CN102516260A - Method for preparing picrinine - Google Patents
Method for preparing picrinine Download PDFInfo
- Publication number
- CN102516260A CN102516260A CN2011104280050A CN201110428005A CN102516260A CN 102516260 A CN102516260 A CN 102516260A CN 2011104280050 A CN2011104280050 A CN 2011104280050A CN 201110428005 A CN201110428005 A CN 201110428005A CN 102516260 A CN102516260 A CN 102516260A
- Authority
- CN
- China
- Prior art keywords
- picrinine
- membrane
- liquid
- preparing
- macroporous resin
- 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
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a method for preparing picrinine. The method comprises the following steps: crushing alstonia leaves; carrying out extraction on the alstonia leaves through percolation with acid water; carrying out ultrafiltration with an ultrafiltration membrane after filtration of an obtained extract; condensing obtained permeate with a nanofiltration membrane; allowing concentrate to pass through a macroporous resin column; carrying out elution with a proper amount of water; collecting eluted liquid and eluting water and adjusting the pH value of obtained mixed liquid to 8 to 10; standing the mixed liquid for deposition; centrifuging the mixed liquid; dissolving an obtained precipitation through reflux dissolving with methanol; decolouring the precipitation with active carbon; adding a proper amount of petroleum ether into decolouring liquid; refrigerating an obtained mixture for crystallization; and carrying out recrystallization on an obtained crystal by using an ethanol solution so as to obtain picrinine. The method has the advantages of simple operation, low energy consumption, a short period and suitability for industrialization.
Description
Technical field
The present invention relates to a kind of method for preparing picrinine, particularly relate to a kind of method that adopts membrane separation technique and macroporous resin to prepare picrinine.
Background technology
Picrinine (Picrinine) is an indoles monoterpenes vegeto-alkali, molecular formula C20H22N2O3, and molecular weight 338, molecular structural formula:
Picrinine has antibechic, relieving asthma, eliminate the phlegm and to effects such as anti-acetylcholine, I4EAs.
Cornus controversa is an Apocynaceae Alstonia plant Cornus controversa
Alstonia scholaris(L.) R. Brown; Be used as medicine with leaf or spray; Cry again dita, big porker leaf, greatly set Herba Hedyotis scandentis, buy load not (Dai Nationality's language), have anti-inflammatory, preventing phlegm from forming and stopping coughing, lenitive effect, be used to treat bronchitis, Whooping cough, stomachache, diarrhoea, malaria and external application and control wound etc.And picrinine is the main pharmaceutical compound of lamp stand leaf.
From the lamp stand leaf, extract the method for picrinine, generally adopt acid extraction or organic reagent to extract, concentrate the back chloroform extraction, extraction liquid separates with the solid packed column again.(application number: 201010571990.6) (application number: 200810219419.0) " a kind of method of extracting picrinine and ursolic acid from the dita leaf simultaneously " all is to adopt this kind method for " picrinine reference substance and preparation method thereof in the Folium Alstoniae Scholaris " and patent like patent.These methods exist industry " three wastes " and produce manyly, and environmental pollution is serious, and consumption of organic solvent is big, and production cost is higher, and technological operation is loaded down with trivial details.
Membrane sepn is the relevant screening process of a kind of and membrane pore size size; Pressure difference with the film both sides is a motivating force, is filtration medium with the film, under certain pressure; The many tiny micropore that gathers in the film surface only allows water and small-molecule substance through becoming through liquid; Volume then is trapped within the liquid feeding side of film greater than the material in film surface micro aperture in the stoste, becomes liquid concentrator, thereby realizes separation and spissated purpose to stoste.In sepn process, can be divided into micro-filtration, ultrafiltration, nanofiltration and r-o-according to holding back molecular weight of material size.Because membrane filtration is a kind of physical separation method, energy consumption is low, pollution is little, processing speed is fast, is used widely in fields such as biology, pharmacy, WWTs.
Summary of the invention
The objective of the invention is to overcome the defective and the deficiency of prior art, a kind of method for preparing picrinine is provided, method is simple, is fit to suitability for industrialized production.
The objective of the invention is to realize through following technical scheme: get the lamp stand leaf and pulverize, add the sour water diacolation and extract, extracting solution filters uses the ultra-filtration membrane ultrafiltration, sees through liquid and concentrates with nf membrane; Liquid concentrator is through macroporous resin column, and the suitable quantity of water wash-out is collected lower column liquid and water lotion and regulated ph8-10 with ammoniacal liquor, places deposition; Centrifugal, throw out refluxes with dissolve with methanol and dissolves, and adds activated carbon decolorizing, and destainer adds an amount of sherwood oil; The refrigeration crystallization, crystallisate is used the ethanolic soln recrystallization again, promptly gets.
The used sour water of production process can be selected 1% aqueous sulfuric acid.
Described ultra-filtration membrane is the hollow cellulose ultra-filtration membrane of molecular weight cut-off 2000-6000.
The hollow cellulose nf membrane of the optional molecular weight cut-off 100-300 of described nf membrane.
Optional polar macroporous resin of described macroporous resin or non-polar macroporous resin, the optional AB-8 of model, ADS-21 or NK-9.
Advantage of the present invention is: method adopts diacolation extraction, membrane sepn, is to carry out at normal temperatures, and energy consumption is low; Membrane sepn and macroporous resin removal of impurities, simple to operate, the spissated sour water of nanofiltration can recycle, and environment is not polluted, and is fit to suitability for industrialized production.
Embodiment
To combine embodiment to further specify the present invention below.
Embodiment 1:
The lamp stand leaf is ground into particle, gets 10kg, extracts with 15 times of amount 1% aqueous sulfuric acid diacolations; Extracting solution filters the hollow cellulose ultra-filtration membrane ultrafiltration that adds molecular weight cut-off 2000, and the hollow cellulose nf membrane that adds molecular weight cut-off 300 through liquid again concentrates, and liquid concentrator is crossed the AB-8 macroporous resin column; The suitable quantity of water wash-out is collected lower column liquid and water lotion and is regulated ph9 with ammoniacal liquor, places deposition; Centrifugal, throw out to be with the dissolving that refluxes of 90% dissolve with methanol, adds 1% activated carbon decolorizing of solution amount; Destainer leaches gac, adds the sherwood oil of 1/10 volume, fully stirs the refrigeration crystallization; Crystallisate is used 70% ethanolic soln recrystallization again, dry white crystal 15g, the content detection 90.5% of getting.
Embodiment 2:
The lamp stand leaf is ground into particle, gets 20kg, extracts with 20 times of amount 1% aqueous sulfuric acid diacolations; Extracting solution filters the hollow cellulose ultra-filtration membrane ultrafiltration that adds molecular weight cut-off 6000, and the hollow cellulose nf membrane that adds molecular weight cut-off 200 through liquid again concentrates, and liquid concentrator is crossed the ADS-21 macroporous resin column; The suitable quantity of water wash-out is collected lower column liquid and water lotion and is regulated ph10 with ammoniacal liquor, places deposition; Centrifugal, throw out to be with the dissolving that refluxes of 99% dissolve with methanol, adds 0.5% activated carbon decolorizing of solution amount; Destainer leaches gac, adds the sherwood oil of 1/12 volume, fully stirs the refrigeration crystallization; Crystallisate is used 85% ethanolic soln recrystallization again, dry white crystal 22g, the content detection 92.3% of getting.
Embodiment 3:
The lamp stand leaf is ground into particle, gets 50kg, extracts with 20 times of amount 1% aqueous sulfuric acid diacolations; Extracting solution filters the hollow cellulose ultra-filtration membrane ultrafiltration that adds molecular weight cut-off 2000, and the hollow cellulose nf membrane that adds molecular weight cut-off 300 through liquid again concentrates, and liquid concentrator is crossed the NK-9 macroporous resin column; The suitable quantity of water wash-out is collected lower column liquid and water lotion and is regulated ph8 with ammoniacal liquor, places deposition; Centrifugal, throw out to be with the dissolving that refluxes of 95% dissolve with methanol, adds 0.5% activated carbon decolorizing of solution amount; Destainer leaches gac, adds the sherwood oil of 1/8 volume, fully stirs the refrigeration crystallization; Crystallisate is used 95% ethanolic soln recrystallization again, dry white crystal 81g, the content detection 91.7% of getting.
Claims (4)
1. method for preparing picrinine is characterized in that: get the lamp stand leaf and pulverize, add the sour water diacolation and extract, extracting solution filters uses the ultra-filtration membrane ultrafiltration; See through liquid and concentrate with nf membrane, liquid concentrator is through macroporous resin column, and the suitable quantity of water wash-out is collected lower column liquid and water lotion and regulated ph8-10 with ammoniacal liquor; Place deposition, centrifugal, throw out refluxes with dissolve with methanol and dissolves, and adds activated carbon decolorizing; Destainer adds an amount of sherwood oil, the refrigeration crystallization, and crystallisate is used the ethanolic soln recrystallization again, promptly gets.
2. according to the said method for preparing picrinine of claim 1, it is characterized in that described ultra-filtration membrane is the hollow cellulose ultra-filtration membrane of molecular weight cut-off 2000-6000.
3. the method for preparing picrinine according to claim 1 is characterized in that the hollow cellulose nf membrane of the optional molecular weight cut-off 100-300 of described nf membrane.
4. the method for preparing picrinine according to claim 1 is characterized in that optional polar macroporous resin of described macroporous resin or non-polar macroporous resin, the optional AB-8 of model, ADS-21 or NK-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104280050A CN102516260A (en) | 2011-12-20 | 2011-12-20 | Method for preparing picrinine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104280050A CN102516260A (en) | 2011-12-20 | 2011-12-20 | Method for preparing picrinine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102516260A true CN102516260A (en) | 2012-06-27 |
Family
ID=46287378
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104280050A Pending CN102516260A (en) | 2011-12-20 | 2011-12-20 | Method for preparing picrinine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102516260A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103230464A (en) * | 2013-05-06 | 2013-08-07 | 西双版纳傣族自治州民族医药研究所 | Dai medical mixture for treating cough |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5290553A (en) * | 1991-07-22 | 1994-03-01 | The United States Of America As Represented By The Secretary Of The Army | Alkaloids of picralima nitida used for treatment of protozoal diseases |
| CN1818636A (en) * | 2006-03-16 | 2006-08-16 | 朱光荣 | Use of picrinine in quality control of Dengtaiye medicine and its preparation |
| CN101084894A (en) * | 2006-06-07 | 2007-12-12 | 中国科学院昆明植物研究所 | Medicine for treating diseases concerned with respiratory and use thereof |
| CN102040613A (en) * | 2010-12-03 | 2011-05-04 | 昆明振华制药厂有限公司 | Picrinine reference substance in common alstonia leaf and preparation method thereof |
-
2011
- 2011-12-20 CN CN2011104280050A patent/CN102516260A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5290553A (en) * | 1991-07-22 | 1994-03-01 | The United States Of America As Represented By The Secretary Of The Army | Alkaloids of picralima nitida used for treatment of protozoal diseases |
| CN1818636A (en) * | 2006-03-16 | 2006-08-16 | 朱光荣 | Use of picrinine in quality control of Dengtaiye medicine and its preparation |
| CN101084894A (en) * | 2006-06-07 | 2007-12-12 | 中国科学院昆明植物研究所 | Medicine for treating diseases concerned with respiratory and use thereof |
| CN102040613A (en) * | 2010-12-03 | 2011-05-04 | 昆明振华制药厂有限公司 | Picrinine reference substance in common alstonia leaf and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| TOH-SEOK KAM,等: "New Indole Alkaloids from Alstonia macrophylla", 《JOURNAL OF NATURAL PRODUCTS》 * |
| 孙赟，等: "灯台叶中鸭脚树叶碱化学对照品的制备", 《云南中医学院学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103230464A (en) * | 2013-05-06 | 2013-08-07 | 西双版纳傣族自治州民族医药研究所 | Dai medical mixture for treating cough |
| CN103230464B (en) * | 2013-05-06 | 2014-11-05 | 西双版纳傣族自治州民族医药研究所 | Dai medical mixture for treating cough |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102106931A (en) | Method for producing diverse extracts of berry tea | |
| CN101904877B (en) | New preparation method of low-phenolic acid gingko flavone extractive | |
| CN102241659A (en) | Purification method of alpha-mangostin | |
| CN105294628A (en) | Method for preparing flavonoid component by separating wild chrysanthemum flower | |
| CN101974049A (en) | Method for extracting aucubin from aucuba japonica leaves | |
| CN103450136A (en) | Method for extracting hinokiflavone from Cacumen Biotae | |
| CN102190693B (en) | Method for preparing hyperin from Dogbane leaves | |
| CN103830306A (en) | Preparation method of honey suckle leaf effective extract product | |
| CN102626448A (en) | Method for extracting total alkaloids from thalictrum plants | |
| CN102526357A (en) | Method for extracting total flavone and esculetin from Chinese violet | |
| CN103251790A (en) | Method for extracting total alkaloids from fritillaria pallidiflora | |
| CN101554394A (en) | Process for extracting total flavonoid from canola plant bee pollen | |
| CN102516260A (en) | Method for preparing picrinine | |
| CN103183658A (en) | Method for extracting effective component of coleus forskohlii | |
| CN102309576A (en) | Preparation method of uncaria total alkaloids | |
| CN101962385A (en) | Method for preparing bergeninum | |
| CN102600215A (en) | Method for extracting peganum harmala alkaloid | |
| CN104231011A (en) | Preparation method of verbascoside | |
| CN103232504A (en) | Method for preparing cyanidenon-7-O-beta-D-glucuronide | |
| CN103193750B (en) | Method for preparing shikimic acid and anise flavonoid by joint separation of macroporous resin XAD7HP | |
| CN102391344A (en) | Method for preparing picfeltarraenin IA from picria feltarrae lour leaves | |
| CN101805345A (en) | Method for purifying protopine from corydalis amabilis | |
| CN105311248A (en) | Tea fruit shell tannin and preparation method thereof | |
| CN104974202A (en) | Method for extracting and separating vitexin xyloside from natural product | |
| CN103242399A (en) | Method for extracting apigenin-7-O-beta-D-glucuronide from broussonetia papyrifera leaves |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120627 |