摘要
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 selfmade 1-naphthalene vancomycin as chiral stationary phase(Na-VAN CSP),and D-tartaric acid(DTar),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 2was obtained. The results showed that the size of alcohol modifier and the three dimensional configuration of CMPA played an important role in the enantioseparation.
出处
《分析测试学报》
CAS
CSCD
北大核心
2017年第2期242-246,共5页
Journal of Instrumental Analysis
基金
国家自然科学基金资助项目(81102408)