CN102198163B - Preparation method of feverfew extractive - Google Patents
Preparation method of feverfew extractive Download PDFInfo
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- CN102198163B CN102198163B CN201110140250.1A CN201110140250A CN102198163B CN 102198163 B CN102198163 B CN 102198163B CN 201110140250 A CN201110140250 A CN 201110140250A CN 102198163 B CN102198163 B CN 102198163B
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Abstract
The invention provides a preparation method of a feverfew extractive. The extractive method taking the feverfew extractive as raw material comprises the following steps: 1) crushing the feverfew, soaking the crushed feverfew with water, carrying out enzymolysis to the crushed feverfew with a combination enzyme, filtering the mixture, and extracting residue with a hydrophilic solvent; 2) recovering extract to prepare a concentrated solution, and adding water into the concentrated solution to prepare precipitates I; 3) dissolving the precipitates I with an alkaline solution, and adding an acid solution to precipitate the mixture to prepare precipitates II; and drying the precipitates II, and recovering the dried precipitates II as the product. The preparation method adopts an enzymolysis and ethamol extraction mode, and has advantages simple process, low extraction cost, easiness in waste solution recovery, and no pollution to enviroment. The preparation method is suitable for industrial production.
Description
technical field: the preparation method that the present invention relates to Effective Component of Chinese Medicine separation technology field, particularly a kind of Feverfew P.E.
background technology: chryanthemum parthenium is the dry flowers of Compositae sagebruss chryanthemum parthenium, in China, has cultivation more, and the ornamental value that tool is certain can be used as medicine, and Chinese medicine is used for alleviating the symptoms such as nephralgia, dizziness, flatulence, vomiting, the malaise symptoms in the time of also can improving flu, fever.
The extract of chryanthemum parthenium contains many components.Although not every component is separated and evaluation all, known chryanthemum parthenium component contains a lot of biological active components.Nowadays, the chemical constituent of whole Feverfew P.E includes but not limited to 4',5,7-trihydroxyflavone-7-glucoside, 4',5,7-trihydroxyflavone-7-glucosiduronic acid, 1-β-hydroxyarbusculin, 6-campherol-3, 7-dimethyl ether, 8-β-reynosin, 10-epicanin, ascorbic acid, beta-carotene, calcium, chromium, Flos Chrysanthemi Indici glycosides, chrysanthemomin, chrysarten-A, chrysarten-C, chrysoeriol-7-glucosiduronic acid, cobalt, cosmosiin, epoxyartemorin, luteolin-7-glucoside, luteolin-7-glucosiduronic acid, mangnoliolide, parthenolide, quercetagitrin-3, 7, 3
,-tri-methyl ethers, quercetagitrin-3
,7-dimethyl ether, reynosin, tanaparthin, tanaparthin-1 α, 4 α-epoxide, tanaparthin-1 β, 4 beta epoxide compounds, β-costunolide, 3-beta-hydroxy-parthenolide, and 3,7,3
,-trimethoxy quercetagitrin.
Modern pharmacology research shows, the main bioactive ingredients of chryanthemum parthenium is sesquiterpenoids material, has the effects such as antiinflammatory, antioxidation and antitumor, and wherein studying more material is parthenolide, is a kind of sesquiterpene lactones material.Beautiful related researcher's recent findings, parthenolide has the leukemic effect for the treatment of, research shows that its mechanism is: parthenolide can be eliminated the stem cell that causes acute and chronic lymphocytic leukemia pointedly, can fundamentally contain the generation of this disease, this splits the disorders of blood new drug that turns white a good direction is provided.
At present the research about chryanthemum parthenium is mainly to its pharmacology aspect, relates to technique prepared by Feverfew P.E less, is really applied to the also rarely seen report of producing.US Patent No. 7537791 be take chryanthemum parthenium as raw material, and juice is soaked, squeezes and to be obtained to remove impurity, after washing, softly, after centrifugal, acid adjustment, microwave treatment, after recentrifuge, be dried to obtain finished product, this technique is simple, pollution-free, but due to the loss of active substance in expressing process, final yield is undesirable.US Patent No. 7229650 patents are passed through supercritical CO
2fluid extraction chryanthemum parthenium, thus prepare the Feverfew P.E of high yield, high level, due to supercritical apparatus expensive, be unfavorable for processing the large-scale production of large quantities of raw materials.
Chinese patent notification number is that CN101190258 be take Magnolia denudata as raw material, after water soaking, and alcohol extraction, petroleum ether extraction, the back extraction of alcohol liquid, organic solvent lixiviate, silicagel column remove impurity, reversed-phase column is separated, obtain after drying high-load parthenolide product, purity reaches 80-100%, and this process route is complicated, use silica gel remove impurity, be unfavorable for commercial production; Domestic patent CN101270102, has prepared the derivant of parthenolide by chemosynthesis mode, its side effect etc. are not yet studied.At present domestic directly about take chryanthemum parthenium as raw material, prepare the research of its extract and not yet report.
summary of the invention:the present invention is exactly the preparation method that a kind of Feverfew P.E will be provided, and it take chryanthemum parthenium plant as raw material production Feverfew P.E, adopts enzymolysis and alcohol extraction mode technique simple, extraction cost is low, be applicable to suitability for industrialized production, waste liquid easily reclaims, environment friendly and pollution-free.
Technical solution of the present invention is a kind of preparation method of Feverfew P.E, take chryanthemum parthenium as raw material, and extracting method is as follows:
1) by chryanthemum parthenium pulverizing water retting, combination enzyme enzymolysis, filters, and filtering residue extracts with hydrophilic solvent, extracting solution processed;
2) extracting solution reclaims solvent, concentrated solution processed, and concentrated solution adds water precipitate I processed;
3) precipitate I is dissolved with alkaline solution, then adds acid solution, precipitation, precipitate II processed; Precipitate II dried recovered is product.
The preparation method of Feverfew P.E of the present invention, preferably carry out as follows:
1) raw material is processed and enzymolysis:
By chryanthemum parthenium raw material pulverizing, and add and account for the heavy 8-12 times of deionized water of raw material, dipping 12-36 hour, is heated to 40-60 ℃, adds the combination enzyme enzymolysis processing 2-6 hour that accounts for the heavy 0.6-1.2% of raw material simultaneously, crosses filtering filtrate and obtains filtering residue;
2) extraction, Separation and Recovery:
In filtering residue, add the concentration 60-80wt% hydrophilic solvent reflux, extract, that accounts for heavy 6-10 times of raw material, filter to obtain extracting solution; Extracting solution is cooled to 5-20 ℃, standing 4-8 hour, centrifugalize obtains supernatant, reclaims solvent, obtains concentrated solution;
3) staticly settle, alkali liquor dissolves:
In concentrated solution, add its weight 1-3 water doubly, cooling, standing 8-72 hour, filters to obtain precipitate I; To adding in precipitate I, account for the alkaline solution that 10-20 times of concentration of its weight is 0.1-0.2wt%, stir 10-20 minute, filtrate is collected in standing filtration;
4) acid adjustment precipitation, dry products
To 3) to add concentration in step filtrate be 0.2-0.8wt% acid solution, stirs, regulating the pH value of filtrate solution is 1-3, and heating, after react, is cooled to 10-20 ℃, standing 10-20 hour, filtration collecting precipitation thing II; By precipitate II vacuum drying at 50-60 ℃ of temperature, obtain Feverfew P.E product.
Combination enzyme of the present invention is cellulase and the pectase ratio mixing of 2-1:1 in mass ratio.
Hydrophilic solvent of the present invention is C
1-C
4alcoholic solution, reflux, extract, at least 2 times, described C
1the alcoholic solution of-C is methanol, ethanol, propanol or butanols.
The present invention is that described alkaline solution is calcium hydroxide, sodium hydroxide or the sodium carbonate of concentration 0.1-0.2wt%; Described acid solution is hydrochloric acid, sulphuric acid or the phosphoric acid solution of concentration 0.2-0.8 wt ﹪.
Chryanthemum parthenium of the present invention is crushed to 10-50 order.
Extracting solution of the present invention adopts centrifugalize to reclaim, and control centrifuge speed is 10000-15000r/min.
Step of the present invention (3) stirs as after mechanical agitation, standing 50-90min.It is 40-50 ℃ that step 4) is controlled reacting by heating temperature, response time 10-50min.
Of the present invention being dried as vacuum drying, vacuum is-0.08～-0.06MPa.
The product that utilizes Feverfew P.E prepared by the inventive method, in HPLC high performance liquid chromatography testing product, chryanthemum parthenium lactone content reaches more than 2.5%, and yield is 10% left and right.
The preparation method that the invention provides a kind of Feverfew P.E, tool has the following advantages:
In process of the present invention, adopt enzymolysis and alcohol extraction mode, improved the leaching efficiency of active substance, improved yield;
Process of the present invention is brief, easy and simple to handle, adapts to the production of factory;
Process energy consumption of the present invention is less, uses solvent and reagent cheap, and production cost is low;
Process of the present invention is used material and waste liquid easily to reclaim, process, Environmental Safety.
the specific embodiment: in embodiment, relate to concentration and be quality than concentration, adopt HPLC and TLC to follow the tracks of and detect.
embodiment 1
The preparation method of a kind of Feverfew P.E that the embodiment of the present invention provides, realizes by following steps:
(1) raw material is processed: by the dry chryanthemum parthenium impurity removing of 10kg, pulverized 10-30 order;
(2) enzymolysis: to the deionized water that adds 80kg in the 10kg raw material after pulverizing, flood 18 hours, slowly be heated to after 50 ℃, the combination enzyme that adds wherein 60g, it consists of quality than cellulase: pectase is 1:1, and W/w processed after 3 hours, filtered, filtrate discards, and dries filtering residue standby;
(3) extract: in filtering residue, add 60kg concentration 60wt% alcohol reflux 2 times, filter, obtain extracting solution;
(4) centrifugal, recovery: extracting solution is cooled to 15 ℃, standing 4-8 hour, centrifugalize, centrifugal speed is 15000r/min, obtains centrifuged supernatant, then reclaims solvent to without till alcohol taste, obtains concentrated solution 8.75kg;
(5) standing, filtration: add after the water of 10kg in the concentrated solution of 8.75kg, be cooled to 20 ℃, standing 8 hours, filter collecting precipitation thing I approximately 0.45 kg;
(6) alkali liquor dissolves: in precipitate I, add the quality of about 4.6kg than concentration 0.1wt% aqua calcis, mechanical agitation, after approximately 10 minutes, standing 80 minutes, is filtered collection filtrate;
(7) acid adjustment precipitation: slowly add the hydrochloric acid solution quality of 0.2wt% than concentration in (6) step filtrate, limit edged stirs, and regulates PH to 2.5, be heated to 50 ℃ simultaneously, keep this temperature after 10 minutes, slowly cool to 20 ℃, after standing 10 hours, filter, collecting precipitation is precipitate II;
(8) dry: gained precipitate II to be placed in to vacuum drying oven and to be dried, baking temperature is 60 ℃, and vacuum is-0.08MPa with HPLC, to follow the tracks of the extract product that detects dry rear collection after being dried, product yield is 9.9%, and parthenolide content is 2.81%.
embodiment 2
The preparation method of Feverfew P.E is as follows:
(1) raw material pre-treatment: will be dried chryanthemum parthenium impurity removing, pulverize 10-30 order and obtain raw material 10kg;
(2) enzymolysis: to the deionized water that adds 120kg in the 10kg raw material after pulverizing, flood 24 hours, slowly be heated to after 50 ℃, the combination enzyme that adds wherein 120g, combination enzyme consists of quality than cellulase: pectase is 2:1, and W/w processed after 4 hours, filtered, filtrate discards, and dries filtering residue standby;
(3) extract: in filtering residue, add 100kg concentration 80wt% propanol countercurrent extraction 2 times, filter, obtain extracting solution;
(4) centrifugal, recovery: cooling extracting solution to 5 ℃, standing 8 hours, centrifugal, separated centrifugal speed was 15000r/min, obtains centrifuged supernatant, then reclaimed solvent to without till alcohol taste, obtained concentrated solution 15.8kg;
(5) standing, filtration: add after the water of 45kg in concentrated solution, be cooled to 10 ℃, standing 12 hours, filter collecting precipitation thing I approximately 0.51 kg;
(6) alkali liquor dissolves: in precipitate I, add the quality of about 5.5kg than concentration 0.1wt% aqua calcis, mechanical agitation, after approximately 20 minutes, standing 50 minutes, is filtered collection filtrate;
(7) acid adjustment precipitation: to the sulfuric acid solution that slowly adds 0.2wt% in (6) step filtrate, limit edged stirs, and regulates PH to 2.5, is heated to 50 ℃ simultaneously, keeps this temperature after 10 minutes, slowly cools to 10 ℃, after standing 20 hours, filters, and obtains precipitate II;
(8) dry: after precipitate II is dried with freeze-drying method, product detects by HPLC high performance liquid chromatography, and parthenolide content is 2.92%, product yield 12.2%.
embodiment 3
(1) raw material pre-treatment: by the dry chryanthemum parthenium impurity removing of 10kg, pulverized 40 orders;
(2) enzymolysis: the deionized water to adding 100kg in the 10kg raw material after pulverizing, flood 30 hours, slowly heat after 40 ℃, the combination enzyme that adds wherein 100g, consists of cellulase: pectase is 2:1, and W/w processed after 3 hours, filter, filtrate discards, and dries filtering residue standby;
(3) extract: in filtering residue, add 80kg70wt% alcohol reflux 2 times, filter, obtain extracting solution;
(4) centrifugal, recovery: cooling extracting solution to 10 ℃, standing 6 hours, centrifugalize, centrifugal speed is 15000r/min, obtains centrifuged supernatant, then reclaims solvent to without till alcohol taste, obtains concentrated solution 10.8kg;
(5) standing, filtration: add after the water of 25kg in concentrated solution, be cooled to 15 ℃, standing 10 hours, filter the about 4.8kg of collecting precipitation thing I;
(6) alkali liquor dissolves: to the 0.15wt% sodium hydroxide solution that adds approximately 7.5 kg in precipitate I, mechanical agitation is after approximately 15 minutes, and standing 40 minutes, filter, collect filtrate;
(7) acid adjustment precipitation: to the hydrochloric acid solution that slowly adds 0.6wt% in filtrate, limit edged stirs, and regulates PH to 2.5, heats to 50 ℃ simultaneously, keeps this temperature after 20 minutes, slowly cools to 15 ℃, after standing 15 hours, filters collecting precipitation thing II;
(8) dry: precipitate II is dried with spray drying process, and baking temperature is 60 ℃, after being dried, product is used HPLC to follow the tracks of and detects, and product yield is 10.6%, and parthenolide content is 2.79%.
embodiment 4
(1) raw material pre-treatment: will be dried chryanthemum parthenium impurity removing, pulverize 10-30 order;
(2) enzymolysis: the deionized water to adding 100kg in the 10kg raw material after pulverizing, flood 24 hours, slowly heat after 50 ℃, add wherein the combination enzyme (cellulase: pectase is 1:1, W/w) of 100g to process after 3 hours, filter, filtrate discards, and dries filtering residue standby;
(3) extract: in filtering residue, add 100kg 80wt% alcohol reflux 2 times, filter, obtain extracting solution;
(4) centrifugal, recovery: extracting solution is cooled to 10 ℃, and standing 8 hours, centrifugal, separated centrifugal speed was 15000r/min, obtains centrifuged supernatant, then reclaims solvent to without till alcohol taste, obtains concentrated solution 14.9kg;
(5) standing, filtration: add after the water of 35kg in concentrated solution, be cooled to 20 ℃, standing 12 hours, filter the about 0.46kg of collecting precipitation thing I;
(6) alkali liquor dissolves: in precipitate I, add the quality of about 9kg than concentration 0.2wt% aqua calcis, mechanical agitation, after approximately 10 minutes, standing 60 minutes, is filtered collection filtrate;
(7) acid adjustment precipitation: to the phosphoric acid solution that slowly adds 0.4wt% in filtrate, limit edged stirs, and regulates PH to 2.5, heats to 45 ℃ simultaneously, keeps this temperature after 30 minutes, slowly cools to 20 ℃, after standing 20 hours, filters collecting precipitation thing II;
(8) dry: precipitate II is placed in to vacuum drying oven and is dried, baking temperature is 60 ℃, vacuum is-0.08MPa, after being dried, to obtain product.With HPLC, follow the tracks of and detect, parthenolide content is 2.82%, and product yield is 11.3%.
Claims (7)
1. a preparation method for Feverfew P.E, take chryanthemum parthenium as raw material, and its extracting method is as follows:
1) raw material is processed and enzymolysis:
Chryanthemum parthenium is pulverized, and add and account for the heavy 8-12 times of deionized water of raw material, dipping 12-36 hour, is heated to 40-60 ℃, adds the combination enzyme enzymolysis processing 2-6 hour that accounts for the heavy 0.6-1.2% of raw material simultaneously, crosses filtering filtrate and obtains filtering residue;
2) extraction, Separation and Recovery:
In filtering residue, add the concentration 60-80wt% hydrophilic solvent reflux, extract, that accounts for heavy 6-10 times of raw material, filter to obtain extracting solution; Extracting solution is cooled to 5-20 ℃, standing 4-8 hour, centrifugalize obtains supernatant, reclaims solvent, obtains concentrated solution;
3) standing alkali liquor dissolves:
In concentrated solution, add its weight 1-3 water doubly, cooling, standing 8-72 hour, filters to obtain precipitate I; To adding in precipitate I, account for the alkaline solution that 10-20 times of concentration of its weight is 0.1-0.2wt%, stir 10-20 minute, filtrate is collected in standing filtration;
4) acid adjustment precipitation dry products:
To 3) to add concentration in step filtrate be 0.2-0.8wt% acid solution, stirs, regulating the pH value of filtrate solution is 1-3, and heating, after react, is cooled to 10-20 ℃, standing 10-20 hour, filtration collecting precipitation thing II; By precipitate II vacuum drying at 50-60 ℃ of temperature, obtain Feverfew P.E product;
Wherein said combination enzyme is cellulase and the pectase ratio mixing of 2-1:1 in mass ratio;
Wherein said hydrophilic solvent is C
1-C
4alcoholic solution, reflux, extract, at least 2 times, described C
1-C
4alcoholic solution be methanol, ethanol, propanol or butanols.
2. according to the preparation method of Feverfew P.E claimed in claim 1, it is characterized in that described alkaline solution is calcium hydroxide, sodium hydroxide or the sodium carbonate of concentration 0.1-0.3wt%; Described acid solution is hydrochloric acid, sulphuric acid or the phosphoric acid solution of concentration 0.2-0.8 wt ﹪.
3. according to the preparation method of Feverfew P.E claimed in claim 1, it is characterized in that described chryanthemum parthenium is crushed to 10-50 order.
4. according to the preparation method of Feverfew P.E claimed in claim 1, it is characterized in that extracting solution centrifugalize recovery, control centrifuge speed is 10000-15000r/min.
5. according to the preparation method of Feverfew P.E claimed in claim 1, it is characterized in that step (3) stirs as mechanical agitation, rear standing 50-90min.
6. according to the preparation method of Feverfew P.E claimed in claim 1, it is characterized in that 4) to control reacting by heating temperature be 40-50 ℃ to step, response time 10-50min.
7. according to the preparation method of Feverfew P.E claimed in claim 1, it is characterized in that described vacuum drying vacuum is-0.08～-0.06MPa.
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|---|---|---|---|
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| CN102198163B true CN102198163B (en) | 2014-10-22 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1498101A (en) * | 2001-03-16 | 2004-05-19 | ���Ǿ� | Composition containing feverfew extract and use thereof |
| CN101190258A (en) * | 2007-05-30 | 2008-06-04 | 北京星昊医药股份有限公司 | Total sesquiterpene lactone extract containing rich parthenolide and preparation method and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1498101A (en) * | 2001-03-16 | 2004-05-19 | ���Ǿ� | Composition containing feverfew extract and use thereof |
| CN101190258A (en) * | 2007-05-30 | 2008-06-04 | 北京星昊医药股份有限公司 | Total sesquiterpene lactone extract containing rich parthenolide and preparation method and application thereof |
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