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Determination Of Diosgenin In Jingangteng By HPLC And Improvement On Its Extraction Technique

Posted on:2006-01-19Degree:MasterType:Thesis
Country:ChinaCandidate:M H JiangFull Text:PDF
GTID:2144360182969918Subject:Inorganic Chemistry
Abstract/Summary:PDF Full Text Request
Jingangteng is the rhizome of Smilax china L. which belongs to Smilax of Liliaceae. It has been used mostly to treat all kinds of inflammation, such as pelvic inflammatory of female, and got satisfactory therapeutic effect, which means it has promising market potential. However, up to now, there haven't had suitable analytical methods for quality control of Jingangteng preparations; On the other hand, to get satisfactory therapeutic effect, large dosage of Jingangteng preparations which is prepared by traditional technology are needed. The traditional technology also needs to use a great deal of organic solvent, which means high cost and environment pollution. To these reasons, in this paper, HPLC method was developed to detect diosgenin in Jingangteng, at the same time, the experimental conditions of ultrafiltration to purify Jingangteng extract were studied, the comparison of the purification effects between ultrafiltration and alcohol sedimentation were made. The main results are as follows: 1. HPLC method was established to determine diosgenin in Jingangteng, and the optimum hydrolytic condition for crude drug and dry steeps were obtained. The optimum hydrolytic condition for crude drug was: zymolysis at 39℃for 72 hours, hydrolysis at 90℃with 5% sulfuric acid for 6 hours under natural pressure; The reserved time of diosgenin was about 10 minutes under its chromatograms conditions, and the R-value between the main peak and the nearby peak was bigger than 2, which means reaching the standard of chromatograms separation. The precision, recurrence and recovery were good. The optimum hydrolytic condition for dry steeps was that with 3% sulfuric acid, hydrolysis for 5 hours at 90℃under natural pressure. In the chromatograms conditions, the reserve time of diosgenin was about 12 minutes, the main peak and the nearby peak were separate well, the precision, recurrence were also good and the lowest quantity which could be detected was 117.8 ng. The results will be better if the sample is passed through a neutro-alumina column before it is carried to analyze. 2. The effects of all kinds of experimental conditions in clarifying Jingangteng extract by ultrafiltrating were studied, the cleanout method of membrane was preliminary studied. The result showed that the extract pre-filtrated with millipore filtration will be easier for further ultrafiltration; the membrane with intercept molecular weight of 60000 was the best, the pressure should less than 0.20 MPa, the temperature should be controlled in 40℃and the concentration was 0.2 g·mL-1. The flux of polluted membrane could resume to 72.80% after it had been cleaned by 0.05 mol·L-1 sulfuric acid and 0.05 mol·L-1 sodium hydroxide alternately. 3. The purification effects of ultrafiltration and alcohol sedimentation to Jingangteng extract were studied. By considering the decreasing ratio of dry steeps, the recovery of diosgenin and diosgenin content of per unit solid matter, the purification effect of 70% alcohol sedimentation was better than that of ultrafiltration and all others concentrations of alcohol sedimentation. However, ultrafiltration could keep the highest recovery of diosgenin, and what's more, could be operated easily, economizing solvent and reducing environment pollution.
Keywords/Search Tags:Jingangteng, Diosgenin, HPLC, Ultrafiltration, Alcohol sedimentation
PDF Full Text Request
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