的纤维素-三苯基氨基甲酸酯(CTPC)作为手性固定相,流动相为正己烷-异丙醇(90:10),添加0.50 mmol·L~(-1) N-苄氧羰基-S-苯基-L-半胱胺酸(BPC)为手性试剂,流动相流速为1.0 mL·min~(-1),检测波长为254 nm,氯胺酮对映体的分离选择性系数为1.21,分离度为1.57。结论:BPC 的辅助识别作用明显提高了 CTPC 对氯胺酮对映体的手性识别能力。
Objective: To study the new technology of resolving ketamine, a racemate. Methods: The enantiomers of racemic chiral drugs were separated and identified by biphasic method using chiral stationary phase and chiral mobile phase simultaneously on HPLC. The mechanism of biphasic identification and resolution was discussed by thermodynamic parameters. Results: Cellulose-triphenylcarbamate (CTPC) as a chiral stationary phase was coated on γ-aminopropyl silica gel with a mass fraction of 15% and the mobile phase was n-hexane-isopropanol ), 0.50 mmol·L -1 N-benzyloxycarbonyl-S-phenyl-L-cysteine (BPC) was added as chiral reagent and the mobile phase flow rate was 1.0 mL · min -1 , The detection wavelength was 254 nm, the separation selectivity of ketamine enantiomer was 1.21 and the resolution was 1.57. CONCLUSION: Auxiliary recognition of BPC significantly improves the chiral recognition of ketamine enantiomers by CTPC.