回流辅助的双水相体系提取防己中粉防己碱

Aqueous two-phase system coupled with heat reflux for the extraction of tetrandrine from Stephania tetrandra S. Moore

目的:改进粉防己碱的提取分离工艺,减少环境污染,降低生产成本。方法:采用乙醇/(NH4)2SO4双水相体系,辅以加热回流,提取并分离纯化防己粉末中粉防己碱,考察了乙醇质量分数、(NH4)2SO4体积分数、料液比、pH、回流时间和提取次数等因素对粉防己碱萃取率的影响,并建立高效液相色谱法测定萃取液中粉防己碱含量的分析方法。结果:在乙醇质量分数为20%、(NH4)2SO4体积分数为35%、料液比为1∶8、pH为9时,双水相萃取率为84.50%;回流提取1次、时间为2 h时,防己粗提物的得率为19.80 mg/g,纯度为20.30%。结论:本方法相比于传统提取分离方法如乙醇回流提取以及酸碱法等,操作简便、萃取率高、方法重复性好,所得粗提物纯度较高,可适用于提取粉防己碱。

Objective： To improve the method of extraction and separation of tetrandrine from Stephania tetrandra S.Moore in order to reduce environment pollution and cut down the cost of production.Methods： The ethanol /（NH4） 2SO4 as a two aqueous phase system for the extraction and separation of tetrandrine was studied.The effect of operating parameters,including the concentration of ethanol and（NH4） 2SO4,pH and temperature on extraction was studied in depth.Results： The extraction rate of tetrandrine in the aqueous two phase system could reach 84.50%.The ratio of solid： solvent was 1 ∶ 8,the time of heat reflux were 2 h,the salinity of（NH4） 2SO4 was 35%,the density of ethanol was 20%（w,%）,the pH level was 9,accordingly.The purity and yield of tetrandrine crude were 20.30% and 19.80 mg / g accordingly after recycling ethanol.Conclusion： The method of aqueous two phases could be applied to extraction and separation of tetrandrine in industry due to conveniently of procedure,highly of extraction rate and repeatability.