咪唑立宾结晶工艺研究

Crystallization Process of Mizoribine

对咪唑立宾的结晶工艺进行优化,探究了抗溶剂种类、溶液初始浓度、抗溶剂滴加速度及抗溶剂加量对咪唑立宾结晶纯度、堆密度、收率和产品稳定性的影响。确定最佳结晶工艺为:以乙醇为抗溶剂、溶液初始浓度0.7 g·mL^-1、抗溶剂滴加速度5 BV·h^-1、抗溶剂加量为咪唑立宾水溶液体积的12倍(12 BV)。该结晶工艺所得产品纯度高、杂质少、堆密度较大、稳定性好,适合工业化生产,有利于长期储存和制剂分装。

We optimized the crystallization process of Mizoribine,and investigated the effects of anti-solvent types,initial concentration of solution,dropping rate of anti-solvent,and anti-solvent dosage on the purity,bulk density,yield,and stability of Mizoribine crystal.The optimal crystallization process is determined as follows:ethanol is used as the anti-solvent,the initial concentration of solution is 0.7 g·mL^-1,the dropping rate of anti-solvent is 5 BV·h^-1,and the anti-solvent dosage is 12 times(12 BV)the volume of Mizoribine aqueous solution.The obtained product has high purity,low impurity,large bulk density,and good stability,and this crystallization process is suitable for industrial production and is beneficial to long-term storage and preparation packaging.