Enantioselective extraction of clorprenaline enantiomers with hydrophilic selector of sulfobutylether-β-cyclodextrin by experimentand modeling简

Enantioselective extraction of hydrophobic clorprenaline （CPE） enantiomers from organic phase to aqueous phases with sulfobutylether-β-cyclodextrin （SBE-β-CD） as the selector was investigated with insight into a number of important process variables, such as the type of organic solvent, concentration of selector, pH, and temperature. Equilibrium of the extraction system was modeled using a reactive extraction modcl with a homogeneous aqueous phase reaction. The important parameters of this model were determined experimentally. The physical distribution coefficients for molecular and ionic CPE were determined as 0.3 and 8.93, respectively. The equilibrium constants of the complexation reaction with SBE-β-CD were determined as 152 and 110 L/mol for R- and S-CPE, respectively. Results show that the experimental data agree with the model predictions perfectly. Comprehensively considering the experiment and model, the extraction conditions are optimized and the best extraction conditions are： pH of 6.0, SBE-β-CD concentration of 0.04 tool/L, and temperature of 5 ℃, providing the enantioselectivity （a） of 1.25, the fraction of R-CPE （φR） in aqueous phase of 0.71 and performance factor （pf） of 0.025.     

均苯四甲酸酐修饰β-环糊精微球电色谱柱的制备及应用

合成了均苯四甲酸酐修饰β-环糊精微球,通过红外光谱、X-射线光电子能谱、扫描电镜对其进行结构和形貌表征,获得了大小均匀、表面光滑、粒径为5~10μm的微球。以该微球为手性固定相,采用溶胶-凝胶法制备了颗粒固定化整体柱,并考察了柱制备过程中的影响因素,获得最佳的柱制备条件:聚乙二醇∶冰乙酸∶正硅酸甲酯为0.25 g∶2.5 m L∶1.5 m L,溶胶∶微球为2 m L∶1 g,水浴时间10 h,水浴温度40℃。利用该颗粒固定化整体柱对盐酸异丙肾上腺素和盐酸氯丙那林对映体进行手性拆分,达到了基线分离。     

基于PCA-SVMR快速测定复方氯丙那林和对乙酰氨基酚

基于主成分分析-支持向量机回归(PCA-SVMR)方法,利用近红外光谱技术研究了复方氯丙那林和复方对乙酰氨基酚两种模型制剂有效组分的快速同时测定,建立了它们的多元校正模型,并以传统的稳健方法偏最小二乘回归(PLSR)为基础考察了PCA-SVMR方法对于小样本药物体系的拟合能力、预测能力和模型稳定性。研究表明,PLSR的预测能力必须以强拟合能力为前提,PCA-SVMR则没有这样的要求,使前者对校正样本的依赖性远强于后者,从而在小样本药物体系中前者的稳定性大大弱于后者,该两种药物制剂的PCA-SVMR多元校正模型的测定准确度总体上优于PLSR。     

Kinetic study on reactive extraction of clorprenaline enantiomers with a combined chiral selector

This paper reports on the kinetic study on reactive extraction of clorprenaline (CPNL) enantiomers with isobutyl (d)-tartrate (DT) and boric acid (BA) as combined chiral selector in a Lewis cell, where exists an interfacial reaction involving three species: BA, DT, and CPNL enantiomers. The important factors that influence the kinetics of reactive extraction are investigated. Through multiple linear regression analysis of the experimental data, the order with respect to BA, CPNL, and DT of the interfacial reaction is 0.6, 0.8, and 0.8, respectively, and the total order of reaction is about 2.2. The forward rate constants have been calculated to be 2.476 × 10^–4 L^1.53/(mol^1.2 s) for (R)-CPNL and 1.349 × 10^–4 L^1.53/(mol^1.2 s) for (S)-CPNL.