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Studies on Separation and Characterizations of Hypotensive Compounds from Eucommia Ulmoides Oliv

Author: CaoHui
Tutor: ChenXiaoQing
School: Central South University
Course: Analytical Chemistry
Keywords: Eucommia ulmoide geniposidic acid geniposide extraction and purification isolation and characterization
CLC: TQ461
Type: Master's thesis
Year: 2005
Downloads: 223
Quote: 4
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Abstract


Based on a large number of resources investigation and literature systematization, the medical bioactive ingredients of Eucommia ulmoide Oliver living in Hunan were made as object. The iridoids constituents of the plant were extracted、 purified、 analyzed and characterization. Two bioactive constituents were separated and identified as geniposidic acid and geniposide by means of HPLC, UV, IR, 1HNMR and MS. Details are as following:1. Extraction of geniposidic acid and geniposide. The extraction methods of ethanol extraction, enzyme extraction, Semi-bionic extraction and SFE were studied systemically. Semi-bionic extraction was chosen for its high extraction ratio of geniposidic acid and geniposide and the best condition was: sample, 10g; H2O, 100ml; pH, 1.5; temperature 60° C; time , 1.5 h. After filtration, the residue was extracted with water which pH were 7.5 and 8.5 for two times. The extraction ratios of geniposidic acid and geniposide were 1.50% and 0.49% respectively.2. Purification of geniposidic acid and geniposide. Solvent extraction was been choosen as the first purification. Then, the purification methods of kieselgur, active carbon, polyamide and A macroporous adsorption resin were studied systemically. The macroporous adsorption resin was chosen for its higher purity. The recovery ratios of geniposidic acid and geniposide were 84.15% and 73.49% respectively.3. Isolation of the medical bioactive ingredients of Eucommia ulmoide Oliver. The silica gel column chromatography was used to attain two monomers of geniposidic acid and geniposide. The obtained product after purification dissolved with methanol was subjected to silica gel column and eluted with the successive eluting solvent mixture of chloroform and methanol. The eluted fractions were analyzed by RP-HPLC-DAD. The purities of attained geniposidic acid and geniposide were 98.69% and 96.54% respectively. Preparation of geniposidic acid and geniposide by preparative high performance liquid chromatography was studied, as well.4. Determination and identification of geniposidic acid and geniposide. Method of RP-HPLC-DAD was established to determine the contents of geniposidic acid and geniposide in extracts and progress of isolation and purification. The analysis condition was following: Column, VP—ODSRP-18 （150mmx4.6mm）; Mobile phase, methanol -water-acetic acid= 20:79.5:0.5（v/v）; Detecting wavelength, 350 nm and DAD; Flow rate, 1.0 mL/min; Column temperature, room temperature; The quantity of injecting sample, 10.0 uL.The structures of two monomers were identified as geniposidic acid and geniposide by means of UV, IR, NMR and MS.

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