【摘要】 用手性源(R) 苯基甘氨酸,采用非对称合成方法制备了3,5 二硝基苯甲酰 (R) 苯基甘氨酸手性固定相(DNB PGCPS),利用它直接拆分了丙卡特罗药物的部分对映体,取得了良好的拆分效果。以不同比例的异丙醇 正己烷(体积比分别为20∶80,10∶90,5∶95,2∶98)为流动相,对丙卡特罗进行了拆分,其分离因子α的范围为1 54～1 67。此外,还测试了不同流动相组成对分离效果的影响,考察了液固吸附色谱保留值方程lnk=a+cCb+blnCb中保留因子k和分离因子α与强极性洗脱剂组分b的浓度Cb的关系,对拆分机理进行了讨论。更多还原

【Abstract】 A chiral stationary phase (CSP) 3,5dinitrobenzoylphenylglycine (DNBPG) for liquid chromatographic separation of procaterol enantiomers was prepared by asymmetric synthesis using (R)phenylglycine and 3,5dinitrobenzoyl. DNBPG was covalently bonded to 3aminopropyltriethoxysilane silica. Direct enantiomeric resolution of procaterol hydrochloride was achieved with satisfactory results. The effect of 2propanol contents in the mobile phase on the resolution was determined experimentally. The separation factors obtained were between 154-167 when using different mobile phase compositions of 2propanolhexane (20∶80, 10∶90, 5∶95, 2∶98, v/v) at 26 ℃ and 20 mL/min. The relationship of 2propanol concentration with k and α of procaterol hydrochloride was developed in the fundamental elution equation lnk=a+cCb+blnCb. In addition, by studying the influence of the structural features of DNBPG CSP on enantioselective recognition of procaterol hydrochloride, a hypothetical chiral recognition mechanism was developed. 更多还原