天山堇菜秦皮乙素大孔树脂分离纯化工艺优化

Optimization on separation and purification process of esculetin from Viola tianshanica Maxim by macroporous resin

通过静态吸附与解吸附试验,从8种大孔树脂中筛选出适合纯化天山堇菜秦皮乙素的树脂,并进行吸附性能的研究。结果表明,HPD500树脂对天山堇菜秦皮乙素具有良好的吸附效果,其吸附动力学可用拟二级动力学方程描述,不同温度下的等温吸附可用Freundlich方程很好地拟合,其吸附的自由能变△G、焓变△H和熵变△S均<0,吸附过程是一个自发、放热的物理行为。最佳纯化工艺条件为上样浓度2.5935mg/mL,最大上样量7.7805mg/g·树脂,上样流速2.0mL/min,除杂用水量7BV,50%乙醇洗脱,洗脱剂用量7BV,洗脱流速2.0mL/min。该条件下,秦皮乙素纯度达到37%,回收率达到93%。

The resin suitable for the purification of esculetin from Viola tianshanica Maxim was selected from eight macroporous resins by static adsorption and desorption experiments, and its kinetics and thermodynamics behavior on compound was studied.The result indicated that HPD500 was the optimum material for the adsorption of esculetin.The adsorption dynamic behavior was well described by the pseudo-second-order kinetics equation.The adsorption isotherm data from the thermodynamics behavior were fitted better with Freundlich equation.The thermodynamic parameters were found to be Δ H <0,Δ S <0, and Δ G <0 respectively, so this adsorbing process was a spontaneous exothermic process.The optimal purification conditions of HPD500 on esculetin were as follows: loading concentration 2.593 5 mg/mL, maximum loading adsorption capacity 7.780 5 mg/g resin, adsorption rate 2.0 mL/min, 7 BV deimpurity water, 7 BV 50% ethanol elution, elution rate 2.0 mL/min.Under these conditions, the purity of esculetin was greater than 37% and the recovery rate was greater than 93.0%.