CN105287677A - Method for extracting and further processing ainsliaea fragrans total flavonoid - Google Patents
Method for extracting and further processing ainsliaea fragrans total flavonoid Download PDFInfo
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- CN105287677A CN105287677A CN201510838753.4A CN201510838753A CN105287677A CN 105287677 A CN105287677 A CN 105287677A CN 201510838753 A CN201510838753 A CN 201510838753A CN 105287677 A CN105287677 A CN 105287677A
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Abstract
The invention relates to the technical field of Chinese pharmaceutical manufacturing, particularly to a method for extracting and further processing ainsliaea fragrans total flavonoid. With ainsliaea fragrans adopted as the raw medicinal material, the method comprises the following steps: firstly, smashing ainsliaea fragrans; carrying out ultrasonic immersion extraction on the smashed ainsliaea fragrans in ethanol water for a plurality of times; then, combining extracting solutions; decompressing and concentrating the extracting solutions; adding ethyl alcohol into the concentrated solution, and carrying out low-temperature standing for alcohol precipitation; filtering with a micropore filter membrane; decompressing and concentrating the filtrate; carrying out vacuum drying on the concentrated solution to obtain refined ainsliaea fragrans total flavonoid extract; finally, adding pharmaceutical excipients for further preparing the ainsliaea fragrans total flavonoid extract into various pharmaceutical preparations. According to the method, ultrasonic wave and continuous countercurrent extraction technologies are combined, so that the dissolution and spreading of the effective components are quickened, the extraction time is greatly shortened, the extraction efficiency is improved, the degradation of heat sensitive components is avoided, the energy consumption and production cost are further reduced, the extraction preparation technology is relatively simple and convenient, and the method is applicable to industrial large-scale production.
Description
Technical field
The invention belongs to Chinese medicine extraction and deep process technology field, be specifically related to the method for the fragrant Herba Ainsliaeae Glabrae total flavones extraction of a kind of Fructus Pruni and deep processing.
Background technology
The fragrant Herba Ainsliaeae Glabrae of Fructus Pruni is the dry herb of Compositae Ainsliaea fragrans Champ. platymiscium Ainsliasa fragrans Champ (AinsliaeafragransChamp).The fragrant Herba Ainsliaeae Glabrae of Fructus Pruni, have heat-clearing and toxic substances removing, removing food stagnancy eliminating stagnation, cough-relieving, the effects such as hemostasis, are usually used in upper respiratory tract infection, lung abscess, hemoptysis of pulmonary tuberculosis, jaundice, infantile malnutrition, dyspepsia, mastitis, otitis media, the treatment of acute and chronic cervicitis and venom etc.The fragrant Herba Ainsliaeae Glabrae of Fructus Pruni, as a common medicine among the people, but literature research report is also few at present; its chemical composition is mainly divided into flavonoid, terpenoid and phenolic acids etc., all has certain pharmacologically active, wherein; total flavonoid content is relatively abundant, is suitable for large-scale production application.
In recent years, about the patent of the application of Ainsliasa fragrans Champ extracting method or mandate mainly comprises: China Patent Publication No.: CN101380347A discloses the patent of invention of a kind of by name " Ainsliaea fragrans Champ total flavone extract and extracting method and purposes " thereof, adopt traditional alcohol reflux and macroporous adsorbent resin isolation technics to carry out obtained Ainsliaea fragrans Champ total flavone extract, the method easily destroys heat-sensitive ingredients, organic solvent used is more, easy generation organic solvent residual and affect the quality of medicine, and operation is comparatively loaded down with trivial details, production cost is higher; Chinese patent Authorization Notice No.: CN101293003B discloses the patent of invention of " fragrant Herba Ainsliaeae Glabrae effective site of a kind of Fructus Pruni and preparation method thereof and application " by name, first pass through ethanol percolate extraction, successively add petroleum ether and extraction into ethyl acetate again, finally obtain total phenolics composition; Chinese patent Authorization Notice No.: CN101332216B discloses the patent of invention of a kind of " fragrant Herba Ainsliaeae Glabrae total phenolic acid extract of Fructus Pruni and preparation method thereof " by name, also be by traditional alcohol reflux, and adjust pH to be separated obtained Xingsiang Tuerfeng total phenolic acid with macroporous adsorbent resin with hydrochloric acid; Chinese patent Authorization Notice No.: CN102100720B discloses the patent of invention of a kind of " the fragrant Herba Ainsliaeae Glabrae coffee mesitoyl quinine acid extract of Fructus Pruni and preparation and application thereof " by name, also be first by traditional alcohol reflux, and regulate pH with dilute hydrochloric acid, adsorb through macroporous resin HPD-826 again, eluting, hydrochloric acid adjusts pH again, then adsorbs through macroporous resin HPD-826, eluting, final drying obtains product; China Patent Publication No.: CN103933094A discloses the patent of invention of " the fragrant Herba Ainsliaeae Glabrae extract of a kind of Fructus Pruni and extracting method, application " thereof by name, first use ethyl acetate heating extraction, concentrate drying obtains ethyl acetate extract, and methanol heating and refluxing extraction used again by medicinal residues, obtains methanolic extract.
These published documents and patent are all that fragrant for Fructus Pruni Herba Ainsliaeae Glabrae is extracted its effective ingredient by traditional extracting method means, these traditional extraction processes also exist general defect and deficiency, comprising: extraction process is more complicated, heating easily causes the destruction of heat-sensitive ingredients, use a large amount of organic reagent during extraction, easily cause the organic solvent residual of extract, extraction efficiency is low, energy consumption and production cost higher, lower etc. to the utilization rate of medical material.
What the present invention relates to is that the fragrant Herba Ainsliaeae Glabrae total flavones of a kind of Fructus Pruni extracts and the new method of deep processing, from our documents and materials of retrieving at present, there is no the document and patent published, also without relevant report.
Summary of the invention
The object of this invention is to provide a kind of extraction process advanced, the fragrant Herba Ainsliaeae Glabrae total flavones of Fructus Pruni of technology maturation extracts and deep working method, by utilizing ultrasonic countercurrent extraction and membrane filtration technique, overcomes defect and the deficiency of the fragrant Herba Ainsliaeae Glabrae traditional extraction technique of existing Fructus Pruni.
The object of the invention is to be achieved by the following technical programs.
A method for the fragrant Herba Ainsliaeae Glabrae total flavones extraction of Fructus Pruni and deep processing, with the fragrant Herba Ainsliaeae Glabrae of Fructus Pruni for raw material, it is characterized in that, the method comprises the following steps:
(1) crude drug pretreatment: the medicinal pulverizer of the fragrant Herba Ainsliaeae Glabrae crude drug of Fructus Pruni is ground into former medicated powder;
(2) ultrasonic countercurrent extraction: the former medicated powder of step (1) is put into continuous single stage type reverse-flow ultrasonic extracting machine, 50% ethanol water being incorporated as former medicated powder 8 times amount is ultrasonic countercurrent extraction 30-45min under the room temperature condition of 40-80KHz at ultrasonic power, filter extracting solution, collect filtrate and filtering residue, filtering residue repeats ultrasonic countercurrent extraction 2-3 time again, and refilter after each extraction, merging filtrate;
(3) concentrated: by the filtrate of step (2) at vacuum 0.85 ~ 0.95Mpa, 60 DEG C of concentrating under reduced pressure become relative density to be the clear paste of 1.05-1.25;
(4) precipitate with ethanol: the alcoholic solution low temperature precipitate with ethanol 24h at the 4-10 DEG C clear paste that step (3) is concentrated being incorporated as 80% of clear paste 6 times amount;
(5) filter and concentrate: by the clear paste filtering with microporous membrane after step (4) precipitate with ethanol, decompression filtrate recycling ethanol, and during simmer down to 60 DEG C, relative density is the clear paste of 1.2-1.3;
(6) dry: the condition of clear paste reduced vacuum drying step (5) concentrated is temperature is 60 DEG C, and vacuum is 0.01-0.1MPa, the water content of the fragrant Herba Ainsliaeae Glabrae extractive of general flavone of Fructus Pruni is 0.5%-3%, and general flavone content reaches 60%-85%;
(7) deep processing: the Ainsliaea fragrans Champ total flavone extract obtained by step (6) is added wherein one or more pharmaceutic adjuvants such as starch, dextrin, sucrose, microcrystalline Cellulose, magnesium stearate, makes granule, tablet or capsule by fragrant for Fructus Pruni Herba Ainsliaeae Glabrae extractive of general flavone.
The invention has the beneficial effects as follows: by utilizing ultrasonic countercurrent extraction and membrane filtration technique, overcome defect and the deficiency of the fragrant Herba Ainsliaeae Glabrae traditional extraction technique of existing Fructus Pruni, ultrasound wave combines with Continuous Countercurrent Extraction technology, accelerate stripping and the diffusion of active ingredient, effectively shorten extraction time, extraction efficiency is for improving, avoid the degraded of heat-sensitive ingredients, and extract is not containing organic solvent, reduce energy consumption and production costs, extraction and preparation technique is also relatively easy, provide a kind of extractive technique advanced, the method of the Fructus Pruni fragrant Herba Ainsliaeae Glabrae extract industrialized great production of technical maturity.
Detailed description of the invention
Below by way of specific embodiment, the invention will be further described; it should be understood that; these embodiments only illustrate the technical scheme of application claims protection, and any restriction not to these technical schemes, the content that protection scope of the present invention is recorded with appending claims is as the criterion.
embodiment 1
Crude drug pretreatment: the medicinal pulverizer of the fragrant Herba Ainsliaeae Glabrae crude drug of Fructus Pruni is ground into former medicated powder;
Ultrasonic countercurrent extraction: 1 kilogram of former medicated powder is put into continuous single stage type reverse-flow ultrasonic extracting machine, 50% ethanol water being incorporated as former medicated powder 8 times amount is ultrasonic countercurrent extraction 30min under the room temperature condition of 80KHz at ultrasonic power, filter extracting solution, collect filtrate and filtering residue, filtering residue repeats ultrasonic countercurrent extraction 2 times again, and refilter after each extraction, merging filtrate;
Concentrated: by filtrate at vacuum 0.85 ~ 0.95Mpa, 60 DEG C of concentrating under reduced pressure become relative density be 1.25 clear paste;
Precipitate with ethanol: the alcoholic solution low temperature precipitate with ethanol 24h at the 4 DEG C clear paste that step (3) is concentrated being incorporated as 80% of clear paste 6 times amount;
To filter and concentrated: by the clear paste filtering with microporous membrane after precipitate with ethanol, decompression filtrate recycling ethanol, and when being condensed into 60 DEG C, relative density is the clear paste of 1.25;
Dry: be temperature by the condition of concentrated clear paste reduced vacuum drying to be 60 DEG C, vacuum is 0.01-0.1MPa, and the water content of the fragrant Herba Ainsliaeae Glabrae extractive of general flavone of Fructus Pruni is about 2%, and general flavone content reaches 80%;
Deep processing: obtained Ainsliaea fragrans Champ total flavone extract is added the pharmaceutic adjuvants such as starch, dextrin, microcrystalline Cellulose and magnesium stearate, makes tablet further by fragrant for Fructus Pruni Herba Ainsliaeae Glabrae extractive of general flavone.
embodiment 2
Crude drug pretreatment: the medicinal pulverizer of the fragrant Herba Ainsliaeae Glabrae crude drug of Fructus Pruni is ground into former medicated powder;
Ultrasonic countercurrent extraction: 1 kilogram of former medicated powder is put into continuous single stage type reverse-flow ultrasonic extracting machine, 50% ethanol water being incorporated as former medicated powder 8 times amount is ultrasonic countercurrent extraction 40min under the room temperature condition of 60KHz at ultrasonic power, filter extracting solution, collect filtrate and filtering residue, filtering residue repeats ultrasonic countercurrent extraction 3 times again, and refilter after each extraction, merging filtrate;
Concentrated: by filtrate at vacuum 0.85 ~ 0.95Mpa, 60 DEG C of concentrating under reduced pressure become relative density be 1.20 clear paste;
Precipitate with ethanol: the alcoholic solution low temperature precipitate with ethanol 24h at 6 DEG C concentrated clear paste being incorporated as 80% of clear paste 6 times amount;
To filter and concentrated: by the clear paste filtering with microporous membrane after precipitate with ethanol, decompression filtrate recycling ethanol, and when being condensed into 60 DEG C, relative density is the clear paste of 1.30;
Dry: be temperature by the condition of concentrated clear paste reduced vacuum drying to be 60 DEG C, vacuum is 0.01-0.1MPa, and the water content of the fragrant Herba Ainsliaeae Glabrae extractive of general flavone of Fructus Pruni is 3%, and general flavone content reaches 85%;
Deep processing: obtained Ainsliaea fragrans Champ total flavone extract is added the pharmaceutic adjuvants such as starch, dextrin, sucrose, is processed as granule further by fragrant for Fructus Pruni Herba Ainsliaeae Glabrae extractive of general flavone.
embodiment 3
Crude drug pretreatment: the medicinal pulverizer of the fragrant Herba Ainsliaeae Glabrae crude drug of Fructus Pruni is ground into former medicated powder;
Ultrasonic countercurrent extraction: 1 kilogram of former medicated powder is put into continuous single stage type reverse-flow ultrasonic extracting machine, 50% ethanol water being incorporated as former medicated powder 8 times amount is ultrasonic countercurrent extraction 45min under the room temperature condition of 40KHz at ultrasonic power, filter extracting solution, collect filtrate and filtering residue, filtering residue repeats ultrasonic countercurrent extraction 3 times again, and refilter after each extraction, merging filtrate;
Concentrated: by filtrate at vacuum 0.85 ~ 0.95Mpa, 60 DEG C of concentrating under reduced pressure become relative density be 1.05 clear paste;
Precipitate with ethanol: the alcoholic solution low temperature precipitate with ethanol 24h at 10 DEG C concentrated clear paste being incorporated as 80% of clear paste 6 times amount;
To filter and concentrated: by the clear paste filtering with microporous membrane after precipitate with ethanol, decompression filtrate recycling ethanol, and when being condensed into 60 DEG C, relative density is the clear paste of 1.2;
Dry: be temperature by the condition of concentrated clear paste reduced vacuum drying to be 60 DEG C, vacuum is 0.01-0.1MPa, and the water content of the fragrant Herba Ainsliaeae Glabrae extractive of general flavone of Fructus Pruni is 0.5%, general flavone content about 60%;
Deep processing: obtained Ainsliaea fragrans Champ total flavone extract is added the pharmaceutic adjuvant such as starch and dextrin, is processed into capsule further by fragrant for Fructus Pruni Herba Ainsliaeae Glabrae extractive of general flavone.
Claims (6)
1. a method for the fragrant Herba Ainsliaeae Glabrae total flavones extraction of Fructus Pruni and deep processing, with the fragrant Herba Ainsliaeae Glabrae of Fructus Pruni for raw material, it is characterized in that, the method comprises the following steps:
Crude drug pretreatment: the medicinal pulverizer of the fragrant Herba Ainsliaeae Glabrae crude drug of Fructus Pruni is ground into former medicated powder;
Ultrasonic countercurrent extraction: the former medicated powder of step (1) is put into continuous flow upstream ultrasonic extractor, ultrasonic countercurrent extraction after adding ethanol water, filters extracting solution, collect filtrate and filtering residue, filtering residue repeats ultrasonic countercurrent extraction 2-3 time again, and refilters after each extraction, merging filtrate;
Concentrated: by the filtrate reduced in volume of step (2), reclaiming ethanol, is the clear paste of 1.05-1.25 to relative density when 60 DEG C;
Precipitate with ethanol: the ethanol low temperature clear paste that step (3) is concentrated being added 80% is placed, precipitate with ethanol 24h;
To filter and concentrated: by the clear paste filtering with microporous membrane after step (4) precipitate with ethanol, decompression filtrate recycling ethanol, and when being condensed into 60 DEG C, relative density is the clear paste of 1.20-1.30;
Dry: by dry for clear paste reduced vacuum concentrated for step (5), to obtain refining Ainsliaea fragrans Champ total flavone extract;
Deep processing: the Ainsliaea fragrans Champ total flavone extract obtained by step (6) is added pharmaceutic adjuvant, and pharmaceutical formulation is made in further deep processing.
2. the method for the fragrant Herba Ainsliaeae Glabrae total flavones extraction of a kind of Fructus Pruni according to claim 1 and deep processing, it is characterized in that: the continuous flow upstream ultrasonic extractor described in step (2) is single stage type 6 pipe joint, wherein 1-2 joint is soak extraction pipe, 3-6 joint is supersound extraction pipe, and 50% ethanol water being incorporated as former medicated powder 8 times amount is each ultrasonic countercurrent extraction 30-45min under the room temperature condition of 40-80KHz at ultrasonic power.
3. the method for the fragrant Herba Ainsliaeae Glabrae total flavones extraction of a kind of Fructus Pruni according to claim 1 and deep processing, is characterized in that: described step (3) filtrate is at vacuum 0.85 ~ 0.95Mpa, and 60 DEG C of concentrating under reduced pressure become the clear paste of 1.05-1.25.
4. the fragrant Herba Ainsliaeae Glabrae total flavones of a kind of Fructus Pruni according to claim 1 extracts and the method for deep processing, it is characterized in that: described step (4) refer to be incorporated as clear paste 6 times amount 80% ethanol low temperature precipitate with ethanol 24h at 4-10 DEG C.
5. the method for the fragrant Herba Ainsliaeae Glabrae total flavones extraction of a kind of Fructus Pruni according to claim 1 and deep processing, it is characterized in that: the condition of described step (6) reduced vacuum drying is temperature is 60 DEG C, vacuum is 0.01-0.1MPa, the water content of the fragrant Herba Ainsliaeae Glabrae extractive of general flavone of Fructus Pruni is 0.5%-3%, and general flavone content reaches 60%-85%.
6. the method for the fragrant Herba Ainsliaeae Glabrae total flavones extraction of a kind of Fructus Pruni according to claim 1 and deep processing, it is characterized in that: the deep processing of described step (7) specifically refers to and adds wherein one or more pharmaceutic adjuvants such as starch, dextrin, sucrose, microcrystalline Cellulose, magnesium stearate, fragrant for Fructus Pruni Herba Ainsliaeae Glabrae extractive of general flavone is made granule, tablet or capsule.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105582132A (en) * | 2016-03-07 | 2016-05-18 | 南京多宝生物科技有限公司 | Preparation method and application of liquorice root formulation granules |
| CN105616468A (en) * | 2016-03-03 | 2016-06-01 | 陈爱华 | Radix et caulis acanthopanacis senticosi extracting method and radix et caulis acanthopanacis senticosi health care product |
| CN105748542A (en) * | 2016-03-07 | 2016-07-13 | 南京多宝生物科技有限公司 | Preparation method and application of angelica sinensis formula granules |
| CN105748572A (en) * | 2016-03-07 | 2016-07-13 | 南京多宝生物科技有限公司 | Preparation method and application of astragalus formula granule |
| CN105748550A (en) * | 2016-03-04 | 2016-07-13 | 陈爱华 | Maca extraction method and Maca health care product |
| CN105769984A (en) * | 2016-04-04 | 2016-07-20 | 孙爱华 | Extraction method of liquorice and antiviral medicine |
| CN115261142A (en) * | 2022-08-29 | 2022-11-01 | 西藏天虹科技股份有限责任公司 | Saffron extraction process and device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105616468A (en) * | 2016-03-03 | 2016-06-01 | 陈爱华 | Radix et caulis acanthopanacis senticosi extracting method and radix et caulis acanthopanacis senticosi health care product |
| CN105748550A (en) * | 2016-03-04 | 2016-07-13 | 陈爱华 | Maca extraction method and Maca health care product |
| CN105582132A (en) * | 2016-03-07 | 2016-05-18 | 南京多宝生物科技有限公司 | Preparation method and application of liquorice root formulation granules |
| CN105748542A (en) * | 2016-03-07 | 2016-07-13 | 南京多宝生物科技有限公司 | Preparation method and application of angelica sinensis formula granules |
| CN105748572A (en) * | 2016-03-07 | 2016-07-13 | 南京多宝生物科技有限公司 | Preparation method and application of astragalus formula granule |
| CN105769984A (en) * | 2016-04-04 | 2016-07-20 | 孙爱华 | Extraction method of liquorice and antiviral medicine |
| CN115261142A (en) * | 2022-08-29 | 2022-11-01 | 西藏天虹科技股份有限责任公司 | Saffron extraction process and device |
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