模拟移动床色谱法分离纯化链甾醇

Separation and Purification of Desmosterol by Simulated Moving Bed Chromatography

以羊毛脂中提取的链甾醇为原料,采用模拟移动床色谱法(SMBC)进行了分离纯化。以C18为固定相,甲醇为洗脱液,采用四区SMBC系统,每区有两根色谱柱(150 mm×10 mm×10μm),经过两次SMBC分离,得到高纯度链甾醇产品。以纯度、生产率和溶剂消耗量为指标,确定链甾醇在SMBC中的最佳分离条件为:切换时间6.4 min,四区流量分别为9.97,7.53,8.53和4.97 mL/min,进料流量1.00 mL/min(第一次SMBC分离);切换时间6.0 min,四区流量分别为9.95,7.98,8.53和6.62 mL/min,进料流量0.55 mL/min(第二次SMBC分离)。结果表明,以90.1%含量的链甾醇粗品为原料,在优化实验条件下,先除去吸附能力比链甾醇强的杂质,再除去吸附能力比链甾醇弱的杂质,得到高纯度(≥98.9%)的链甾醇产品,回收率为93.8%。

Separation and purification of crude desmosterol originated from lanolin were conducted with simulated moving bed chromatography（SMBC）.Using C18 as stationary phase,methanol as eluent,four zone SMBC system,two columns in every zone,high purity desmosterol was obtained through twice SMBC separations.The column used was 150 mm×10 mm i.d.,particle size 10 μm.Based on purity,productivity and eluent consumption,the optimal SMBC separation conditions for desmosterol were determined as follows： switch time 6.4 min;flow rate of Q1=9.97 mL/min,Q2=7.53 mL/min,Q3=8.53 mL/min,Q4=4.97 mL/min;QF=1.00 mL/min（first SMBC separation）;switch time 6.0 min;flow rate of Q1=9.95 mL/min,Q2=7.98 mL/min,Q3=8.53 mL/min,Q4=6.62 mL/min;QF=0.55 mL/min（second SMBC separation）.Under above conditions,firstly the impurity with adsorption capacity stronger than desmosterol was removed,and then the impurity with adsorption capacity weaker than desmosterol was removed.Desmosterol with more than 98.9%purity and 93.8% recovery was obtained from 90.1% purity crude desmosterol.