CN1439367A - Pratensein extraction and preparation thereof - Google Patents
Pratensein extraction and preparation thereof Download PDFInfo
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- CN1439367A CN1439367A CN 03118845 CN03118845A CN1439367A CN 1439367 A CN1439367 A CN 1439367A CN 03118845 CN03118845 CN 03118845 CN 03118845 A CN03118845 A CN 03118845A CN 1439367 A CN1439367 A CN 1439367A
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Abstract
An extract of red clover herb is prepared through extracting in methanol or alcohol, filtering, concentrating, centrifugal separating to obtain dregs, deoiling and drying with petroleum ether or n-hexane, extracting with ethylacetate, concentrating, crystallizing to obtain extract A, extracting from the extracted dregs in alcohol, recovering alcohol to obtain concentrated liquid, regulating the pH value of its mother liquid and the concentrated liquid to 8-10, separating by microreticular resin adsorbent to obtain extract B, mixing A with B, and refining. It can be used along with epimedium, VB1 and VB6 to prepare the medicine for preventing and treating breast cancer, prostatic cancer, colon cancer, osteoporosis and climacteric syndrome.
Description
Technical field
The invention belongs to extract and the preparation thereof of Herba Trifolii Pratentis, wherein the extract of Herba Trifolii Pratentis can get crystallize by centrifugal, ethyl acetate extraction, the further alcohol extraction of mother solution and recrement, by transferring pH value, last macroporous adsorbent resin obtains further refining the separation, and obtains the red clover total isoflavones extract.
Background technology
Herba Trifolii Pratentis has another name called Trifolium pratense, red bean grass, red clover, Flos Carthami car, Herba Trifolii Pratentis, Herba Loti Tenuis etc.It (is sesame handle florigen (formononetin) and A (biochaninA), genistein (genistein), big legumin (daidzein), pratensein, SANYE Lignum pterocarpi indici glycoside, linariin that the Herba Trifolii Pratentis herb contains the plain B of multiple flavones ingredient chemical compound chick pea bud, still contain a and beta-carotene, vitamin D, E, saccharide and starch in the herb, also find to contain three kinds of flavonols chemical compounds at present.
In fact, people's researcher before 40 years just finds that the sheep reproductivity in some pasture of Australia is strong, researcher finds that this is because contain special Herba Trifolii Pratentis plant in the pasture, wherein being rich in sesame handle florigen is the plain B of chick pea bud, and it is one of a few plant that contains 4 kinds of isoflavone (phytoestrogen).Osajin estrogen mainly comprises genistein isoflavone and daidzein.The genistein isoflavone is transformed by the plain A of its precursor chick pea bud, and metabolism is that no estrogen is active to ethyl phenol, and the former precursor of daiazi is formononetin, daiazi, and metabolism is equol and oxygen-demethyl angolensin (0-DMA).Isoflavone in the plant mostly is the glucosides of combining form greatly, and under the intestinal effect, removing glucosides is the aglycone that the non-binding form of biological activity is arranged, and through different activation metabolic pathway, produces different metabolites, after the absorption through enterohepatic circulation.Most of in liver and glucuronic acid combination, small part is discharged with the form of sulfate, sulphuric acid glucuronide.
Modern study confirms that red clover total isoflavones has following effect:
(1) effect of similar female estrogen effect and hormone antagonist;
(2) effect, particularly cheese egg acid kinase of inhibition and cancer related enzyme activity;
(3) has the effect of the blood vessel hyperplasia of inhibition in the promotion stage of cancer cell multiplication;
(4) elimination activity oxygen, thus antioxidation had;
(5) regulate cell cycle;
(6) the genistein isoflavone has and suppresses some and with the DNA cut-out effect of enzymatic activity is arranged in addition.
In a word, the Herba Trifolii Pratentis isoflavone plays certain prophylaxis of cancer effect by different preparations, particularly weak estrogen action.Can play the class estrogenic effect during oestrogen deficiencies, and estrogen plays estrogenic antagonist again, i.e. dual regulation when superfluous.For Breast Cancer Prevention, carcinoma of prostate, colon cancer, improve osteoporosis and improve Woman climacteric symptom etc. and have certain effect, and be applied to clinical more and more widely.
Summary of the invention
Present commercially available Herba Trifolii Pratentis extract content most about 10%, have been found that stable now, particularly has the different ketone extract of active red clover total, it contains the main compound that pharmacologically active is worked, specifically be plain A of chick pea bud and B, genistein, big legumin, daiazi etc., it can make by such method, and this method comprises the following steps:
(1) with methanol or ethanol extraction Herba Trifolii Pratentis herb;
(2) filter this extracting solution and concentrated;
(3) with concentrated solution centrifuging and taking slag;
(4) medicinal residues are used the oil-based solvent degreaser drying;
(5) concentrate with the extraction of aliphatic esters after, crystallize obtains extract a;
(6) will be insoluble to of the alcohol extraction of the medicinal residues of esters in the step (5), and extracting solution is concentrated with 50-90%;
(7) concentrated solution in mother solution behind the middle crystallize of step (5) and the step (6) is transferred in pH value=8-10, crossed the polystyrene macroporous adsorbent resin and separate, get extract b;
(8) extract obtained a and b are merged, re-refine with alcohol.
The specific embodiment
Preferred realization method of the present invention is to carry out extracting for the first time the heavy volume ratio of (step (1)) medical material and solvent in 1: 2 to 1: 20 scope with methanol or ethanol, be preferably in 1: 2 to 1: 10 the scope, temperature is in room temperature arrives the range of circulating flow of solvent, preferably at 50-80 ℃.
Being used for step (4) gained medicinal residues is centrifugal gained or natural subsidence gained.
It is preferred between 200# industrial naptha, petroleum ether, the n-hexane being used for the described degreasing solvent of step (4), and n-hexane is best.
The aliphatic esters that is used for step (5) is preferred between ethyl acetate, methyl acetate or the butyl acetate, and ethyl acetate is best.
Described degreasing solvent ratio is preferred within 1: 2 to 1: 10 scope, and the best is 1: 4.
Described esters solvent is interior preferred with 1: 2 to 1: 10 scope of volume ratio, and the best is 1: 10.The most handy new equal portions solvent repeats to extract, and generally at least 3 times, it is 1.02-1.15 that the gained extracting solution is concentrated into relative density with it, sufficient standing and realize that this step gained total isoflavone content is between the 30-60%.
The extraction of carrying out step (6) is that used methanol or concentration of alcohol are preferably between the 5-95% for abundant total isoflavone with its slag the inside fully extracts fully, and the best is between the 50-80%.
Carrying out step (7) is mother liquid obtained and step (6) gained concentrated solution merging with step (5), and the remove impurity of re-refining is because the Herba Trifolii Pratentis active substance is water insoluble, so it must be transferred pH value=8-10, to allow it fully dissolve, the pH value preferable range is between pH value=8-11, and the best is pH value=9.
Realize that the selected range of resin of this step is silica gel, polyamide, ion exchange resin, macroporous adsorbent resin, be preferably macroporous resin for best.
Performing step (8) is that selected solvent is methanol, ethanol, ethyl acetate, acetone for extract obtained content further improves, and is best with ethanol.
The factor that influences this extraction and purification process has the content of total isoflavone in the quality of raw material and the practical operation situation in the course of processing, the raw material should be not less than 0.6%, this content than big-difference depend on the time of collecting this plant and handle exsiccant mode and this raw medicinal herbs in the shared ratio of stem.
Compare with total extract, be used for preventing and treating various that this extract unexpectedly has high activity in climacteric syndrome, the osteoporosis pharmacology model, and do not need further special handling, As time goes on activity is stable.
The invention provides a kind of application Herba Epimedii, vitamin B
1, B
6And contain vitamin for combination and Herba Trifolii Pratentis compatibility, and under instruction of Chinese Medicine theory, the kidney invigorating, replenish phytoestrogen, it is not fully exerted, thus Breast Cancer Prevention, carcinoma of prostate, colon cancer and prevent and treat osteoporosis, climacteric syndrome better.
The application of this invention is described with embodiment below, but should not be construed as limitation of the present invention.
The composition proportioning of Herba Trifolii Pratentis extract and other drug composition is as follows:
Herba Trifolii Pratentis extract 30g
Herba Epimedii extract 60g
Microcrystalline Cellulose 120g
Starch 105g
With above composition mixing, tabletting, the tablet that makes is mainly used in complementing estrogen, Breast Cancer Prevention.
Herba Trifolii Pratentis extract is according to the preparation method preparation of summary of the invention in the said ratio, wherein contain red clover total isoflavones 50-70%, Herba Epimedii extract is oneself preparation or purchase, wherein contained Herba Epimedii total flavones is 50-60%, microcrystalline Cellulose and starch are the known pharmaceutical aids of this area professional, mainly as filler and disintegrating agent.
Claims (10)
1. prepare the method for Herba Trifolii Pratentis extract, it comprises:
(1) with methanol or ethanol extraction Herba Trifolii Pratentis herb;
(2) filter this extracting solution and concentrated;
(3) with concentrated solution centrifuging and taking slag;
(4) medicinal residues are used the oil-based solvent degreaser drying;
(5) concentrate with the extraction of aliphatic esters after, crystallize obtains extract a;
(6) mother solution behind the crystallize in the step (5) is transferred in pH value=8-10, crossed resin isolation, get extract b;
(7) extract obtained a and b are merged, re-refine with alcohol.
2. the method for claim 1 wherein is insoluble to the alcohol extraction of the slag of esters with 50-90% in the step (5), reclaim alcohol and obtain concentrated solution, and this concentrated solution mixes with mother solution behind step (5) crystallize.
3. the method for claim 1 is carried out the extraction of step (1) with methanol or ethanol.
4. the method for claim 1 is wherein carried out the defat of step (4) with 200# industrial naptha, petroleum ether or n-hexane, and n-hexane is best.
5. the method described in claim 1, wherein used aliphatic esters is selected from ethyl acetate, methyl acetate or butyl acetate in the step (5), and ethyl acetate is best.
6. the method for claim 1, wherein step (6) range of resin is silica gel, polyamide, ion exchange resin, macroporous adsorbent resin, macroporous adsorbent resin is best.
7. the method for claim 1, wherein the recrystallization of step (7) is selected from 95% methanol, ethanol or acetone, and ethanol is best.
8. the method according to claim 1-7 gets the high-load Herba Trifolii Pratentis extract.
9. according to the described extract of claim 8, it contains the total isoflavone of 10-85% (weight).
10. claim 8 or 9 extract are prevented and treated the application of the medicine of climacteric syndrome, osteoporosis in the preparation complementing estrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03118845 CN1439367A (en) | 2003-03-27 | 2003-03-27 | Pratensein extraction and preparation thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 03118845 CN1439367A (en) | 2003-03-27 | 2003-03-27 | Pratensein extraction and preparation thereof |
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| CN1439367A true CN1439367A (en) | 2003-09-03 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1305869C (en) * | 2004-05-21 | 2007-03-21 | 薛存宽 | Tech. for preparing isoflavone of red clover from red clover |
| WO2008120105A3 (en) * | 2007-03-30 | 2009-02-05 | 9898 Ltd | Pharmaceutical platform technology for the development of natural products |
| CN1981799B (en) * | 2006-05-25 | 2010-11-10 | 湖南省中药提取工程研究中心有限公司 | Preparing method for extracts of red clover |
| CN101684431B (en) * | 2008-09-27 | 2012-07-18 | 湖北中烟工业有限责任公司 | Method for enriching and purifying furfural products in clover extracts by molecular distillation |
| CN101559094B (en) * | 2009-05-16 | 2012-09-05 | 花垣恒远植物生化有限责任公司 | Production technique for extracting and separating isoflavone from red clover |
| CN103251050A (en) * | 2013-05-10 | 2013-08-21 | 龙岩学院 | Method for preparing trifolium pretense oral liquid |
| CN106913613A (en) * | 2017-04-01 | 2017-07-04 | 林婷 | A kind of antitumor use flavone extract and its manufacture method |
| CN109276589A (en) * | 2018-11-08 | 2019-01-29 | 浙江中医药大学 | A kind of clover extract improves the application in sleep drug in preparation |
| CN112125894A (en) * | 2020-09-30 | 2020-12-25 | 内蒙古民族大学 | Method for green and efficient extraction of red clover isoflavone by using natural deep eutectic solvent |
-
2003
- 2003-03-27 CN CN 03118845 patent/CN1439367A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1305869C (en) * | 2004-05-21 | 2007-03-21 | 薛存宽 | Tech. for preparing isoflavone of red clover from red clover |
| CN1981799B (en) * | 2006-05-25 | 2010-11-10 | 湖南省中药提取工程研究中心有限公司 | Preparing method for extracts of red clover |
| WO2008120105A3 (en) * | 2007-03-30 | 2009-02-05 | 9898 Ltd | Pharmaceutical platform technology for the development of natural products |
| CN101790682A (en) * | 2007-03-30 | 2010-07-28 | 9898有限公司 | Pharmaceutical platform technology for the development of natural products |
| CN101684431B (en) * | 2008-09-27 | 2012-07-18 | 湖北中烟工业有限责任公司 | Method for enriching and purifying furfural products in clover extracts by molecular distillation |
| CN101559094B (en) * | 2009-05-16 | 2012-09-05 | 花垣恒远植物生化有限责任公司 | Production technique for extracting and separating isoflavone from red clover |
| CN103251050A (en) * | 2013-05-10 | 2013-08-21 | 龙岩学院 | Method for preparing trifolium pretense oral liquid |
| CN106913613A (en) * | 2017-04-01 | 2017-07-04 | 林婷 | A kind of antitumor use flavone extract and its manufacture method |
| CN109276589A (en) * | 2018-11-08 | 2019-01-29 | 浙江中医药大学 | A kind of clover extract improves the application in sleep drug in preparation |
| CN109276589B (en) * | 2018-11-08 | 2022-03-18 | 浙江中医药大学 | Application of herba Trifolii Pratentis extract in preparation of sleep improving medicine |
| CN112125894A (en) * | 2020-09-30 | 2020-12-25 | 内蒙古民族大学 | Method for green and efficient extraction of red clover isoflavone by using natural deep eutectic solvent |
| CN112125894B (en) * | 2020-09-30 | 2022-05-27 | 内蒙古民族大学 | Method for green and efficient extraction of red clover isoflavone by using natural deep eutectic solvent |
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