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Method for separating and purifying epicatechin gallate (ECG) monomer

A technology for the separation and purification of epicatechin gallate, which is applied in the direction of organic chemistry, can solve the problems of no industrialized preparation of EGC monomer, expensive bonded silica gel, and large amount of organic solvents, so as to improve wound wounds The effect of healing, short preparation cycle and simple method

Active Publication Date: 2012-05-02
湖北宇隆生物工程有限责任公司
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Problems solved by technology

Zhang Ying et al. used a self-made preparative countercurrent chromatograph to separate and purify ECG monomer from catechin with petroleum ether-ethyl acetate-water (0.2:1:2, v / v) as the solvent system, with a purity of 98%. %[8]; Huang Yongdong et al. used B-type three-zone simulated moving bed technology, with C18 bonded silica gel as the stationary phase, ethanol and water (20:80, v / v) is the mobile phase, the ECG with a purity of 91.33% can be obtained by using the Varicol process, and the recovery rate is 91.41%[9], but the above two methods have C18 Bonded silica gel is expensive, the amount of organic solvent is large, and the separation platform (counter-current chromatography, moving bed) has shortcomings such as small loading capacity, which is not suitable for scale-up
So far, there are no reports on the industrial preparation of EGC monomer at home and abroad.

Method used

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Embodiment Construction

[0030] The present invention will be further clarified through the detailed description of specific embodiments below, but it is not intended to limit the present invention, but only for illustration.

[0031] The method for separating and purifying epicatechin gallate (ECG) monomer from raw materials of Yunnan big-leaf green tea comprises the following steps:

[0032] 1. Ethyl acetate extraction of total catechins in green tea raw materials:

[0033] Weigh the raw material of Yunnan big-leaf green tea (purchased from Shuangjiang County, Yunnan, with an ECG content of 4.10%), add 7 BV / 6BV / 4BV ethyl acetate and heat and extract three times (1h / time, keep the water bath temperature at 45°C-50°C) , intermittent 30min and stirring for 5min), combine all the extraction solutions, recover ethyl acetate under reduced pressure, add pure water to fully replace the ethyl acetate in the later stage, concentrate to 6-7 Pomi degrees, and then spray dry with a centrifugal spray tower to con...

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Abstract

The invention discloses a method for separating and purifying an epicatechin gallate (ECG) monomer, which comprises the following steps of: with Yunnan broad-leaf green tea as a raw material, directly extracting by using ethyl acetate; chromatographically adsorbing and eluting a crude extract by two different adsorbent resin columns respectively; collecting desorption fractions containing ECG; concentrating and recovering ethanol in a high-efficiency external-circulation way and concentrating by a reverse osmosis membrane at low temperature; refrigerating and crystallizing 95% ethanol at low temperature; at last, freezing and drying to obtain 98% ECG monomer. The method disclosed by the invention is simple and convenient, short in preparation cycle and low in cost, complies with environment friendliness and safety requirements and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a method for separating and purifying epicatechin gallate (ECG) monomer from green tea raw materials, which belongs to the technical field of food. Background technique [0002] Catechins have obvious pharmacological functions such as anti-aging, anti-cancer and anti-mutation, fat loss and weight loss, lowering blood sugar, blood lipid and cholesterol, and preventing cardiovascular diseases. They have been widely used in food processing, medical care, and daily chemical industries. [1-3] . In October 2006, the U.S. Food and Drug Administration (FDA) approved tea polyphenols as a new prescription drug for topical (external) treatment of genital warts caused by human papillomavirus. The first plant (herbal) drug approved for marketing [4] . In the past two decades, due to breakthroughs in the research on the health care and pharmacological functions of tea polyphenols / catechins, not only the share of green tea in the internati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/62
Inventor 张盛刘仲华李适李银花
Owner 湖北宇隆生物工程有限责任公司
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