CN103463160A - Preparation method of high-content total flavones of chrysanthemum - Google Patents
Preparation method of high-content total flavones of chrysanthemum Download PDFInfo
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- CN103463160A CN103463160A CN 201310425670 CN201310425670A CN103463160A CN 103463160 A CN103463160 A CN 103463160A CN 201310425670 CN201310425670 CN 201310425670 CN 201310425670 A CN201310425670 A CN 201310425670A CN 103463160 A CN103463160 A CN 103463160A
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Abstract
The invention relates to a preparation method of high-content total flavones of chrysanthemum, and specifically relates to a method for extracting the total flavones in the chrysanthemum by an enzyme-microwave method. The preparation method comprises the following treatment steps of raw material crushing, enzyme-microwave method-based extraction, petroleum ether extraction and macroporous adsorption resin purification. The method can be used for producing the high-quality and high-content total flavones of the chrysanthemum, and is capable of reducing material loss, shortening the production period, increasing the product yield and reducing the production cost, and suitable for industrial production. The content of total flavones in a chrysanthemum extract obtained by the preparation method provided by the invention is above 70%.
Description
technical field:
The present invention relates to a kind of isolation and purification method of effective components in plants, particularly relate to a kind of method that adopts enzyme-microwave method to extract chrysanthemum total flavone.
background technology:
The dry capitulum that Flos Chrysanthemi is the Compositae herbaceos perennial, have the effects such as heat-clearing and toxic substances removing, dispelling wind item, suppressing the hyperactive liver removing heat from blood.Its chemical composition has flavone compound, triterpenoid compound and volatilization wet goods.Wherein total flavones is the main pharmacodynamics active component of Flos Chrysanthemi, has the effects such as blood pressure lowering, coronary artery dilator is atherosis, clinical hypertension and the coronary heart disease etc. of being used for the treatment of, the normal quality of estimating Flos Chrysanthemi with the content of total flavones.Flavone compound is a class natural product widely distributed in plant, extensively is present in plant kingdom, is the effective composition of many Chinese herbal medicine, and its major part in plant is combined into glycoside with sugar, and fraction exists with the form of dissociate (aglycon).The research of flavone compound in recent years, to tend to the exploitation of its medical value, relates to the applied research of extraction process, assay and the preparation preparation of flavone compound more.
The extracting method of flavone crude product mainly contains both at home and abroad at present: solvent extraction, ion precipitation method, resin absorption partition method, supercritical fluid extraction, ultrasonic-leaching method, microwave extraction, enzymatic isolation method etc.Have that length consuming time, effective component extraction rate are low, the shortcoming of complicated operation, do not meet the requirement of the modernization of Chinese medicine, also be unfavorable for the be applied to development of chrysanthemum total flavone at industry-by-industry.
summary of the invention:
The present invention be directed to the existing research for preparing the existing defect of method of high-load chrysanthemum total flavone and carry out, but aim to provide a kind of high efficiency and selectivity, easy and simple to handle, productive rate is high, the preparation method of the few realization of industrialization of by-product.
Technical scheme of the present invention is carried out according to the following step:
A. dry Flos Chrysanthemi is pulverized, crossed 50 mesh sieves;
B. be 0.3% ~ 0.7% of raw material to adding the enzyme amount in above-mentioned raw materials, add 60 ~ 70% alcoholic solution, solid-liquid ratio is 1:15 ~ 25, and adjusting pH value is 4.5 ~ 5.5, and microwave extraction power is 250 ~ 350W, and the microwave extraction time is 90 ~ 150s;
C. extracting solution is reclaimed to the aqueous solution that ethanol obtains extract, then use the petroleum ether extraction of 3 ~ 5BV, until extract is aobvious colourless, reclaim solvent, obtain thick paste;
D. the macroporous resin adsorption of 10 ~ 15 times for the gained thick paste, first wash with water, then uses 50 ~ 70% ethanol elution of 3 ~ 5 times of amount of resin, finally reclaims solvent, drying, pulverizing and obtain powdered extract.
Macroreticular resin described in steps d is AB-8, HPD-20 or D-101.
Flavone compound is intracellular organic matter, and its cell wall three major polymers: cellulose forms.Cellulase is the compound enzyme that cellulose hydrolysis can be become to water-soluble sugar.Flos Chrysanthemi is with after cellulose treatment, and the hydrolysis of cell wall is broken, and is conducive to the stripping of intracellular matter.And microwave is a kind of ultrahigh speed electromagnetic wave, there is very strong penetration, moisture or the rapid increasing temperature and pressure of mailing solvent in plant cell, cell wall perforation, make composition stripping from cell, to increase the dissolving of effective ingredient in solvent in Flos Chrysanthemi, and microwave electromagnetic field makes aggravation in the molecular motion short time, thereby shortened the time, improved extraction ratio.The present invention, enzyme process and two kinds of technology couplings of microwave extraction, has complementary advantages, and has improved widely the extraction ratio of chrysanthemum total flavone.
Further illustrate the present invention below in conjunction with the specific embodiment, but the scope of protection of present invention is not limited to following embodiment.
the specific embodiment:
Embodiment 1:
Dry Flos Chrysanthemi is pulverized, crossed 50 mesh sieves; To adding the enzyme amount in raw material, it is 0.3% of raw material, add 60% alcoholic solution, solid-liquid ratio is 1:15, and adjusting pH value is 4.5, and microwave extraction power is 250W, the microwave extraction time is 100s, extracting solution is reclaimed to the aqueous solution that ethanol obtains extract, then use the petroleum ether extraction of 3BV, until extract is aobvious colourless, reclaim solvent, obtain thick paste; The AB-8 macroporous resin adsorption of 10 times for the gained thick paste, first wash with water, then uses 50% ethanol elution of 3 times of amount of resin, finally reclaim solvent, drying, be ground into fine powder, obtain the chrysanthemum total flavone extract, after testing, extract ZHONGJUHUA general flavone content is 68.6%.Assay method, take the rutin standard substance as contrast, presses the ultraviolet spectrophotometry trap, calculates the content of total flavones.Lower same.
Embodiment 2:
Dry Flos Chrysanthemi is pulverized, crossed 50 mesh sieves; To adding the enzyme amount in raw material, it is 0.5% of raw material, add 70% alcoholic solution, solid-liquid ratio is 1:20, and adjusting pH value is 5.0, and microwave extraction power is 300W, the microwave extraction time is 120s, extracting solution is reclaimed to the aqueous solution that ethanol obtains extract, then use the petroleum ether extraction of 4BV, until extract is aobvious colourless, reclaim solvent, obtain thick paste; The HPD-20 macroporous resin adsorption of 15 times for the gained thick paste, first wash with water, then uses 60% ethanol elution of 4 times of amount of resin, finally reclaim solvent, drying, be ground into fine powder, obtain the chrysanthemum total flavone extract, after testing, extract ZHONGJUHUA general flavone content is 71.4%.
Embodiment 3:
Dry Flos Chrysanthemi is pulverized, crossed 50 mesh sieves; To adding the enzyme amount in raw material, it is 0.7% of raw material, add 65% alcoholic solution, solid-liquid ratio is 1:25, and adjusting pH value is 5.5, and microwave extraction power is 350W, the microwave extraction time is 150s, extracting solution is reclaimed to the aqueous solution that ethanol obtains extract, then use the petroleum ether extraction of 5BV, until extract is aobvious colourless, reclaim solvent, obtain thick paste; The D-101 macroporous resin adsorption of 12 times for the gained thick paste, first wash with water, then uses 70% ethanol elution of 5 times of amount of resin, finally reclaim solvent, drying, be ground into fine powder, obtain the chrysanthemum total flavone extract, after testing, extract ZHONGJUHUA general flavone content is 70.1%.
Claims (2)
1. the preparation method of a high-load chrysanthemum total flavone is characterized in that:
A. dry Flos Chrysanthemi is pulverized, crossed 50 mesh sieves;
B. be 0.3% ~ 0.7% of raw material to adding the enzyme amount in above-mentioned raw materials, add 60 ~ 70% alcoholic solution, solid-liquid ratio is 1:15 ~ 25, and adjusting pH value is 4.5 ~ 5.5, and the extraction power of microwave is 250 ~ 350W, and the microwave extraction time is 90 ~ 150s;
C. extracting solution is reclaimed to the aqueous solution that ethanol obtains extract, then use the petroleum ether extraction of 3 ~ 5BV, until extract is aobvious colourless, reclaim solvent, obtain thick paste;
D. the macroporous resin adsorption of 10 ~ 15 times for the gained thick paste, first wash with water, then uses 50 ~ 70% ethanol elution of 3 ~ 5 times of amount of resin, finally reclaims solvent, drying, pulverizing and obtain powdered extract.
2. preparation method according to claim 1, it is characterized in that: the macroreticular resin described in steps d is AB-8, HPD-20 or D-101.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105326876A (en) * | 2015-11-11 | 2016-02-17 | 南阳师范学院 | Method for extracting total flavonoids of chrysanthemum |
| CN107164449A (en) * | 2017-08-03 | 2017-09-15 | 广州立达尔生物科技股份有限公司 | A kind of utilization marigold flower dregs of rice extract solution is method and the application that fermenting raw materials produce astaxanthin |
| CN107468738A (en) * | 2017-09-22 | 2017-12-15 | 安徽菊泰滁菊草本科技有限公司 | A kind of extracting method of chrysanthemum total flavone |
| CN108851195A (en) * | 2018-07-26 | 2018-11-23 | 湖北中烟工业有限责任公司 | A kind of preparation method of cigarette alfalfa extract |
| CN111632076A (en) * | 2020-05-20 | 2020-09-08 | 伊犁师范大学 | Method for preparing total flavonoids of alpine yarrow herb by microwave-assisted enzymolysis |
-
2013
- 2013-09-18 CN CN 201310425670 patent/CN103463160A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105326876A (en) * | 2015-11-11 | 2016-02-17 | 南阳师范学院 | Method for extracting total flavonoids of chrysanthemum |
| CN107164449A (en) * | 2017-08-03 | 2017-09-15 | 广州立达尔生物科技股份有限公司 | A kind of utilization marigold flower dregs of rice extract solution is method and the application that fermenting raw materials produce astaxanthin |
| CN107164449B (en) * | 2017-08-03 | 2021-06-25 | 广州立达尔生物科技股份有限公司 | Method for producing astaxanthin by fermenting marigold flower meal extracting solution as raw material and application |
| CN107468738A (en) * | 2017-09-22 | 2017-12-15 | 安徽菊泰滁菊草本科技有限公司 | A kind of extracting method of chrysanthemum total flavone |
| CN108851195A (en) * | 2018-07-26 | 2018-11-23 | 湖北中烟工业有限责任公司 | A kind of preparation method of cigarette alfalfa extract |
| CN108851195B (en) * | 2018-07-26 | 2021-05-18 | 湖北中烟工业有限责任公司 | Preparation method of alfalfa refined extract for cigarettes |
| CN111632076A (en) * | 2020-05-20 | 2020-09-08 | 伊犁师范大学 | Method for preparing total flavonoids of alpine yarrow herb by microwave-assisted enzymolysis |
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Application publication date: 20131225 |
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