基于山苍子核油的高纯度月桂酸的制备

以山苍子核油为原料,经酸炼、皂化酸化水解、减压精馏及混合溶剂结晶纯化工艺分离制备高纯度月桂酸,并采用单因素实验和正交实验优化了溶剂结晶纯化月桂酸的工艺。得到的最优溶剂结晶纯化工艺条件为:料液比1∶2∶10(m第二馏分∶V95%乙醇∶V正己烷),结晶时间4 h,结晶温度-17.5℃。在最优工艺条件下,月桂酸的纯度达到98%以上。该组合工艺具有条件温和、产品纯度高及溶剂易回收再利用等优点,适合于山苍子核油的深度开发利用。

Effect of Mixed Solvents and Additives on the Habit Modification of 6-APA Crystals

6-aminopenicillanic acid (6-APA) crystals obtained under different physical and chemical conditions of the solutions may present different habits. The habits of diamond-shaped plates are desirable compared with other habits of 6-APA crystals. To obtain ideal 6-APA crystals, the effects of the mixed solvents and additives on 6-APA crystal habits were investigated. Ethanol or acetone was used as the organic solvent, and impurities existing in the 6-APA purification process were used as the additives. 6-APA growth habits were changed when the concentrations of ethanol, acetone or phenyl acetic acid were increased to exceed their critical concentration. The observed results show that the dominant face on 6-APA crystals was identified to be {020}, but the overall habit was controlled by the relative growth rates of the {101} and {002} faces. Crystal growth rates and habits can be appreciably changed by specific adsorption of additives on crystal faces.In some cases solvent molecules can act in a similar way and may be regarded as bulk additives. The effects of additives and organic solvents on 6-APA crystal habits were the results of adsorption effect, which fitted the experimental results quite well.

吡罗昔康-苯甲酸共晶的制备与体外释放研究

目的:本实验采用共晶技术制备难溶性药物吡罗昔康的共晶物,以期提高难溶性药物的溶解度和溶出度。方法:采用混合溶剂结晶法制备了吡罗昔康共晶,采用差示扫描量热分析(DSC)、高效液相色谱(HPLC)及X射线粉末衍射(XRPD)对制备得到的产品进行表征,并对共晶物的粒径、稳定性和体外释放等性质进行了考察。结果:吡罗昔康与苯甲酸之间形成了共晶物。形成的共晶物粒径分布均匀、晶体性质稳定。同时提高了吡罗昔康的溶解度并改善其体外释放性质。结论:共晶技术在提高难溶性药物溶解度和溶出度方面具有广阔的应用前景。