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Simultaneous Extraction of Glabridin and Glycyrrhizic Acid from Glycyrrhiza Glabra L.
Author: LiYuHui
Tutor: ZhangLianFu
School: Jiangnan University
Course: Agricultural Products Processing and Storage Engineering
Keywords: Glabridin Glycyrrhizic acid Glycyrrhiza glabra Extract Purification
CLC: TQ461
Type: Master's thesis
Year: 2011
Downloads: 120
Quote: 1
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Abstract
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Licorice is a traditional Chinese medicine in China, including the main functional ingredient glycyrrhizin, glycyrrhetinic acid, flavonoids and polysaccharides compounds. The current in licorice development practice, most of the extraction of glycyrrhizic acid, glabridin flavonoids and other ingredients with the dregs discarded, resulting in a tremendous waste of resources. In order to improve the the licorice utilization expand licorice industry chain, the optical light licorice Glycyrrhiza given, while the two most important active ingredient of licorice acid extraction and separation processes. First light while licorice the fixed and licorice acid extraction process. Selection of ammonia alcohol solution to extract glabridin and glycyrrhizic acid through single factor and orthogonal experiment to determine the optimum extraction conditions: 60% ethanol solution containing 0.6% ammonia water as the extraction agent, the solid-liquid ratio 1:20 (w / v) , 80oC extraction 2h, glabridin under the optimum conditions was 0.238%, glycyrrhizic acid was 5.08%, extracting the product glabridin content 6.30 mg / g, the content of the glycyrrhizic acid 0.134 g / g; preliminary exploration ultrasonic assisted extraction method of extraction conditions: ultrasonic power 150W, extraction time 75min, extraction temperature 50oC, solid to liquid ratio of 1:15 (w / v), in this condition glabridin was 0.249 % of glycyrrhizic acid was 5.42%, to extract the content of the product glabridin 8.54mg / g, glycyrrhizic acid content of 0.19g / g. Secondly, glabridin and glycyrrhizic acid extraction process, the choice of ethyl acetate as extraction solvent, the extract was concentrated to the original volume of 1/4, and adding an equal volume of ethyl acetate and extracted four times the content glabridin 40.60mg / g, the extraction rate was 92.0%, The glycyrrhizic acid extraction residue retention rate was 94.9%, glabridin and glycyrrhizic acid reached a basic separation. Further purification of the last two main object product: Select the polyamide (60-80 mesh) was purified by column chromatography (20mm × 300mm) glabridin, the sample concentration of 25mg/mL, the sample flow rate 2mL/min 40 % ethanol eluent were collected after the 50% ethanol elution fraction was concentrated under reduced pressure to a concentrated paste in the impurity, and finally were freeze-dried to give a brick red powder. LC-MS/MS analysis identified the glabridin the purity of 53.4%, higher than the commercial products on the market, compared with the crude extract purification factor of nearly 85 times; choose refined licorice acid and acid precipitation, use of concentrated hydrochloric acid and Crafts raffinate pH 2,0-4 oC low temperature and acid precipitation, and centrifuged to obtain the glycyrrhizic acid precipitation in 95% ethanol eluates, the extract liquid plus NH3 · H2O adjusted to pH 7.5, centrifuged glycyrrhizic acid ammonium salt precipitated by 4 times of glacial acetic acid hot dissolved after standing cooling the crystallization Glycyrrhetate ammonium salt. Final glycyrrhizic acid monoammonium salt purity of 85.7%, the total purification recovery was 71.2%.
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