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Extraction And Separation Of Effective Components From Polygonum Cuspidatum And Detection Of Resveratrol

Posted on:2013-05-25Degree:MasterType:Thesis
Country:ChinaCandidate:C R WangFull Text:PDF
GTID:2234330362974589Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
In order to resolve the problem of extraction process of resveratrol frompolygonum cuspidatum, such as poor efficiency of extraction, low degree of utilizationof extraction scraps and low value-added products, medicinal ingredients of polygonumwere explored to provide support for the full use of the medicinal materials residue afterextraction in this paper. According to the needs of resveratrol detections, appropriatedetection methods were established to guide improvement of process and reducing ofproduction costs. Based on the detection method, the hydrolysis processes werecompared to improve the yield of resveratrol.Taken water as solvent, water extract of polygonum cuspidatum was obtainedthrough the micro-wave extraction and stage extraction. Integrated extraction andseparation of the water extract which was extracted with ethyl acetate was carried out byrepeated column chromatography, preparation thin layer chromatography andrecrystallization. Ten compounds were obtained. Seven kinds of ingredients such asemodin, were identified by TLC, IR, NMR. Most of these compounds wereanti-inflammatory, antibacterial, antioxidant and full of development value, which canprovide reference for the comprehensive development and utilization of residues ofpolygonum cuspidatum after extracting resveratrol.In this paper, the standard addition curve was established to meet the demand ofresveratrol detection of polygonum cuspidatum extraction. Extraction officiency ofresveratrol in methanol extract of polygonum cuspidatum was0.18%. This methodwhich was simple, low cost of test and high accuracy, would be able to optimize of theextraction process. HPCE detection method of resveratrol was established to detectresveratrol in polygonum cuspidatum extraction. In the optimization of separationconditions, response peak migration time of resveratrol was7.121min. The testingcurve resveratrol detection was y=86591x+1805.7, related coefficient was about0.993, range of linearity of calibration curve was0.050.80mg/mL,linearity was good.When this method was applied to the resveratrol detection of methanol extract, thecontent of resveratrol was0.3598mg/L, the relative error compared with UV methodwas1.49%. Baseline separation of resveratrol and polydatin by HPCE was achieved tocompare the acid hydrolysis and enzyme hydrolysis processes of polydatin. Based onprinciples of chemiluminescence (CL) and microchip, the CL system on chip was designed and built to establish the relation curve of light intensity changes andconcentration of resveratrol. The curve was in the range of1.0×10-9mol/L1.0×10-5mol/L. When the method was applied to the analysis of syntheticsamples, the results were fit with UV and HPCE. The method using micro-pipeline asplace of reaction on-chip with less reagents, less samples and rapid analysis, can beused for content testing of resveratrol.HPCE was used to compare the acid hydrolysis and enzyme hydrolysis processesof polydatin. In the acid environment, the highest content of resveratrol was197.36mg/L after acid hydrolysis for1h, and hydrolysis rate of polydatin was62.87%.Because yeast grown slowly,the highest content of resveratrol was123.32mg/L and thehydrolysis rate of polydatin was35.33%after enzyme hydrolysis for24h. Enzymatichydrolysis with slow speed, mild conditions, and less disruptive of resveratrol, was stilldominant position in industrial production. In the process of acid hydrolysis, the hightemperature and a large number of H+would catalyed the alcohol addition reaction ofresveratrol to decrease the concentration of resveratrol. The acid hydrolysis process hada fast response, high efficiency of hydrolysis with high requirements of equipment.Two-phase acid hydrolysis and strictly control of reaction time were carried to protectthe resveratrol.In this research, integrated extraction and separation of ethyl acetate layerextraction of water extract of polygonum cuspidatum was carried out to provideguidance for the comprehensive utilization of polygonum cuspidatum. Seven kinds ofcompounds were obtained, which had anti-inflammatory, antibacterial and antioxidantactivity. Second, three kinds of detection methods of resveratrol were established toprovide reference for the analysis of resveratrol in the process of extracting, hydrolysisand content detection. Thirdly, compared the hydrolysis processes of polygonumcuspidatum relying on the analytical method established in this paper, can provide areference for the improvement of hydrolysis efficiency of polydatin.
Keywords/Search Tags:polygonum cuspidatum, comprehensive extraction and separation, analysisof resveratrol, hydrolysis technology
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