[Objectives] To establish the high performance liquid chromatography( HPLC) determination method for oxysophocarpine and optimize the extraction and purification technology of oxysophocarpine from Sophora alopecuroide...[Objectives] To establish the high performance liquid chromatography( HPLC) determination method for oxysophocarpine and optimize the extraction and purification technology of oxysophocarpine from Sophora alopecuroides by inverse three-phase membrane cycle.[Methods]Based on the single-factor experiment,the effects of aqueous phase and organic phase volume ratio,the concentration of sodium hydroxide,concentration of hydrochloric acid and extraction cycle time on extraction process of oxysophocarpine were investigated using orthogonal design method,to determine the optimal extraction process. [Results]The oxysophocarpine was determined by Shim-pack VP-ODS chromatographic column( 4. 6 mm × 250 mm,5 μm),mobile phase was methanol-0. 2% phosphoric acid aqueous solution( 7∶ 93),gradient elution,flow rate was 1 m L/min,the sample size was 5 μm,column temperature was 30℃,detection wavelength was 221 nm. Aqueous phase and organic phase volume ratio was 1∶ 1,hydrochloric acid concentration was 0. 3 mol/L,sodium hydroxide concentration was 0. 75 mol/L,water pump flow rate was 6 m L/min,60 min cycle time. The extraction rate of oxysophocarpine 98. 21 % within 60 min under the best experimental conditions. Oxysophocarpine has good linearity relationship within the range of 0. 01-0. 7 mg/m L( r^2= 0. 9978,n = 6),the respective average recovery rate was 97. 47%( RSD = 1. 95%). [Conclusions] This extraction process is simple in operation,the organic solvent has low consumption,and can be used for extraction of alkaloid.展开更多
文摘目的优化逆三相膜萃取烟叶中烟碱的提取工艺。方法采用聚四氟乙烯膜(PTFE)作为萃取膜,硫酸溶液作为酸相、氢氧化钠溶液作为碱相、氯仿作为有机相的逆三相膜萃取循环系统萃取烟碱叶中烟碱。依据烟碱在261 nm处有特征吸收,采用紫外分光光度计检测烟碱叶中游离烟碱的含量。以烟碱萃取率为指标,考察酸浓度、碱浓度、循环时间、酸碱水相及有机相体积比和流速5个因素,选定最佳工艺。结果提取烟叶中烟碱的最佳提取工艺条件为:酸浓度0.01%,碱浓度5%,循环时间25 min,体积比(酸碱相∶有机相)2.5∶1,流速6 m L/min,烟碱的提取率达到99.07%。对正交试验数据进行统计分析,差异有统计学意义(P<0.05)。按最佳工艺进行3次重复实验,结果显示烟碱提取率均值达到99.01%。结论该工艺操作简单,萃取时间快,有机溶剂的消耗量少,易实现工业化,环境污染少,适用于烟叶中烟碱的提取。
基金Supported by Project of National Natural Science Foundation(21162030)
文摘[Objectives] To establish the high performance liquid chromatography( HPLC) determination method for oxysophocarpine and optimize the extraction and purification technology of oxysophocarpine from Sophora alopecuroides by inverse three-phase membrane cycle.[Methods]Based on the single-factor experiment,the effects of aqueous phase and organic phase volume ratio,the concentration of sodium hydroxide,concentration of hydrochloric acid and extraction cycle time on extraction process of oxysophocarpine were investigated using orthogonal design method,to determine the optimal extraction process. [Results]The oxysophocarpine was determined by Shim-pack VP-ODS chromatographic column( 4. 6 mm × 250 mm,5 μm),mobile phase was methanol-0. 2% phosphoric acid aqueous solution( 7∶ 93),gradient elution,flow rate was 1 m L/min,the sample size was 5 μm,column temperature was 30℃,detection wavelength was 221 nm. Aqueous phase and organic phase volume ratio was 1∶ 1,hydrochloric acid concentration was 0. 3 mol/L,sodium hydroxide concentration was 0. 75 mol/L,water pump flow rate was 6 m L/min,60 min cycle time. The extraction rate of oxysophocarpine 98. 21 % within 60 min under the best experimental conditions. Oxysophocarpine has good linearity relationship within the range of 0. 01-0. 7 mg/m L( r^2= 0. 9978,n = 6),the respective average recovery rate was 97. 47%( RSD = 1. 95%). [Conclusions] This extraction process is simple in operation,the organic solvent has low consumption,and can be used for extraction of alkaloid.
