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Method for separating cucurbitacin B from muskmelon vine by virtue of catalytic reaction

A catalytic reaction, melon vine technology, applied in the fields of organic chemistry, steroids, etc., can solve the problems of inability to provide tons of raw materials, hidden dangers of fermentation tank and site safety, undesired industrial products, etc. The effect of short time and increased yield

Active Publication Date: 2014-10-08
西安天丰生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] 1. The source of raw materials: According to data calculations, 1 mu of melons can produce about 3-5 kilograms of dry melon stalks. In 2014, the price of melon stalks in the Bozhou market was 800 yuan / kg
And there is no way to provide tons of raw materials
[0015] 2. The temperature problem of enzymatic hydrolysis: Enzymatic hydrolysis is actually a fermentation process, which is greatly affected by temperature. There is a huge difference between winter and summer. As a product, the change of production season will lead to periodic changes in product delivery time. Very undesirable for an industrial product
[0016] 3. According to the technical information of the patent, the enzymatic hydrolysis time of 2 to 4 days greatly wastes the cost of manpower and material resources, and large-scale fermentation tanks and sites have many safety hazards and are not environmentally friendly
[0019] The biggest problem of this method is that simply using the conventional acid hydrolysis conversion method, only part of the cucurbitacin B-2-glucoside is converted, and the long-term acidic environment will lead to the destruction of cucurbitacin B, and the conversion yield is low. Significant waste of raw materials

Method used

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  • Method for separating cucurbitacin B from muskmelon vine by virtue of catalytic reaction
  • Method for separating cucurbitacin B from muskmelon vine by virtue of catalytic reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] Get 1.5 kilograms of raw materials, add 9 liters of ethanol, heat and extract three times in a 20L wide-mouthed bottle, each time for 1 hour, concentrate to obtain 163 grams of extract, detect that the concentration of cucurbitacin B is 18.4 mg / g, 163 grams of extract, add 24.45 1 gram of concentrated hydrochloric acid, then add 4.89 gram of ferric chloride hexahydrate, react for 30 minutes, the pH after washing is 4~6, obtain 78 gram of crude product, detect that the content of cucurbitacin B is 61.5 mg / gram, the yield of cucurbitacin B increases It was 59.94%, and carried out crystallization and suction filtration according to the invention process. Obtain product 3.53 grams, content detection is 98.33%.

Embodiment 2

[0090] Get 15 kilograms of raw materials, add 90 liters of ethanol, heat and extract three times in a 200L extraction tank, each time for 1 hour, concentrate to obtain 1576 grams of extract, detect that the concentration of cucurbitacin B is 17.95 mg / g, 1576 grams of extract, add 236.4 gram of concentrated hydrochloric acid, then add 47.28 grams of ferric chloride hexahydrate, react for 30 minutes, wash pH4-6 to obtain 791 grams of crude product, detect that the content of cucurbitacin B is 56.83 mg / gram, and the yield of cucurbitacin B increases to 58.9%. And carry out crystallization and suction filtration according to the inventive process. 36.7 g of product was obtained.

[0091] The content detection is 99.13%.

Embodiment 3

[0093] Get 50 kilograms of raw materials, add 300 liters of ethanol, heat and extract three times in the extraction tank of 500L, each time 1 hour, concentrate and obtain 4961 grams of extract, detect that the concentration of cucurbitacin B is 17.64 mg / g, 4961 grams of extract, add 744.15 1 gram of concentrated hydrochloric acid, then add 148.83 gram of ferric chloride hexahydrate, react for 30 minutes, wash pH4-6 to obtain 2473 gram of crude product, detect that the content of cucurbitacin B is 55.72 mg / gram, and the yield of cucurbitacin B increases to 57.46%. And carry out crystallization and suction filtration according to the inventive process. Obtain product 121.7 grams,

[0094] The content detection is 98.81%.

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Abstract

The invention discloses a method for separating cucurbitacin B from muskmelon vines by virtue of catalytic reaction. The method comprises the following steps: an extraction process, namely taking 1 part of the muskmelon vines, soaking by using ethanol, performing reflux extraction, and filtering and concentrating an extracting solution to obtain an extract; the catalytic reaction, namely adding concentrated hydrochloric acid into the extract, then adding ferric trichloride hexahydrate, stirring and reacting, cooling to the room temperature, filtering, performing water rinsing, and drying; a refining process, namely stirring and dissolving a crude product by using ethyl acetate, then adding activated carbon, decoloring, concentrating to a small volume, and standing overnight to perform crystallization; a recrystallization process, namely dissolving a like fine product by using ethanol, filtering and concentrating to a small volume while hot, standing overnight to perform crystallization, and filtering; and putting the fine product in a vacuum drying box, and drying for 8 hours to obtain a cucurbitacin B fine product. The method disclosed by the invention is wide in raw material source and low in production cost, and can be used for reducing the damages of an acid environment to cucurbitacin B; the production rate reaches more than 60%, the purity is more than 99.0%, and the wastewater BOD (biochemical oxygen demand) is less than 100; the method is suitable for the industrial production of recycling water, and can be widely applied to plant extraction industries.

Description

technical field [0001] The invention relates to a method for separating cucurbitacin B by catalytic reaction, in particular to a method for separating cucurbitacin B from muskmelon vines by catalytic reaction. Background technique [0002] Cucurbitacin B is a new type of drug used in the treatment of acute and persistent chronic hepatitis and primary liver cancer. [0003] APIs are widely used in various fields such as pharmaceuticals, cosmetics and health products. [0004] According to literature reports, the content of cucurbitacin B in the melon pedicle is the highest, which can reach 0.6%---0.8%. Not high, and the limited quantity of product supply and other defects. [0005] Because of the novelty of the futures market and the strict confidentiality of the process route by domestic and foreign manufacturers, cucurbitacin B has not applied for many patents. [0006] The Chinese patent (201010235780.X) applied by Nanjing Zelang Agricultural Development Co., Ltd. on J...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 杨海鹰王晓龙
Owner 西安天丰生物科技股份有限公司
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