摘要
建立了卡维地洛对映体的高效液相色谱分析方法。使用Chiralpak AD-H手性色谱柱,考察了流动相中极性调节剂的种类和体积分数、流动相中二乙胺的体积分数、柱温以及流速对卡维地洛对映体拆分的影响。确定了最佳拆分条件:流动相为正己烷-异丙醇-二乙胺(体积比70∶30∶0.05);流速1.0 mL/min;检测波长243 nm;柱温30℃。卡维地洛与固定相相互作用的焓变差值Δ(ΔH0)和熵变差值Δ(ΔS0)分别为-505.6 J/mol和-1.055 J/(mol.K)。研究手性合成了(S)-卡维地洛,对映体过量值(e.e.)达99.0%以上。在优化实验条件下,通过考察峰面积的显著差异,得到卡维地洛对映体的出峰顺序为:先S体,后R体。所建立的方法简单快捷、重复性好,可用于卡维地洛的质量研究和控制。
A method of HPLC with Chiralpak AD-H Chiral column for enantiomeric separation of carvedilol was developed.The influences of concentration of organic solvent,proportion of diethylamine,column temperature and flow rate on the enantiomeric separation were investigated.The optimal chromatographic conditions were as follows：mobile phase：hexane-isopropanol-diethylamine（70∶30∶0.05,by volume）;flow rate：1.0 mL/min;detection wavelength：243 nm;column temperature：30 ℃.The differences of enthalpy change and entropy change for the interaction of carvedilol and stationary phase were calculated to be-505.6 J/mol and-1.055 J/（mol·K）,respectively.The enantiomeric excess（e.e.） of the synthesized（S）-carvedilol was beyond 99.0%.Under the optimal conditions,according to the significant difference of peak area,the elution order of two enantiomers was obtained to be S-carvedilol followed by R-carvedilol.The developed HPLC method was simple,rapid and reproducible,and could be used for the quality study and control of carvedilol.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第9期923-927,共5页
Journal of Instrumental Analysis
基金
国家自然科学基金资助项目(20876076)
国家重点基础研究发展计划资助项目(2009CB724700)
