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大孔吸附树脂分离纯化赤雹根总皂苷的工艺研究
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篇名: 大孔吸附树脂分离纯化赤雹根总皂苷的工艺研究
TITLE:
摘要: 目的:考察大孔吸附树脂分离纯化赤雹根总皂苷(TSTR)的工艺。方法:采用紫外-可见分光光度法测定TSTR含量。通过比较不同型号(AB-8、D101、DM130、HPD100、HPD300、HPD450、HPD600、HPD826、NKA-9)大孔吸附树脂的静态吸附、解吸性能,筛选大孔吸附树脂型号;以TSTR含量为指标,考察大孔吸附树脂对TSTR吸附的影响因素(树脂径高比、药液质量浓度、吸附体积流量、饱和吸附量)、解吸的影响因素(解吸溶剂体积分数、解吸溶剂体积流量、解吸溶剂体积),筛选最优工艺条件并进行验证及TSTR的纯化制备。结果:以HPD100型大孔吸附树脂对TSTR的吸附和解吸性能较佳;吸附的最优工艺条件为树脂柱径高比  1 ∶ 5、药液质量浓度1 g/mL、吸附体积流量1 BV/h、饱和吸附量为1.25 g生药/1 g HPD100树脂;解吸的最优工艺条件为解吸溶剂乙醇体积分数75%、解吸体积流量3 BV/h、解吸溶剂体积5 BV;验证工艺中TSTR的平均解吸保留率为77.96%(RSD=0.46%,n=3),最终所制备的TSTR干膏中TSTR的纯度为52.47%(RSD=1.53%,n=3)。结论:该优选纯化工艺稳定可行,可用于TSTR的分离纯化。
ABSTRACT: OBJECTIVE: To investigate the separation and purification technology of total saponins from the root of Thladian- tha dubia (TSTR). METHODS: The content of TSTR was determined by UV-visible spectrophotometry. By comparing static adsorption and desorption properties of different types (AB-8, D101, DM130, HPD100, HPD300, HPD450, HPD600, HPD826, NKA-9) of macroporous adsorption resin, the type of macroporous adsorption resin was screened. With the content of TSTR as the index, influential factors of macroporous adsorption resin for adsorbing (ratio of height to diameter of resin, mass concentration of medicine liquid, adsorption volume flow, saturated extent of adsorption) and desorbing (desorption solvent volume fraction, desorption solvent volume flow, volume of desorbed solvent) TSTR were investigated. The optimal technology was screened. The technology validation, purification and preparation were conducted. RESULTS: HPD100 type macroporous adsorption resin had good adsorption and desorption properties for TSTR. The optimal adsorption technology was that the ratio of the height to diameter of the resin column was 1 ∶ 5; mass concentration of medicine liquid was 1 g/mL; adsorption volume flow rate was 1 BV/h; saturated adsorption capacity was 1.25 g per 1 g HPD100 resin; the optimal desorption technology was that the volume fraction of desorption solvent ethanol was 75%; volume flow rate of desorption was 3 BV/h; the volume of desorption solvent was 5 BV. The average desorption retention rate of TSTR was 77.96% in technology validation (RSD=0.46%, n=3) and the purity of prepared TSTR in TSTR dry cream was 52.47% (RSD=1.53%, n=3). CONCLUSIONS: The optimal purification technology is stable, feasible and suitable for the separation and purification of TSTR.
期刊: 2018年第29卷第3期
编辑: 聂佳,李忠思,佟继铭,刘春楠,刘克明,刘永平
AUTHORS: NIE Jia,LI Zhongsi,TONG Jiming,LIU Chunnan,LIU Keming,LIU Yongping
关键字: 大孔吸附树脂;分离;纯化;赤雹根;总皂苷
KEYWORDS: Macroporous adsorption resin; Separation; Purification; Root of Thladiantha dubia; Total saponins
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