阴离子交换树脂对人参皂苷的吸附/洗脱特性考察及LC-MS分析  

Investigation of Adsorption and Desorption Properties of Total Ginsenosides on Anion-exchange Resins and Its LC-MS Analysis

作　　者：伍法杰 孙琳 赵媚 邱智东[1] 王伟楠[1] WU Fa-jie;SUN Lin;ZHAO Mei;QIU Zhi-dong;WANG Wei-nan(Changchun University of Chinese Medicine,Changchun 130117,China)

机构地区：[1]长春中医药大学,长春130117

出　　处：《中国实验方剂学杂志》2021年第13期127-136,共10页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家自然科学基金项目(81703643,81973712);吉林省教育厅项目(JJKH20181264KJ)。

摘　　要：目的:比较不同阴离子交换树脂对人参总皂苷的吸附和洗脱性能,阐明其吸附/洗脱机制,建立适合人参总皂苷纯化的阴离子交换树脂方法。方法:以比吸附量、比洗脱量、洗脱率和回收率为指标,考察5种大孔树脂(D301,D315,D312,D330,D201)的吸附/洗脱特性。利用拟一级、拟二级动力学模型,以及Langmuir和Freundlich等温吸附模型对优选树脂和D101型大孔树脂的吸附动力学和热力学过程进行研究,阐明阴离子交换树脂与常规大孔树脂之间的吸附机制差异。通过动态吸附/洗脱试验优选阴离子交换树脂柱色谱纯化工艺参数并进行验证试验,通过液质联用法(LC-MS)对纯化前后9种单体人参皂苷类成分进行定性和定量分析。结果:D301型阴离子交换树脂明显优于其他4种阴离子交换树脂,最佳工艺条件为上样液pH 8,上样体积2 BV,上样流速4 BV·h^(-1),用水和20%乙醇各3 BV洗脱杂质,加80%乙醇8 BV洗脱,洗脱流速4 BV·h^(-1)。经D301型树脂纯化后,9种单体人参皂苷类成分的富集系数均得到了不同程度的提高,整体富集系数达5.3,整体回收率80.9%,人参总皂苷纯度也从粗提物的17.07%提高至91.19%。结论:D301型阴离子交换树脂纯化人参总皂苷的方法简便可行,实现了从人参药材中一维柱色谱富集高纯度人参总皂苷的目的。Objective:To compare the adsorption and desorption properties of different anion exchange resins for total ginsenosides,clarify their adsorption/desorption mechanism,and establish a simple protocol for the purification of total ginsenosides.Method:The adsorption and desorption properties of five different resins(D301,D315,D312,D330,D201)on total ginsenosides were evaluated with specific adsorption capacity,specific desorption capacity,desorption rate and recovery rate as indices.The adsorption kinetics and thermodynamics of the selected resin and D101 macroporous resin were investigated by pseudo-first-order and pseudo-second-order kinetic models,as well as Langmuir and Freundlich isothermal adsorption models,and the differences of adsorption mechanism between anion exchange resin and conventional macroporous resin were elucidated.The dynamic adsorption and desorption experiments were used to determine the optimum chromatographic parameters for anion exchange resin.After verifying the purification process of total ginsenosides,nine individual ginsenosides were qualitatively and quantitatively analyzed by liquid chromatography-mass spectrometry(LC-MS).Result:D301 anion exchange resin was obviously superior to the other four kinds of anion exchange resin,the optimum parameters were set as follows:pH 8 of loading solution,loading volume of 2 BV,loading speed of 4 BV·h^(-1),eluted with 3 BV of water and 20%ethanol for the impurities,eluted with 8 BV of 80%ethanol with elution speed of 4 BV·h^(-1).After purified by D301 resin,the enrichment coefficients of 9 monomer ginsenosides were simultaneously increased to different degrees,the overall enrichment coefficient was up to 5.3,the recovery rate for the total amount of these ginsenosides was calculated to be 80.9%,and the purity of total ginsenosides in Ginseng Radix et Rhizoma extract increased from17.07%to 91.19%.Conclusion:D301 anion exchange resin is suitable for rapid and practical purification of total ginsenosides,hence allowing for the enrichment of high-puri

关 键 词：阴离子交换树脂 人参皂苷 吸附性能 洗脱特性 柱色谱 液质联用(LC-MS) 大孔树脂 

分 类 号：R943[医药卫生—药剂学] O657[医药卫生—药学]