CN102875559A - Method for extracting simulenoline from zanthoxylum simulans hance - Google Patents
Method for extracting simulenoline from zanthoxylum simulans hance Download PDFInfo
- Publication number
- CN102875559A CN102875559A CN201210359999XA CN201210359999A CN102875559A CN 102875559 A CN102875559 A CN 102875559A CN 201210359999X A CN201210359999X A CN 201210359999XA CN 201210359999 A CN201210359999 A CN 201210359999A CN 102875559 A CN102875559 A CN 102875559A
- Authority
- CN
- China
- Prior art keywords
- zanthoxylum simulans
- extracting
- chloroform
- zanthoxylum
- simulans
- 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.)
- Pending
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a method for extracting simulenoline from zanthoxylum simulans hance. The method comprises the following steps of: crushing zanthoxylum simulans hance barks to form 40 to 60-mesh powder, adding the powder into 80 to 95 volume percent of ethanol aqueous solution in an amount which is 5 to 8 times that of the powder, performing reflux and extracting for 2 to 3 times, and recovering ethanol from an extracting solution under reduced pressure; adding an extract into a hydrochloric acid aqueous solution for dissolving, filtering, adding a silica-gel desiccant for drying, and performing ultrasonic extraction by using petroleum ether and chloroform sequentially; recovering the chloroform from a chloroform extracting solution, adding silica gel, mixing uniformly, drying, and packing the mixture; and eluting a mixed solution of the chloroform and methanol, performing thin-layer detection, collecting high-concentration fractions, recovering a reagent, and drying to obtain a pure simulenoline product. The method for producing the simulenoline is high in stability and specificity, and the pollution to environment is reduced.
Description
Technical field
The invention belongs to the crude drug field, particularly relate to a kind of method of from Zanthoxylum simulans, extracting Zanthoxylum simulans alcohol alkali.
Background technology
Zanthoxylum simulans alcohol alkali (Simulenoline) is to separate a kind of quinoline alkaloid that obtains, molecular formula C from Zanthoxylum simulans
20H
23NO
3, molecular weight 325.41 is colorless oil.Pharmacological research shows that Zanthoxylum simulans alcohol alkali has platelet aggregation inhibitory activity, and the rabbit platelet aggregation that arachidonic acid, collagen and PAF are induced is restraining effect, when 100 μ g/mL, suppresses collagen-induced platelet aggregation fully.
Zanthoxylum simulans
Zanthoxylum simulansHance is Rutaceae (Rutaceae) Zanthoxylum (Zanthoxylum Linn) plant, has another name called seed of Zanthoxylum armatum DC.(Z.Planispinum Sieb.et Zucc.), rock green pepper, Zanthoxylum planispinum, mainly be distributed on the south the Changjiang river and the ground such as Henan, Hebei, but its leaf, really, equal hyoscine such as root.This platymiscium resource is than horn of plenty, and the whole world has 250 kinds approximately, is distributed in the subtropical and tropical zones of Asia, Africa, Oceania, North America, and China has 45 kinds approximately, 13 mutation.Modern study shows, the fruit of xanthoxylum, root, stem, Ye Junke are used as medicine, mainly contain the chemical ingredientss such as alkaloid, acid amides, lignanoid, tonka bean camphor, volatile oil and lipid acid, obvious blood coagulation, calmness, analgesia, anti-inflammatory, antibacterial desinsection, the pharmacologically active such as antitumor are arranged.The research of this platymiscium had many reports both at home and abroad, but very few about the report of Zanthoxylum simulans stem skin chemical ingredients.Zhu Dan adopts 95% ethanol cold soaking 4 times in the master thesis of delivering " research of Zanthoxylum simulans chemical ingredients ", each 2d, the gained ethanol extraction is dissolved in methyl alcohol, then use successively sherwood oil, ethyl acetate, n-butanol extraction, carry out again silica gel column chromatography, separation to chemical ingredientss such as alkaloids, lignanoid, tonka bean camphor, terpene.
Summary of the invention
The technical problem that present method will solve provides a kind of method of extracting Zanthoxylum simulans alcohol alkali from Zanthoxylum simulans, and the method industrialization degree is high, can prepare high-content Zanthoxylum simulans alcohol alkali.
In order to realize above-mentioned purpose of the present invention, the invention provides following technical scheme:
A kind of method of from Zanthoxylum simulans, extracting Zanthoxylum simulans alcohol alkali, it is characterized in that may further comprise the steps: get Zanthoxylum simulans stem skin and pulverize the 40-60 order, add 5-8 and doubly measure aqueous ethanolic solution refluxing extraction 2-3 time that concentration of volume percent is 80-95%, the extracting solution decompression recycling ethanol, medicinal extract adds the aqueous hydrochloric acid dissolving, filter, after adding the silica-gel drier drying, use successively again sherwood oil, the chloroform supersound extraction, chloroform extracted solution reclaims chloroform, add the silica gel mixing and mix oven dry thoroughly, the dress post, chloroform methanol mixing solutions wash-out, thin layer detects, collect the high density flow point and reclaim reagent, be drying to obtain Zanthoxylum simulans alcohol alkali sterling.
Described aqueous hydrochloric acid mass percent concentration is 1-3%, and consumption is 3-5 times of medicinal extract amount.
The 1-3 that described silica-gel drier consumption is amount of solution doubly.
Described chloroform methanol miscible fluid volume ratio is 20:1-1:1.
The present invention adopts alcohol reflux, and solvent load is less than sour water percolation ration, and solvent can recycle and reuse, and is beneficial to environmental protection.
The present invention adopts chloroform methanol mixing solutions gradient, and is simple to operate, easily reappears and amplifies production, and reagent easily reclaims and reuses.
Embodiment:
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment 1:
Get Zanthoxylum simulans pulverizing medicinal materials 40-60 order, take by weighing 10kg, added the 50L95% alcohol reflux 1 hour, filter extracting solution, added the 30L95% alcohol reflux 1 hour again, and leached and add 30L refluxing extraction hour behind the extracting solution again, united extraction liquid Recycled ethanol is to medicinal extract, add the dissolving of 8L1% aqueous hydrochloric acid, filter, add 2kg silica-gel drier drying after, add 5L sherwood oil supersound extraction 1 hour, leach sherwood oil, add 4L chloroform supersound extraction 1 hour, chloroform extracted solution reclaims chloroform, adds silica gel 1kg(120-200 again) the order oven dry, with 3kg silica gel dress post, the chloroform methanol mixing solutions is 20:1 by volume, 10:1,5:1,3:1,1:1 carries out gradient elution, and thin layer detects, and collects the high density flow point and reclaims reagent, dry Zanthoxylum simulans alcohol alkali sterling, the content 95.8% of getting.
Embodiment 2:
Get Zanthoxylum simulans pulverizing medicinal materials 40-60 order, take by weighing 10kg, added the 60L90% alcohol reflux 1.5 hours, filter extracting solution, added again the 5L99% alcohol reflux 1 hour, united extraction liquid Recycled ethanol adds the dissolving of 5L3% aqueous hydrochloric acid to medicinal extract, filters, after adding 3kg silica-gel drier drying, add 6L sherwood oil supersound extraction 1 hour, leach sherwood oil, add again 5L chloroform supersound extraction 1 hour, chloroform extracted solution reclaims chloroform, add silica gel 800g(120-200) the order oven dry, and 2.5kg silica gel dress post, the chloroform methanol mixing solutions is 20:1 by volume, 10:1,5:1,3:1,1:1 carries out gradient elution, thin layer detects, collect the high density flow point and reclaim reagent, dry Zanthoxylum simulans alcohol alkali sterling, the content 93.5% of getting.
Embodiment 3:
Get Zanthoxylum simulans pulverizing medicinal materials 40-60 order, take by weighing 20kg, added the 160L80% alcohol reflux 2 hours, filter extracting solution, added again the 30L90% alcohol reflux 1.5 hours, united extraction liquid Recycled ethanol adds the dissolving of 10L2% aqueous hydrochloric acid to medicinal extract, filters, after adding 8kg silica-gel drier drying, add 8L sherwood oil supersound extraction 1 hour, leach sherwood oil, add again 6L chloroform supersound extraction 1 hour, chloroform extracted solution reclaims chloroform, add silica gel 1.2kg(120-200) the order oven dry, and 5kg silica gel dress post, the chloroform methanol mixing solutions is 20:1 by volume, 10:1,5:1,3:1,1:1 carries out gradient elution, thin layer detects, collect the high density flow point and reclaim reagent, dry Zanthoxylum simulans alcohol alkali sterling, the content 92.7% of getting.
Claims (4)
1. method of from Zanthoxylum simulans, extracting Zanthoxylum simulans alcohol alkali, it is characterized in that may further comprise the steps: get Zanthoxylum simulans stem skin and pulverize the 40-60 order, add 5-8 and doubly measure aqueous ethanolic solution refluxing extraction 2-3 time that concentration of volume percent is 80-95%, the extracting solution decompression recycling ethanol, medicinal extract adds the aqueous hydrochloric acid dissolving, filter, after adding the silica-gel drier drying, use successively again sherwood oil, the chloroform supersound extraction, chloroform extracted solution reclaims chloroform, add the silica gel mixing and mix oven dry thoroughly, the dress post, chloroform methanol mixing solutions gradient elution, thin layer detects, collect the high density flow point and reclaim reagent, be drying to obtain Zanthoxylum simulans alcohol alkali sterling.
2. the described method of extracting Zanthoxylum simulans alcohol alkali from Zanthoxylum simulans according to claim 1 is characterized in that the described aqueous hydrochloric acid mass percent concentration of step is 1-3%, consumption be the medicinal extract amount 3-5 doubly.
3. the described method of extracting Zanthoxylum simulans alcohol alkali from Zanthoxylum simulans according to claim 1 is characterized in that 1-3 that the described silica-gel drier consumption of step is amount of solution doubly.
4. the described method of extracting Zanthoxylum simulans alcohol alkali from Zanthoxylum simulans according to claim 1 is characterized in that the described chloroform methanol miscible fluid of step volume ratio is 20:1-1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210359999XA CN102875559A (en) | 2012-09-25 | 2012-09-25 | Method for extracting simulenoline from zanthoxylum simulans hance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210359999XA CN102875559A (en) | 2012-09-25 | 2012-09-25 | Method for extracting simulenoline from zanthoxylum simulans hance |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102875559A true CN102875559A (en) | 2013-01-16 |
Family
ID=47477112
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210359999XA Pending CN102875559A (en) | 2012-09-25 | 2012-09-25 | Method for extracting simulenoline from zanthoxylum simulans hance |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102875559A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105638779A (en) * | 2016-02-03 | 2016-06-08 | 陈翔 | Gardening herbicide |
| CN107625834A (en) * | 2017-09-21 | 2018-01-26 | 重庆第二师范学院 | The high efficiency extraction separation method and system of a kind of available things of Zanthoxylum bungeanum |
| CN111905018A (en) * | 2020-09-21 | 2020-11-10 | 中国科学院西双版纳热带植物园 | Preparation method and application of zanthoxylum bungeanum maxim extract |
-
2012
- 2012-09-25 CN CN201210359999XA patent/CN102875559A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105638779A (en) * | 2016-02-03 | 2016-06-08 | 陈翔 | Gardening herbicide |
| CN107625834A (en) * | 2017-09-21 | 2018-01-26 | 重庆第二师范学院 | The high efficiency extraction separation method and system of a kind of available things of Zanthoxylum bungeanum |
| CN111905018A (en) * | 2020-09-21 | 2020-11-10 | 中国科学院西双版纳热带植物园 | Preparation method and application of zanthoxylum bungeanum maxim extract |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR102185474B1 (en) | Extracts effective in treating drug addiction and preparation method thereof | |
| CN102875559A (en) | Method for extracting simulenoline from zanthoxylum simulans hance | |
| CN103130752B (en) | A kind of method producing root of Beijing euphorbia factor L1 from Euphorbia lathyris fruit fast | |
| CN105503807A (en) | Catechin derivative named as epicatechin trans caffeic acid ester and preparation method and application thereof | |
| CN103446195A (en) | Preparation method of ginkgo biloba extract | |
| KR102570122B1 (en) | Novel compounds and their preparation methods and applications | |
| CN106831909A (en) | The extracting method of double benzene pyrrones compounds in wind-weed fibrous root | |
| CN101091734A (en) | Method for preparing extractive of pubescent angelica root coumarin | |
| CN100526327C (en) | Process for producing ursolic acid | |
| CN101301370B (en) | Method for preparing monoester type alkaloids using Chinese medicinal material of aconitum as raw material | |
| CN103524578B (en) | A kind of method of extraction and isolation paeoniflorin compound from tree peony stamen | |
| CN102040642A (en) | Process for extracting pristimerin | |
| CN104592322A (en) | Method for extracting and separating curculigoside from curculigo gaertn plants | |
| CN102351825B (en) | Method for extracting and separating ginkgetin | |
| CN103961427B (en) | A kind of bush cinqefoil extract treating type 2 diabetes mellitus and preparation method thereof | |
| CN104804011A (en) | Method for separating and purifying isoimperatorin and imperatorin from angelica dahurica | |
| CN103058979A (en) | Method for extracting procyanidine in ginkgo leaves | |
| CN102649808A (en) | Method for separating ursolic acid from plantain herb | |
| CN103588745B (en) | A kind of method of Extraction and separation not this Kelin from Coleus forskohlii Briq. | |
| CN102836280A (en) | Folium Lycii total flavone extract and preparation method thereof | |
| CN101974054A (en) | Improved method for extracting hemsleyadin | |
| CN105348338A (en) | Method for extracting and separating paederosidic acid from Saprosma merrillii Lo | |
| CN101497846A (en) | Method for extracting Calophyllum essential oil constituent | |
| CN102241682A (en) | Preparation method for fissistigine A | |
| CN105267357B (en) | The purposes of Herba Hedyotis Lanceae or its extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130116 |