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Method for producing trifolium pratense L. isoflavones

A technology of red clover and its production method, which is applied in the production field of red clover isoflavones, can solve the problems of immature extraction and separation technology and high requirements for extraction technology, and achieve the effects of energy saving, solvent saving, and prolonging the use cycle

Active Publication Date: 2012-01-04
ENSHI JIYUAN PHARMA TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commonly used high-performance liquid chromatography technology for detection, red clover isoflavones usually calibrate four components: daidzein (Daidzein), genistein (Genistein), biochanin A (Biochanin A) and formononetin (Formononetin) ), the higher content of red clover isoflavones requires high extraction technology. At present, the extraction and separation technology of high-content red clover is immature in China, which has become a research hotspot in the field of phytochemistry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1. Extraction Put 10KG of crushed red clover material, add 4.5L of 80% methanol each time, soak for 1 hour, stir and heat to 80°C for 3 hours to extract. Extract 4 times, combine about 118L of the first three extracts, of which about 44L of the fourth extract is used for the next batch of extracts.

[0019] 2. Filtration Cool the extracts for the first three times for 1 hour and then vacuum filter (300 mesh filter cloth).

[0020] 3. Pretreatment of activated carbon Soak 6KG activated carbon in 5% HCL solution for 3 hours, filter, then wash with water until the pH value is 7, then soak in 5% NaOH solution for 3 hours, filter, and wash with water to pH 7, the column.

[0021] 4. Decolorization Put the 118L solution on the column slowly, and control the flow rate to 12L / H.

[0022] 5. Concentration Concentrate the solution passed through the activated carbon column in step 4 at 70°C, and stop concentrating when the remaining 10L is concentrated. Transfer to extraction ...

Embodiment 2

[0031] 1. Extraction Put 200KG of crushed red clover material, add 920L of 80% methanol each time, soak for 1.5 hours, stir and heat to 80°C for 3 hours to extract. Extract 4 times, combine about 2450L of the first three extracts, of which about 900L of the fourth extract is used for the next batch of extracts.

[0032] 2. Filtration After cooling the first three extracts for 2 hours, filter the plate and vacuum filter (500, 400, 300 mesh filter cloth).

[0033] 3. Pretreatment of activated carbon Soak 110KG activated carbon in 5% HCL solution for 4 hours, filter, then wash with water until the pH value is 7, then soak in 5% NaOH solution for 4 hours, filter, and wash with water To PH value of 7, on the column.

[0034] 4. Decolorization Put the 2450L solution on the column slowly, and control the flow rate to 200L / H.

[0035] 5. Concentration Concentrate the solution passed through the activated carbon column in step 4 at 70°C, and stop concentrating when the remaining 200L...

Embodiment 3

[0043]1. Extraction Put 800KG of crushed red clover material, add 3800L of 80% methanol each time, soak for 1.5 hours, stir and heat to 80°C for 3 hours to extract. Extract 4 times, combine about 7400L of the first three extracts, of which about 3700L of the fourth extract is used for the next batch of extracts.

[0044] 2. Filtration After cooling the first three extracts for 2 hours, filter the plate and vacuum filter (500, 400, 300 mesh filter cloth).

[0045] 3. Pretreatment of activated carbon First soak 450KG activated carbon in 5% HCL solution for 4 hours, filter, then wash with water until the pH value is 7, then soak in 5% NaOH solution for 4 hours, centrifugal filter, and rinse with water Wash until the pH value is 7, and put on the column.

[0046] 4. Decolorization Put the 7400L solution on the column slowly, and control the flow rate to 200L / H.

[0047] 5. Concentration Concentrate the solution passed through the activated carbon column in step 4 at 70°C, and st...

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Abstract

The invention relates to a method for producing trifolium pratense L. isoflavones, which is characterized by comprising the following steps of: a, extracting, namely extracting trifolium pratense L. by using methanol; b, filtering, namely standing extract in a storage tank, and filtering to remove slag; c, decolorizing and concentrating, namely decolorizing by using an activated carbon column, concentrating, extracting by using petroleum ether and ethyl acetate respectively, and concentrating to obtain a dry product; d, regulating the ph value, namely dissolving the dry product in NaOH aqueous solution, and controlling the ph value to be between 7 and 9; e, loading to a column, namely loading AB-8 macroporous adsorption resin to the column, eluting by using methanol solution, and evaporating until solution is dried; and f, extracting and crystallizing, namely dissolving the dry product in the NaOH aqueous solution, extracting by using the ethyl acetate, concentrating to reach certain volume, and performing cooling crystallization. An isoflavone product with high purity is obtained through steps of extracting solution and column chromatography solution recycling, two-time extraction, column chromatography and the like; a large quantity of solvent, electricity and heat are saved, and the service cycle of resin is prolonged; and by the process, product quality is improved, and energy consumption is reduced.

Description

technical field [0001] The invention relates to a production method of red clover isoflavones. Background technique [0002] Red clover (Trifolium pratense L.) is a leguminous perennial herb, also known as red clover, red clover and clover. Originating in Europe and West Asia, it is now widely distributed all over the world and is a temperate distribution plant. It is cultivated in all parts of the north and south of my country. Wild red clover is rich in resources. The red clover isoflavones in red clover mainly include biochanin A (biochanin A), daidzein (daidzein), genistein (genistein) and formononetin (formononetin), in addition, it also contains willowerin (pectolinarigenin), red cloverin (pratensein) and wild indigoside (pseudobaptigenin) and other isoflavone components. Red clover isoflavones have a series of health effects such as anti-oxidation (delaying aging), anti-cancer, anti-atherosclerosis, anti-thrombosis, and lowering blood lipids, especially for estrog...

Claims

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Application Information

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IPC IPC(8): A61K36/48A61P3/06A61P7/02A61P9/10A61P35/00A61P39/06
Inventor 何美军廖朝林喻大昭王华张宇穆森廖璐婧何银生
Owner ENSHI JIYUAN PHARMA TECH DEV
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