大孔吸附树脂及高速逆流色谱分离纯化石榴皮中安石榴苷

Separation and Purification for Punicalagin from Pomegranate Husk by Macroporous Adsorption Resin and High-Speed Countercurrent Chromatography

为了从石榴皮中制备高纯度安石榴苷,采用大孔吸附树脂和高速逆流色谱分离纯化石榴皮中安石榴苷。响应面分析结果显示,最优纯化条件为:吸附液浓度1.0 mg/mL,吸附时间50 min,吸附流速1.0 mL/min,在此条件下,吸附率达到86.16%,各因素对吸附率影响顺序为吸附流速>吸附液浓度>吸附时间;洗脱乙醇体积分数40%,洗脱时间150 min,洗脱流速1.0 mL/min,在此条件下,洗脱率达到71.89%,各因素对洗脱率影响顺序为乙醇体积分数>洗脱流速>洗脱时间;以正丁醇-三氟乙酸-水(100︰1︰100)为溶剂体系,上相为流动相,下相为固定相,流速1.5 mL/min,转速800 r/min,可以得到纯度为90%以上的安石榴苷纯化产物。该工艺可为石榴皮综合利用提供技术参考。

In order to prepare punicalagin of high purity from pomegranate husk, macroporous adsorption resin and High- Speed Countercurrent Chromatography （HSCCC） were used to separate and purify punicalagin from pomegranate husk with the purpose of punicalagin purification. Response Surface Test results showed the optimal condition for separation and purification was the absorption reagent concentration of 1.0 mg/mL, the time of 50 min and the flow rate of 1.0 mL/min, respectively. And under this condition the adsorption rate reached to 86.16%. The most significant effective factor was flow rate, following by content while time was the least influence factor for adsorption rate. Elution rate arrived at 71.89% with condition of 40% of ethanol concentration, the time for 150 min of elution and 1.0 mL/min of flow rate. Among these, ethanol concentration was most influenced factor for elution, followed by elution time and flow rate ranked the last position. Solvent system was consisted of N-butanol, trifluoroacetic acid and water with rates of 100 ： 1 ： 100. The punicalagin with purity of over 90% was achieved with the flow rate of 1.5 mL/min, the speed of 800 r/min, upper phase as mobile phase and lower phase as stationary ohase. This technology provided a reference for comprehensive utilization of pomegranate husk.