昆明医科大学药学院暨云南省天然药物药理重点实验室
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姚艳云, 孙孔春, 王永茜, 等. 手性流动相添加剂法拆分西那卡塞原料及中间体[J]. 分析测试学报, 2017,36(2):242-246.
Enantiomeric Separation of Raw Material and Intermediate of Cinacalcet Using Chiral Mobile Phase Additives[J]. 2017,36(2):242-246.
以自制1-萘万古霉素(Na-VAN)为手性固定相(CSP),D-酒石酸(D-Tar)、L-酒石酸二乙酯(L-TADE)、D-酒石酸二乙酯(D-TADE)分别为手性流动相添加剂(CMPA),建立了西那卡塞原料1-(1-萘基)乙胺(化合物1)及西那卡塞中间体(化合物2)的高效液相色谱手性拆分方法。考察了流动相中醇类改性剂、CMPA对对映体分离的影响,初步探讨了手性识别机理。以Na-VAN为CSP,正相模式下,添加不同种类的CMPA,化合物1、化合物2均可获得一定程度的分离,其中以D-TADE为CMPA时,化合物1、化合物2获得最佳分离。结果表明,醇的分子体积、CMPA的立体构型均对手性分离有影响。
An HPLC method was established for the chiral separation of cinacalcet raw material,1-(1-naphthyl)-ethylamine(compound-1) and intermediate of cinacalcet(compound 2),by using self made 1 naphthalene vancomycin as chiral stationary phase(Na-VAN CSP),and D-tartaric acid(D-Tar),L-tartaric acid diethyl ester(L-TADE) and D-tartaric acid diethyl ester(D-TADE) as chiral mobile phase additives(CMPA),respectively.The influences of alcohol modifiers and CMPA types were studied.The mechanism of enantioseparation was also discussed.On Na-VAN CSP,compound 1 and 2 got certain degree of enantioseparation with different CMPA under normal phase conditions.When D-TADE was used as CMPA,the optimal enantioseparation for both compound 1 and 2 was obtained.The results showed that the size of alcohol modifier and the three dimensional configuration of CMPA played an important role in the enantioseparation.
1-(1-萘基)乙胺西那卡塞中间体1-萘万古霉素手性流动相添加剂对映体分离
1-(1-naphthyl) ethylamineintermediate of cinacalcet1-naphthalene vancomycinchiral mobile phase additiveenantioseparation
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