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The Studies On Extraction And Concentration Process Of Phenylethanoid Glycosides In Callicarpa Kwangtungensis Chun. And Chemical Constituents From Callicarpa Macrophylla Vah.

Posted on:2017-03-30Degree:MasterType:Thesis
Country:ChinaCandidate:H XuFull Text:PDF
GTID:2284330503980540Subject:Pharmacognosy
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The genus Callicarpa, belonging to the Verbenaceae plant family. Forty-eigh t species from Callicarpa L. have been found in the provinces to the south of the Yangzi River in China. Plants of this genus have important pharmaceutica l value and have the anti-inflammatory and hemostatic activities.They are exten sively used in clinical and civilian treatment. As two representative medicinal p lants of genu, Callicarpa kwangtungensis Chun. and Callicarpa macrophylla Va h. were both collected in the 2010 edition of Chinese Pharmacopeia. The distri bution of Callicarpa kwangtungensis Chun is in the Jiangxi, Guangdong and G uangxi Province etc. Modern medicine has indicated that it possesses various p harmacological effects involving clearing heat, removing toxicity, hemostatic, ast ringent and desslpating blood stasis effect and has been widely used in the tre atment of rheumatism, hematuria, hematemesis, and women amenorrhea. It cont ains a variety of active ingredients, including phenylethanoid glycoside which h as attracted much interest.Such components have antioxidative, antimicrobial an d anti-inflammatory activity which are closely related to the pharmacological ef fects of the plant.Our previous studies have shown that phenylethanoid glycosid e is the basis of its anti-inflammatory activity. Callicarpa macrophylla Vah. is mainly distributed in Gui Zhou, Guangdong and Guangxi Provinces etc. It has t he effect to eliminate stasis to activate blood circulation and stop bleeding,als o has the actions of detumescence and analgesia. It has been reported containin g flavonoids, essential oils, terpenoids and phenylpropanoids. However the res earch on Callicarpa macrophylla Vah. is relatively small and the material basis of its efficacy is not clear enough. In order to further develop and utilize of Callicarpa medicinal plants, we choose Callicarpa kwangtungensis Chun and C allicarpa macrophylla Vah. as the objects of study and plan to undertake the f ollowing studies:1. The study of extraction process of phenylethanoid glycosides in Callicarpa kwangtungensis Chun.The cycle of ultrasonic extraction、reflux extraction 、dipping extraction m ethod were examined.Finally we choose reflux extraction. Based on the results of single factor experiments, orthogonal experiment was designed to investigate ethanol concentration, refluxing time, extraction times and ethanol volume, refl uxing time for the yield of phenylethanoid glycosides.Therefore, the extraction technology of phenylethanoid glycosides: ethanol concentration: 90%; ethanol volume: 10; extraction times: 3 times; extraction time: 60 min. And the yield r ate of phenylethanoid glycosides is 2.66%.2. Concentration process of phenylethanoid glycosides in Callicarpa kwangtung ensis Chun. Five kinds of macroporous resins were used to compare their absorption a nd desorption of phenylethanoid glycosides. LS-300 B resin was determined to bebetter absorbent material and it possessed high absorption and desorption cap acity. Depending on LS-300 B resin’s dynamic absorption capacity,we finally d ecide the parameters of the processs,such as: sample weight, the concentrati on of sample, the speed of loading sample, the ratio of eluent, et al.And the p urity of phenylethanoid glycosides is 66%, the transport rate is over 80%.3. The study of the compoents of the Callicarpa macrophylla Vah. The chemical investigations of the Callicarpa macrophylla Vah. were carrie d out. Sixteen compounds were isolated from the ethanol extracts from Callic arpa macrophylla Vah. by using silica gel column chromatography, Sephadex L H-20 gel chromatography, polyamide column chromatography, semi-preparative HPLC and TLC etc, including six abietane diterpenes,five flavonoids and five phenolic compounds. These compounds were identified as β-Asarone(1), γ-as aron(2),(E)-asarone(3), 4-Methoxybenzoic acid(4), Asaronaldehyde(5),Angustanoic acid G(6), 1,2,3,4,4a,9,10,10a-octahydro-1,4a-dimethyl-7-(1-methyl ethenyl)-9-oxo-1-phenanthrenecarboxylic acid(7), Macrophyllastic acid A(8), Angustanoic acid E(9), 4-epi-dehydroabietic acid(10),Angustanoic acid F(11),(﹣)-pinocembrin(12), 5-hydroxy-3,7,4’-trimethoxyflavone(13),5-hy droxy-3,6,7,4’-tetramethoxyflavone(14),(﹣)-pinostrobin(15), 5-hydroxy-3,7,3’,4’-tetramethoxyflavone(16)by physicochemical property and spectroscopic analysis(MS, 1D-NMR, 2D-NMR). Compound 8 is a new compound, compo unds 1, 2, 3,4, 5, 6, 7, 9, 10, 11,12, 15 are isolated from the plants of genu s Callicarpa L. for the first time; 13, 14, 16 are isolated from this plant for the first time.
Keywords/Search Tags:Callicarpa L, Callicarpa kwangtungensis Chun, Callicarpa macrop hylla Vah., Extraction process, Concentration process, Chemical constituents
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