Study On Preparation Process And Quality Standard Of Gynostemma Total Saponins

Objective:The purpose of this project is to compare the quality difference of Gynostemma pentaphyllum from different places of origin;To design a lowcost preparation process for Gynostemma total saponins raw materials;To conduct a pilot scale-up validation of the preparation process of the Gynostemma total saponins;And to establish the determination of the marker components in Gynostemma total saponins.Methods and develop quality standards.Method:Taking the Gynostemma total saponins(measured by Gypenoside A)as the evaluation index,quality evaluation was performed on multiple batches of Gynostemma pentaphyllum from three different producing areas of Guangxi,Yunnan,and Shaanxi.Ultraviolet spectrophotometry was used to compare and determine Gynostemma pentaphyllum in each medicinal material.The content of total saponins;comparing various extraction methods,the dry paste rate and transfer rate of Gynostemma total saponins in crude extracts were used as evaluation indicators,and the best extraction method was selected.The single factor test was used to examine the amount of extraction solvent,extraction time,degree of crushed herbs,determine the best extraction conditions and parameters;single factor test was used to examine the adsorption rate and elution rate of the crude extract over the D101 macroporous resin,and to investigate the best adsorption and The elution conditions were determined to determine the process conditions and parameters for purification of Gynostemma total saponins from macroporous adsorption resin;the preparation process was scaled up and validated to determine the feasibility of large-scale industrial production;this subject used ultraviolet spectrophotometry to determine the total saponin content of Gynostemma pentaphyllum,The content of Gypenoside A and Gypenoside XVII was determined by HPLC simultaneously.The quality of the Gynostemma total saponin raw materials was evaluated by combining the two,and the quality standard of Gynostemma total saponin raw materials was established on the basis of technological research and quality research.Result:The best quality of Shaanxi medicinal materials was selected from different producing areas,so Shaanxi was selected as the origin of the medicinal materials;the best preparation process route has been determined through small-scale experiments: Crude herbs from Shaanxi Gynostemma pentaphyllum were crushed to No.2 sieve.Powder,50 times the amount of 0.1% NaOH solution,add the appropriate amount of solvent to make the medicine fully wetted,into the infiltration device,dipping for 8 hours,began to infiltrate(permeation time 16 h to complete),collect percolation fluid,with 1.2 Mol/L hydrochloric acid adjusts the permeation fluid to neutrality as the sample fluid.The sample solution was passed through a D101 macroporous resin column,and the ratio of the medicinal material to the macroporous resin was 1:2.5.After the adsorption was completed,the macroporous resin column was eluted with 4 BV purified water(BV is the volume of the resin bed),and finally 2.8 BV of 90% ethanol was used as an elution.The agent is eluted at an elution rate of 1 BV/h,the eluent is collected,the eluent is concentrated and dried,and ethanol is recovered to obtain the Gynostemma total saponin raw material;the preparation process is subjected to a pilot scale-up verification,and the average of the obtained three batches of Gynostemma total saponins is greater than 85.03% The average yield is 5.56%,indicating that the preparation process is stable and reliable,and it can be used in industrial production.By supplementing the original Gynostemma total saponin quality standard,the use of high performance liquid chromatography for the determination of gypenoside A and gypenoside XVII monomer has been added.The content of the constituents is verified by the analytical method of the method,and the verification result meets the requirements.Conclusion:In this study,the method of extraction,enrichment,purification and quality control of Gynostemma pentaphyllum was established.According to the actual production demand of Gynostemma process,not only the related problems in the process of Gynostemma pentaphyllum were solved,but also a low industrialization cost,saponin yield High,high purity,low energy consumption and the best production technology,The quality of Gypenoside is evaluated by controlling the total Gynostemma total saponins and Gynostemma saponin monomers,and the quality standard of Gynostemma total saponins is established.