大孔吸附树脂分离纯化湿生扁蕾总[口山]酮  

Separation and Purification of Total Xanthones from Gentianopsis paludosa Using Macroporous Adsorption Resin

作　　者：寇亮 刘越敏 柳娜 曲馨 薄双琴 景明 KOU Liang;LIU Yuemin;LIU Na;QU Xin;BO Shuangqin;JING Ming(College of Pharmacy,Gansu University of Chinese Medicine,Lanzhou 730000 Gansu,China)

机构地区：[1]甘肃中医药大学药学院,甘肃兰州730000

出　　处：《中药新药与临床药理》2022年第4期522-530,共9页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：国家自然科学基金资助项目(81860788,81560717);兰州市人才创新创业项目(2019-RC-1017)。

摘　　要：目的建立湿生扁蕾总[口山]酮的含量测定方法,通过大孔吸附树脂分离纯化湿生扁蕾总[口山]酮。方法采用ZrOCl_(2)比色法测定湿生扁蕾中总[口山]酮含量,并对该法进行方法学验证。通过静态吸附及解吸试验,优选出最佳树脂。以优选大孔吸附树脂为固定相,通过吸附动力学、热力学探讨其吸附机理,并优化分离纯化工艺。结果建立的湿生扁蕾总[口山]酮的含量测定方法精密度和准确度较好。所优选的大孔吸附树脂为DM130型树脂,吸附过程可以用准二级动力学、颗粒扩散动力学、Langmuir和Freundlich模型较好地解释,该过程为自发的、吸热的、熵增的吸附过程。分离纯化湿生扁蕾总[口山]酮的较优工艺为:上样液质量浓度1.5 mg·mL^(-1),洗脱剂为体积分数80%的乙醇,上样液pH为5,洗脱剂用量为10倍柱体积(BV),洗脱剂流速为2 BV·h^(-1)。按优化工艺分离纯化后,湿生扁蕾总[口山]酮含量由13.39%提高到51.26%。结论所建立的总[口山]酮含量测定方法操作简便,精密度和准确度良好,可用于湿生扁蕾提取物中总[口山]酮的含量测定。DM130大孔吸附树脂可有效分离纯化湿生扁蕾总[口山]酮,优化后的分离纯化工艺条件稳定可行,纯化效率较高。Objective To establish a method for the content determination of total xanthones from Gentianopsis paludosa,and to optimize the separation and purification process of total xanthones from Gentianopsis paludosa using macroporous adsorption resin. Methods The ZrOCl_(2) colorimetric method was used to determine the content of total xanthones from Gentianopsis paludosa, and the method was validated. The most suitable macroporous adsorption resin was selected by static adsorption and desorption tests. Using the optimal macroporous adsorption resin as the stationary phase,the adsorption mechanism was discussed through the adsorption kinetics and thermodynamics,and the separation and purification process was optimized. Results The established method for the determination of total xanthones from Gentianopsis paludosa was precise and accurate. The optimal macroporous adsorption resin was DM130 resin. The adsorption process could be well explained by pseudo-second-order kinetics,particle diffusion kinetics,Langmuir and Freundlich models,and the process was a spontaneous,endothermic,entropy-increasing adsorption process. The optimized processes for the separation and purification of total xanthones from Gentianopsis paludosa were as followed:the mass concentration of loading liquid was 1.5 mg·mL^(-1),the eluent was 80% ethanol(V/V),the pH value of the sample liquid was 5,the volumes of eluent were 10 BV,and the flow rate of eluent was 2 BV·h;. After separation and purification according to the optimized process,content of the total xanthones from Gentianopsis paludosa increased from 13.39% to 51.26%. Conclusion The established method for the content determination of total xanthones was easy to operate, with good precision and accuracy. It can be used for the determination of total xanthones content from Gentianopsis paludosa extracts. DM130 macroporous adsorption resin could effectively separate and purify the total xanthones from Gentianopsis paludosa. The optimized conditions of separation and purification process were

关 键 词：湿生扁蕾 总(口山)酮 含量测定 大孔吸附树脂 分离 纯化 工艺优化 

分 类 号：R284.2[医药卫生—中药学]