摘要
目的:优选大黄总蒽醌提取物的大孔树脂纯化工艺。方法:采用静态吸附和动态吸附考察相结合的方法,以大黄总蒽醌为指标筛选8种不同性质的大孔吸附树脂,通过考察上样液pH、上样量、流速、径高比、除杂溶剂种类和用量、洗脱溶剂种类和用量等因素,优选大黄总蒽醌提取物的纯化工艺条件。结果:大黄总蒽醌提取物的最佳纯化工艺条件:制备浓度为0.2 g生药/mL、pH=9的大黄上样液,湿法装柱径高比约为1∶5的D101大孔吸附树脂,以1 BV/h的速度上样约1.5 BV,以2 BV/h的速度上样约5 BV的0.1 mol/L NaOH溶液除杂,以2 BV/h的速度上样约10 BV的0.4 mol/L HCl的85%乙醇溶液进行洗脱,从洗脱剂加入开始接取洗脱流出液,舍去前1.5 BV后正式开始收集,70℃下真空干燥24 h。纯化后得到的原料药中大黄总蒽醌纯度能达到50%以上,大黄中5种游离蒽醌单体的纯度平均值分别约为10.02%、2.45%、19.31%、11.15%、4.72%,大黄中5种游离蒽醌单体之和占总蒽醌比例高达93.45%。结论:D101型大孔树脂可用于大黄总蒽醌的纯化研究,优选出的纯化工艺稳定可行,可作为大黄总蒽醌的纯化工艺条件。
Objective:To optimize purification process of the total anthraquinones in Radix et Rhizoma Rhei extract.Methods:By using the method of the combination of static adsorption and dynamic absorption,the final purity of total anthraquinones as indexes,we selected 8 different properties of the macroporous resin.Through the study of the pH of sample,sample volume,flow rate,ratio of diameter to height,impurity removing solvent,elution solvent and other factors,we determined the final preliminary establishment of purification process of total anthraquinones.Results:Optimal purification conditions were as following:the drug solution concentration was 0.2 g of medicinal material/mL,pH=9,D101 macroporous adsorption resin with diameter height ratio of about 1:5 was loaded by wet method.At a speed of 1 BV/h sample was about 1.5 BV,5 BV of 0.1 mol/L sodium hydroxide purified water eluted resin column to removed impurities,the flow rate was 2 BV/h,10 BV of 0.4 mol/L hydrochloric acid 85%ethanol as eluent.2 BV/h flow rate washing resin column,eluate eluate was taken from the beginning of the eluent addition,discard 1.5 BV before formal collection,collecting the eluted liquid.Then with the temperature of 70 vacuum concentration and 70℃vacuum drying for 24 h to obtain the total anthraquinones of Rhubarb extract.After purification,the purity of rhubarb anthraquinone could reach more than 50%,the five kinds of free anthraquinones monomer purity were 10.02%,2.45%,19.31%,11.15%,4.72%,respectively.The sum of five free anthraquinone monomer for the proportion of total anthraquinone in Radix et Rhizoma Rhei as high as 93.45%.Conclusion:The optimized purification process is stable and feasible,and has a good application prospect.
作者
陈俊沲
余平
李晶晶
万浩芳
石森林
CHEN Junduo;YU Ping;LI Jingjing;WAN Haofang;SHI Senlin(College of Pharmaceutical Sciences,Zhejiang Chinese Medical University,Hangzhou 310053,China;Tongde Hospital of Zhejiang Province,Hangzhou 310012,China;Zhejiang Heze Pharmaceutical Technology Co.,Ltd.,Hangzhou 311199,China)
出处
《中华中医药杂志》
CSCD
北大核心
2023年第12期6039-6045,共7页
China Journal of Traditional Chinese Medicine and Pharmacy
基金
浙江省基础公益研究计划项目(No.LGF20H280004)。
关键词
大黄
总蒽醌
大孔树脂
纯化工艺
动态吸附
静态吸附
Radix et Rhizoma Rhei
Total anthraquinones
Macroporous resin
Purification process
Dynamic absorption
Staticabsorption
