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Study On Immobilized Ionic Liquids And Deep Eutectic Solvents Molecularly Imprinted Separation Of Active Constituents From Acanthopanax Senticosus Efficiently

Posted on:2021-04-15Degree:MasterType:Thesis
Country:ChinaCandidate:J H LiFull Text:PDF
GTID:2404330605964548Subject:Forest Chemical Processing Engineering
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In this study,eleutheroside B1 was used as the hydrolysis target,and the acid-base catalytic ability of the ion exchange resin was used to hydrolyze the eleutheroside B1 in the extract of Acanthopanax senticosus by heating and refluxing to obtain the increase of isofraxidin.Then,the polymerization method was used to immobilize the ionic liquid on the AB-8 macroporous resin,and use it to enrich the free isofraxidin.In this study,the Acanthopanax sentcosus glycosides and isofraxidin were used as the common research object.The deep eutectic solvent and microwave magnetic field were used to extract the syringin,eleutheroside E and isofraxidin in the Acanthopanax senticosus.The three-molecule template imprinted polymer was prepared,and the extracts of syringin,eleutheroside E and isofraxidin were simultaneously adsorbed and separated in order to obtain high-purity syringin,eleutheroside E and isofraxidin.The specific research content was as follows:1.Taking eleutheroside B1 as the hydrolysis target,using basic ion exchange resin as the catalyst,the eleutheroside B1 in the extract of Acanthopanax senticosus was hydrolyzed by heating and refluxing to obtain the increase of isofraxidin.By analyzing the increment of isofraxidin obtained from the single factor experiment,the optimal experimental conditions for the screening of the hydrolysis efficiency were:D202 macroporous strong base styrene anion exchange resin as the catalyst,0.5 g(absolute dry)/100 mL of Acanthopanax Senticosus extracting solution,hydrolyzed at reflux temperature 75℃ for 4 h,the increment of free isofraxidin was 7.1717 mg/100 g,and the mechanism of ion exchange resin catalytic hydrolysis of eleutheroside B1 was explained.2.Taking isofraxidin in the hydrolysate as the research object,the ionic liquid was immobilized on the AB-8 macroporous resin by the polymerization method,and the free isofraxidin was enriched with it.The effects of different kinds of ionic liquid immobilized on resins on the adsorption capacity of isofraxidin were screened.The adsorption of 1-butyl-3-methylimidazolium hydrosulfate ionic liquid immobilized on AB-8 will have the optimal adsorption and desorption effect of isofraxidin,the adsorption conditions were static adsorption at 303 K for 2 h,the adsorption capacity was 101.2 mg/g;after elution with 75%ethanol,the purity of isofraxidin was 28.7%after purification.3.In this study,the Acanthopanax sentcosus glycosides and isofraxidin were used as the common research objects.The deep eutectic solvent and microwave magnetic field were used to extract syringin,eleutheroside E and isofraxidin in Acanthopanax senticosus.In this process,the less polar isofraxidin and the more polar eleutheroside can be extracted at the same time.Choosing deep eutectic solvent as choline chloride-ethylene glycol(1:3,5:5 v/v),extraction solid-liquid ratio 1:10 g/mL,microwave time 10 min,microwave power 400 W,the contents of syringin,eleutheroside E and isofraxidin were 0.282 mg/g,1.486 mg/g,and 0.0485 mg/g,respectively.Through the analysis of the microscopic morphology of the material,explained the microwave extraction mechanism.4.In this study,the three-molecule template imprinted polymer was synthesized for the separation of syringin,eleutheroside E and isofraxidin in the deep eutectic solvent extract.The polymer can be directly adsorbed in the deep eutectic solvent aqueous environment,and the solvent recovery process was omitted.Prepared a solid-phase extraction column that simultaneously enriches the three,and the solid-phase extraction process was optimized.It was concluded that 1.0 mL H2O was used as the washing solvent,the loss rates of the template molecule were 10.8%,17.1%,6.90%,and 2.0 mL MeOH-HOAc(95:5 v/v)was used as the eluant(the washing solvent was 0.25 mL H2O at this time),the recovery rates of syringin,eleutheroside E and isofraxidin were 92.8%,94.3%,88.4%,respectively.
Keywords/Search Tags:Acanthopanax sentcosus, Macroporous resin, Ionic liquid, Deep eutectic solvent, Molecularly imprinted polymer
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