CN101279945A - Extracting method of valerine - Google Patents
Extracting method of valerine Download PDFInfo
- Publication number
- CN101279945A CN101279945A CN 200810018679 CN200810018679A CN101279945A CN 101279945 A CN101279945 A CN 101279945A CN 200810018679 CN200810018679 CN 200810018679 CN 200810018679 A CN200810018679 A CN 200810018679A CN 101279945 A CN101279945 A CN 101279945A
- Authority
- CN
- China
- Prior art keywords
- valerianine
- chloroform
- alcohol
- valerian
- extracting method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a valerianine distillation method. After being ground, the valerianine is degreased through aether which is a solvent with low boiling point; after that the valerianine is marinated in t chloroform methanol mixture for distillation; the target product valerianine A is produced through dilute hydrochloric acid extraction process, together with silica gel and alumina column chromatographic separation process and recrystalization process. The purity of the valerianine A reaches 98%, satisfying requirements to medical materials. Valerianine is a natural quaternary ammonium alkaloid and has antidepressant function and sedative, hypnotic and anti-convulsion effects.
Description
Technical field
The present invention relates to a kind of extracting method of natural quartermary ammonium alkaloids, be the N-para hydroxybenzene ethyl derivative of actinidine, is valerian antidepressant function, calm, sleep peacefully, one of the main effective constituent of anticonvulsant action.
Background technology
Along with the quickening of social development, rhythm of life, the aggravation of competition, people's stress also increases gradually, and increasing people begins to pay close attention to can be alleviated stress, regulates the flow of vital energy and calm the nerves and the medicine of promote sleep.But the present commodity of selling with similar effect on the market mostly are to use the chemical process synthetic.Take the back and can produce apparent side effect and malaise symptoms, and produce drug dependence neural system.Therefore, a kind of safe and effective, stress of having no side effect, can help people to alleviate routine work and life to produce of market in urgent need, feel depressed, and medicine or heath food that can promote sleep.Develop this series products and have huge market outlook and scientific value.Valerian is widely used in industries such as medicine, food, makeup abroad, and existing multiple heath food is on sale.And domesticly still not having similar commodity of manufacturer production, the preparation made from valerian also still belongs to blank at home.
Valerian (Valerian), another name punching Lysimachia sikokiana, rhizoma nardostachyos are the wild per nnial herb of Valerianaceae valeriana (Valeriana L)) root and rhizome, originate in Europe, there is a small amount of distribution southwests such as China Hubei.The flat flavor of valerian property is hot, has tranquilizing and allaying excitement, separates contraction lenitive effect; Its rhizome is used among the people for a long time always as tranquilizer, as far back as the Ming Dynasty＜Compendium of Materia Medica〉in just on the books.According to incompletely statistics, the whole world has 81 kinds of valerians of 25 countries to obtain the different research of degree at present, wherein V.officiolis.L has been put into Germany, Britain, Norway, Holland, Japanese Pharmacopoeia, in the medicine catalogue of second edition Europe, also include multiple valerian preparation, Roten List income 57 kinds of valerian preparations (12 kinds on folk prescription, 45 kinds of compounds) in nineteen ninety Germany's medicine catalogue.Recently relevant its patent report is also increasing, and the pharmaceutical use of this platymiscium has obtained paying much attention to.Valerian mainly contains iridoid, sesquiterpene, alkaloid and flavones four major types chemical ingredients, and it is about 1% that wherein radix valerianae contains alkaloid, and the alkaloid main component is valerianine A, valerianine B, actinidine etc.Have document to show that valerianine A is an antidepressant function in the valerian, calm, sleep peacefully, one of the main active ingredient of pharmacological action such as anticonvulsion.
Summary of the invention
The extracting method that the purpose of this invention is to provide a kind of valerianine, extraction separation obtains a kind of antidepressant function that has from valerian, calm, the natural alkaloid of sleeping peacefully---valerianine A, purity reaches more than 98%, meets the requirement of medical material medicine.
Technical scheme of the present invention is as follows:
A kind of extracting method of valerianine, the valerianine structural formula of compound is as follows:
It is characterized in that may further comprise the steps:
(1), earlier valerian is pulverized, with the ether dipping, with degreasing, deoil;
(2), behind the mixed liquid dipping of valerian slag with chloroform and alcohol, soak solution reclaims alcohol and gets oily matter with chloroform, with alcohol, chloroform dilution oily matter, adds diethyl ether and separates out oily matter;
(3), add the dilute hydrochloric acid extraction in the oily matter, hcl as extraction agent liquid adds weak base and regulates pH to 8～10, adds the mixed solution extraction of chloroform and alcohol again, reclaims alcohol and gets the valerian biology total alkali with chloroform;
(4), the valerian biology total alkali adopt silicagel column separate the valerianine crude product; It is complete that TLC detects the valerianine wash-out that adsorbs on the silicagel column;
(5), the valerianine crude product separates with the aluminum oxide chromatographic column;
(6), the elutriant of aluminum oxide chromatographic column obtains valerianine through recrystallization.
The extracting method of described valerianine, when it is characterized in that ether dipping valerian, add-on should be 1～3ml/g of valerian weight, and dipping extracts 2～3 times, at least 5 days at every turn.
Described alcohol is meant methyl alcohol or ethanol, and described weak base is meant sodium bicarbonate.
In chloroform and the pure mixed solution, when pure nail was pure, the volume ratio ratio of chloroform and methyl alcohol was 1～3: 1; When alcohol referred to ethanol, chloroform and alcoholic acid volume ratio were 3～5: 2.
When separating with silicagel column, wherein eluent is that the ratio of chloroform methanol is 4～6: 1; Separate with alumina column, wherein eluent is that the ratio of chloroform methanol is 8～11: 1; The developping agent that TLC detects is an ethyl acetate: Virahol: ammoniacal liquor=45: 35: 20.
The solvent of recrystallization is water, methyl alcohol, acetone, ether or its mixed solvent.
The present invention extracts a kind of natural valerianine A in the valerian, wherein adopts lower boiling solvent ether degreasing, deoils; After extracting with the chloroform methanol mixed liquid dipping, adopt conventional separation means, binding silica gel, aluminum oxide column chromatography separation means, recrystallization obtains target product valerianine A, has the antidepressant function, calm, sleep peacefully, pharmacological action such as anticonvulsion.Purity reaches more than 98%, meets the requirement of medical material medicine.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention.
Embodiment
4Kg exsiccant valerian is added in the 5L ether, at room temperature soak 5d under the condition, behind the suction filtration, residue adds the 5L ether again, continues to soak 5d.The dregs of a decoction are volatilized, and 5L soaks three times (5d, 5d, 4d) with the chloroform methanol mixed solution.Vacuum-evaporation is reclaimed solvent and is obtained viscosity oily matter then, and this oily matter with the dilution of 120ml chloroform, adds the 1L ether after diluting with 80ml methyl alcohol more again, places in refrigerator and spends the night; Oily precipitation 100ml1% hcl as extraction agent, aqueous solution extraction oily matter precipitation is with 1% hydrochloric acid soln 20ml extraction three times.Merge mixed aqueous solution, be neutralized to pH8～10, chloroform alcohol mixed solution 75ml extraction 12 times, solvent evaporated with sodium bicarbonate.60g residuum silica gel chromatography wash-out, chromatographic silica gel 1kg, elutriant are the chloroform-methanol wash-out, and every collection 50ml is a fraction, collects compound and is the alkaloid-positive reaction, and developping agent is an ethyl acetate: propyl alcohol: ammoniacal liquor (45: 35: 20).After main alkaloid is eluted, wide at interval 4 of fixed position～5 points that have have been obtained.Merge main fraction, decompression and solvent recovery gets 12g medicinal extract, last neutral alumina (500g) chromatographic column, eluent is the chloroform methanol wash-out, collects the cut of front, reclaims solvent, add the ether crystallization, with methyl alcohol, acetone, ether recrystallization, three crystallizations obtain 2.1g crystal (muriate).Mp201～203 ℃ (decomposition).The fusing point of picrate is 151～152 ℃, and is easily molten in water and ethanol, indissoluble in most of organic solvents.
Claims (6)
1, a kind of extracting method of valerianine, the valerianine structural formula of compound is as follows:
It is characterized in that may further comprise the steps:
(1), earlier valerian is pulverized, with the ether dipping, with degreasing, deoil;
(2), behind the mixed liquid dipping of valerian slag with chloroform and alcohol, soak solution reclaims alcohol and gets oily matter with chloroform, with alcohol, chloroform dilution oily matter, adds diethyl ether and separates out oily matter;
(3), add the dilute hydrochloric acid extraction in the oily matter, hcl as extraction agent liquid adds weak base and regulates pH to 8～10, adds the mixed solution extraction of chloroform and alcohol again, reclaims alcohol and gets the valerian biology total alkali with chloroform;
(4), the valerian biology total alkali adopt silicagel column separate the valerianine crude product; It is complete that TLC detects the valerianine wash-out that adsorbs on the silicagel column;
(5), the valerianine crude product separates with the aluminum oxide chromatographic column;
(6), the elutriant of aluminum oxide chromatographic column obtains valerianine through recrystallization.
2, the extracting method of valerianine according to claim 1, when it is characterized in that ether dipping valerian, add-on should be 1～3ml/g of valerian weight, and dipping extracts 2～3 times, at least 5 days at every turn.
3, the extracting method of valerianine according to claim 1 is characterized in that described alcohol is meant methyl alcohol or ethanol, and described weak base is meant sodium bicarbonate.
4, the extracting method of valerianine according to claim 1 is characterized in that in chloroform and the pure mixed solution, and when pure nail was pure, the volume ratio ratio of chloroform and methyl alcohol was 1～3: 1; When alcohol referred to ethanol, chloroform and alcoholic acid volume ratio were 3～5: 2.
5, the extracting method of valerianine according to claim 1, when it is characterized in that separating with silicagel column, wherein eluent is that the ratio of chloroform methanol is 4～6: 1; Separate with alumina column, wherein eluent is that the ratio of chloroform methanol is 8～11: 1; The developping agent that TLC detects is an ethyl acetate: Virahol: ammoniacal liquor=45: 35: 20.
6, the extracting method of valerianine according to claim 1, the solvent that it is characterized in that recrystallization are water, methyl alcohol, acetone, ether or its mixed solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810018679 CN101279945B (en) | 2008-03-10 | 2008-03-10 | Extracting method of valerine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810018679 CN101279945B (en) | 2008-03-10 | 2008-03-10 | Extracting method of valerine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101279945A true CN101279945A (en) | 2008-10-08 |
| CN101279945B CN101279945B (en) | 2011-10-26 |
Family
ID=40012638
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200810018679 Expired - Fee Related CN101279945B (en) | 2008-03-10 | 2008-03-10 | Extracting method of valerine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101279945B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112402519A (en) * | 2020-12-14 | 2021-02-26 | 武汉惠尔生物科技有限公司 | Valerian total alkaloid extract and preparation method thereof |
-
2008
- 2008-03-10 CN CN 200810018679 patent/CN101279945B/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112402519A (en) * | 2020-12-14 | 2021-02-26 | 武汉惠尔生物科技有限公司 | Valerian total alkaloid extract and preparation method thereof |
| CN112402519B (en) * | 2020-12-14 | 2022-06-07 | 武汉惠尔生物科技有限公司 | Valerian total alkaloid extract and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101279945B (en) | 2011-10-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109568389A (en) | A kind of preparation method of high-purity cannabinoids extract | |
| CN101735030B (en) | Method for preparing 6-shogaol | |
| AU649111B2 (en) | Method for the extraction of sesquiterpene lactones | |
| CN107118219B (en) | The method of separating-purifying gelsevirine, koumidine, koumine, gelsemine and furans koumine from elegant jessamine | |
| CN101624393B (en) | Method for extracting cytosine and thermopsine from thermopsis lanceolata seeds | |
| CN103739586A (en) | Method for extracting diterpenoid compounds from Blumea aromatic DC. | |
| CN101157717B (en) | Preparation method of Ardisia mamillata B and uses thereof | |
| CN102150851A (en) | Sea cucumber saponin, preparation method thereof and application thereof in food or medicine | |
| Kalinina et al. | Diuretic activity and toxicity of some Verbascum nigrum extracts and fractions | |
| CN101279945B (en) | Extracting method of valerine | |
| CN101480419B (en) | Polysaccharide extract of Periploca forrestii Schltr, and preparation method thereof | |
| CN100435810C (en) | Dogwood fruit extract and its preparation process | |
| CN104434930B (en) | Composition comprising 24 acetylalisol A and 23 acetylalisol B and its in Adjust-blood lipid, the application prepared on HMG CoA inhibitor | |
| CN102302615A (en) | Effective site group of daphne giraldii nitsche leaf, preparation method, medicinal composition and application thereof | |
| CN109280090A (en) | One kind having the active aspongopus class Pentatomidae Insects extraction method of polysaccharides of warming kidney and enhancing body and application | |
| CN101732322B (en) | Application of corosolic acid in preparation of antidepressant drug | |
| CN107595906A (en) | The application of hederagenin and its glucosides in antiviral drug is prepared | |
| CN103340917A (en) | Extraction method for flavonoids in mugwort | |
| CN101543523B (en) | Uyghur drug compound recipe extracting technology for chiccory | |
| CN110251543A (en) | Become application of the leaf tree conopsea extraction in preparation antidepression natural drug | |
| CN100528170C (en) | Mangiferin preparation and production thereof | |
| CN101991592A (en) | Application of paederoside to preparation of analgesic and/or anti-inflammatory medicaments | |
| CN101195645B (en) | Anti-hepatitis B virus streblus extract and extracting technique thereof | |
| CN101129365B (en) | Analgesics use of ricinine | |
| CN101596205B (en) | Antiphlogistic medicinal composition and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111026 Termination date: 20130310 |