Studies On The Separation And Purification Of SQS (Sasanquasaponin)

This dissertation studies the separation and purification of SQS based on the previous researching.Four parts divided in this thesis are as follows:Partâ… :To establish a preparative method for total oil tea saponins as reference substance from the seeds of Camellia Oleiferal Abel.by dry column chromatography.After raw material being extracted with 60%ethanol,the ethanol extracts were evaporated to alcoholess in vacuum.And the solution was extracted by petroleum benzine.Then taking off the upper solution,and adding three times volume of BuOH for extracting,and this time the upper solution was evaporated to dryness in vacuum.The dry powder was fractionated by dry column chromatography on silica gel(100～200 mesh)using the upper solution of EtOAc-MeOH-BuOH-H₂O(3:2:5:10)as the eluent.The collected fraction was taken out by the Rf value,and then put the fraction into glass column to collecting the solution by using MeOH as eluent.After evaporating MeOH with the solution to get the total oil tea-saponins,and detecting the saponins by TLC(Thin-layer chromatography)and physical & chemical properties.The purity of the product quantized by TLC was over 98%. Therefore,the developed method is simple,rapid and the quantity of oil tea saponins also is more than normal preparation methods.All the results showed that the preparation substance of all the oil-tea saponins should be as reference substance.Partâ…¡:Used the HPLC(High Performance Liquid Chromatography)and HPLC-MS (Mass Spectrometry)-ESI(Electronic Spray Ionization)to separate and analysis the sasanquasaponin which got from the dry column chromatography.Through the chromatogram of HPLC and the spectrometry of ESI,as a result,the sasanquasaponin was a mixture which might be containing two or three Mono-glycosides.And the molecular weight of the sasanquasaponin was from 800～1200 Dalton,which in accord with the literatures.Partâ…¢:Used the ceramic membrane to remove the residues of crude extracts from the cake of C.Oleifera Abel.Seeds for improving the product and purity of the sasanquasaponin.The ultrasonic extraction with the alcohol of 50%was treated by the membrane of 0.5μm pores,the feed concentration was3%(w/v),the operation pressure was about 0.1 Mpa～0.15 Mpa,and the temperature was about 40℃.Under those conditions,we acquired a better conclusion that the metastasis rate of the total sasanquasaponin was about 89.25%,and the elimination rate was about 14.5%.Also the permeation liquid of the micro-filtration was clarification,so the ceramic membrane was a promising field in the pretreatment of the crude extraction of the sasanquasaponin and a possibility in the Industrialization.Partâ…£:Selected a special Granular activated carbon to purify sasanquasaponin.Using the production & purity as index of examination through all the experiments.And the Vanillin-H₂SO₄ colorimetry was used to analyze the content of total saponins,and the adsorption performance and the elution parameters and the regeneration were investigated. The results showed that the effect of 90%ethanol with a flow rate of 1.0 BV/h was better; and the elution ratio of sasanquasaponin was 92.4%including water elution.And the recovery of the saponins was 62.9%without water elution,the purity of saponins was more than 87.1%.As a result,this Granular activated carbon can be used to refine the sasanquasaponin in the cake of C.Oleifera Abel.Seeds for its simple application process, low price and so on.