CN1537573A - Extraction of active ingredient of Zuanshanfeng, and method for preparing its prepn. - Google Patents
Extraction of active ingredient of Zuanshanfeng, and method for preparing its prepn. Download PDFInfo
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- CN1537573A CN1537573A CNA03118278XA CN03118278A CN1537573A CN 1537573 A CN1537573 A CN 1537573A CN A03118278X A CNA03118278X A CN A03118278XA CN 03118278 A CN03118278 A CN 03118278A CN 1537573 A CN1537573 A CN 1537573A
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- radix fissistigmatis
- fissistigmatis oldhamii
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- oldhamii
- extract
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Abstract
A process for extracting the active component from szechwan sabia root and stem and then using it to prepare the Chinese medicines for treating ischialgia, rheumatic arthritis, bone fracture and injury includes such steps as extracting in alcohol or acidic water, alkali depositing to obtain its general extract, processing the extracting liquid by chromatographe, eluting and drying to obtain its general alkali, and using said general extract and general alkali to prepare Chinese medicines. Its advantages are high curative effect and low dosage.
Description
Technical field
This invention relates to the Chinese medicine technology field, relates in particular to the Radix Fissistigmatis Oldhamii extraction process of effective component.
Background technology
Radix Fissistigmatis Oldhamii is the annonaceae plant, have another name called Radix Fissistigmatis Oldhamii, has wind-expelling pain-stopping, the effect of promoting blood circulation to remove obstruction in the collateral, be used for diseases such as sciatica, rheumatic arthritis, traumatic injury, its main effective ingredient is an alkaloids, the preparation Radix Fissistigmatis Oldhamii syrup of Radix Fissistigmatis Oldhamii is for being the compound preparation of principal agent with the Radix Fissistigmatis Oldhamii, listed in the 10th of the Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation ", the existing extraction process of Radix Fissistigmatis Oldhamii is a boiled process, it is not refining to have preparation, the deficiency that dose is big.Based on this, we extract the Radix Fissistigmatis Oldhamii effective ingredient, refining, make the Radix Fissistigmatis Oldhamii total extract, the Radix Fissistigmatis Oldhamii total alkali, and further be processed into folk prescription or the various dosage forms of compound recipe as raw material, it is refining to have preparation, consumption is little, and eutherapeutic advantage can better satisfy and ensure people's medication demand.
Summary of the invention
The preparation of Radix Fissistigmatis Oldhamii total extract
Technology one is got Radix Fissistigmatis Oldhamii and is ground into coarse powder, and with the ethanol extraction of 60-95%, extracting solution filters, and filtrate recycling ethanol continues purification or transfers pH2-3, filters, and filtrate is transferred pH9-10, filters, and collecting precipitation is for the preparation preparation.
Technology two is got Radix Fissistigmatis Oldhamii and is ground into coarse powder, is solvent with the acid of 0.2-10%, and percolation to alkaloid extracts fully, and percolate continues purification, or adjust pH 9-10, filters, and collecting precipitation is for the preparation preparation.
The alcohol extraction condition of Radix Fissistigmatis Oldhamii is in the technology one: the ethanol with 60-95% is solvent, adopt heating reflux method or percolation to extract, the best is a solvent for the ethanol with 80%, heating and refluxing extraction 3 times, the solubilizer flow control once is 10 times of amounts, second and third time is 8 times of amounts, first and second time 2 hours, 1 hour for the third time.
The percolation condition is for being solvent with acid such as the acetic acid of 0.2-10%, sulphuric acid, hydrochloric acid in the technology two, and the best be complete to the alkaloid extraction with the hydrochloric acid percolation of 1-2%.
Whether fully available alkaloid extraction alkaloid precipitation reagent detect in the technology.
Filter in the technology and also can adopt centrifugation method
The preparation of Radix Fissistigmatis Oldhamii total alkali
Technology one above-mentioned Radix Fissistigmatis Oldhamii alcohol extract reclaims ethanol, transfers pH to 2-3 with hydrochloric acid, filters, last acidity is positive in exchange resin column, or acid cation exchange resin on the above-mentioned Radix Fissistigmatis Oldhamii acid percolate, after exchange back resin water, ethanol wash successively, resin is dried, reuse ammonia alcohol (adding ammonia to pH value 9-10 in ethanol) gradation backflow eluting is eluted to alkaloid and extracts fully, merges eluent, after reclaiming ethanol, drying gets Radix Fissistigmatis Oldhamii total alkali extract, can be for the various dosage forms of preparation.
Technology two above-mentioned Radix Fissistigmatis Oldhamii alcohol extracts reclaim ethanol, transfer pH to 2-3 with hydrochloric acid, filter, last acidity is positive in exchange resin column, or acid cation exchange resin on the above-mentioned Radix Fissistigmatis Oldhamii acid percolate, after exchange back resin water, ethanol wash successively, reuse ammonia alcohol (adding ammonia to pH value 9-10 in ethanol) is eluted to alkaloid and extracts fully, collect eluent, behind the recovery ethanol, drying, get Radix Fissistigmatis Oldhamii total alkali extract, can be for the various dosage forms of preparation.
Technology three above-mentioned Radix Fissistigmatis Oldhamii alcohol extracts, reclaim ethanol, transfer pH to 2-3 with hydrochloric acid, filter, on the filtrate acid positive on exchange resin column or the sour percolate of above-mentioned Radix Fissistigmatis Oldhamii the acid cation exchange resin post, exchange back resin washes with water to water elution liquid pH6-7, discards, and continues to be eluted to alkaloid with the 2-20% sour water and extracts fully.Collect eluent, transfer pH9-10, filtration or centrifugal, the dry Radix Fissistigmatis Oldhamii total alkali extract that gets of collecting precipitation can be for the various dosage forms of preparation.
Technology four above-mentioned Radix Fissistigmatis Oldhamii alcohol extracts reclaim ethanol, transfer pH to 2-3 with hydrochloric acid, filter, get filtrate or above-mentioned Radix Fissistigmatis Oldhamii acid percolate, adjust pH, macroporous adsorptive resins on the filtrate, with distilled water flush away impurity, with ethanol elution, the collection eluent of 50-90%, after eluent reclaims ethanol, concentrate, drying gets Radix Fissistigmatis Oldhamii total alkali extract, can be for the various preparations of preparation.
The prescription of technology one, two cation exchange resiies can adopt following any method:
New cationic resin fully expands it with distilled water immersion 1-2 days, wash with water to eluate clear and bright colourless till, surplus water is removed, add 2-5 and doubly measure 0.5-2mol/l hydrochloric acid, constantly stir, soaked 1-3 hour, remove acid solution, wash with water till the eluate pH3-4, incline and remove surplus water.Add 2-5 and doubly measure 0.5-2mol/lNaOH solution, constantly stir, soaked about 1-3 hour, remove alkali liquor, reuse is washed to eluate pH7, and Yu Shui inclines.Add 2-5 at last and doubly measured the 1-2mol/lHCl solution soaking 1-3 hour, make cationic resin transfer the H type to, the disacidify liquid that inclines, wash with water to pH be 3-5, can adorn post and use.
New cationic resin was immersed in the distilled water 1-2 days, make its fully expand wash with water to eluate clear and bright colourless till, in the chromatographic column of packing into.Earlier with resin volume 10-20 0.5-2mol/l hydrochloric acid doubly, exchange with the flow velocity of every square centimeter of 1ml of per minute, make it become Hydrogen, wash with water then to effluent and be neutral.Then the 0.5-2mol/l sodium hydroxide (or sodium chloride) doubly measured of reuse resin volume 5-15 exchanges, and makes it reply the sodium type, and reuse is washed to eluate and does not contain sodium ion (inspect with flame method, if there is sodium ion to exist, flame is yellow during calcination).Repeat the processing of hydrochloric acid and sodium hydroxide (or sodium chloride) again.The 1-2mol/l hydrochloric acid of doubly measuring with resin volume 5-15 exchanges at last, makes it become Hydrogen, is washed to pH3-5 and can supplies usefulness.
The used water of aforesaid operations is distilled water.
Whether fully available alkaloid extract alkaloid precipitation reagent and detect.
The dry vacuum drying that adopts.The vacuum drying temperature is 50-90 ℃, and optimum temperature is 60-70 ℃.
Used eluent is ammonia alcohol (adding ammonia to pH value 9-10 in ethanol) in the technology one, two.
Used eluent is that the acetic acid, sulphuric acid, hydrochloric acid etc. of 2-204 are solvent in the technology three, and the best is the hydrochloric acid with 10%.
Macroporous resin adopts D-101 type resin or AB-8 type resin in the technology four, the D-101 type is washed till effluent with 95% ethanol to be mixed with water and not to produce muddiness at 1: 2, use massive laundering instead, the water logging bubble is standby, the AB-8 type soaks a couple of days with acetone, be washed till effluent with acetone behind the dress post and mix with water and do not produce muddiness, use massive laundering instead, water logging is steeped standby.
In the technology four macroporous resin be regenerated as that to be washed till eluate with 0.05～0.2mol/L caustic lye of soda colourless, be washed till neutrality with distilled water after, be washed till colourlessly with 95% ethanol, remove alcohol with massive laundering, get final product.
Adjust pH 5-9 in the technology four, the best is a pH value about 6.
In the technology four, be eluent with the ethanol of 50-90%, the best is 80% ethanol.
With Radix Fissistigmatis Oldhamii total extract or Radix Fissistigmatis Oldhamii total alkali is that raw material further is processed into folk prescription or the various dosage forms of compound recipe, has preparation and makes with extra care, and consumption is few, eutherapeutic advantage.This invention its superiority compared with the prior art is: the consumption of preparation is little, and the dispensing material accurately is convenient to take and carry, and is convenient to improve the quality standard comprehensively.
The specific embodiment
The preparation of embodiment 1 Radix Fissistigmatis Oldhamii total extract
Getting Radix Fissistigmatis Oldhamii and be ground into coarse powder, is solvent with 1% hydrochloric acid, and percolation to alkaloid extracts fully, and percolate continues purification or transfers pH9-10, filters, and collecting precipitation is for preparation, tablet, granule, dispersible tablet, capsule, various dosage forms such as syrup.
The preparation of embodiment 2 Radix Fissistigmatis Oldhamii total alkalis
Acid cation exchange resin on the above-mentioned Radix Fissistigmatis Oldhamii acid percolate after exchange back resin water, ethanol wash successively, dries resin, reuse ammonia alcohol (adding ammonia to pH9-10 in ethanol) gradation backflow eluting is eluted to alkaloid and extracts fully, merges eluent, after reclaiming ethanol, drying gets cobalt mountain breeze total alkali extract, can be for the various dosage forms of preparation, as injection, tablet, granule, capsule, oral liquid.
Embodiment 3 Radix Fissistigmatis Oldhamii total alkali freeze-dried powders
Getting an amount of cysteine adds in an amount of water for injection, after the stirring and dissolving, add Radix Fissistigmatis Oldhamii total alkali extract, transfer pH4-5 with 1ml/ hydrochloric acid, stirring and dissolving, add benzyl alcohol, stir, add the injection water to ormal weight, adding an amount of needle-use activated carbon stirs, the microporous filter membrane classification filters, and the filtrate quantitative aseptic is sub-packed in washing the vial with sterilizing-drying, puts on the lyophilizing frame, press the selected condition of freeze-drying curve, strict with time adjustable plate layer temperature and vacuum, finish until lyophilizing, recharge high-purity N then
2, jump a queue, roll lid, promptly.
Embodiment 4 Radix Fissistigmatis Oldhamii total alkali capsules
Get Radix Fissistigmatis Oldhamii total alkali and appropriate amount of auxiliary materials mixing, encapsulated, promptly.
Added adjuvant can be in the technology: any or multiple mixing in micropowder silica gel, starch, dextrin, the magnesium stearate etc. is used.
Embodiment 5 Radix Fissistigmatis Oldhamii total alkali sheets
Get Radix Fissistigmatis Oldhamii total alkali and appropriate amount of auxiliary materials mixing, the direct compression or the back tabletting of granulating, promptly.
Adding adjuvant in the technology can be microcrystalline Cellulose, polyvinylpolypyrrolidone, carboxymethylstach sodium, 30 POVIDONE K 30 BP/USP
30, any or multiple mixing in the micropowder silica gel, low-substituted hydroxypropyl cellulose, starch, dextrin, magnesium stearate etc. uses.
Claims (5)
1, the preparation of a kind of Radix Fissistigmatis Oldhamii extracts active ingredients and preparation, it is characterized in that adopting the root of annonaceae plant Radix Fissistigmatis Oldhamii or rattan is raw material, carry through alcohol extraction/sour water, the treated upper prop of alcohol extract or acid water extracting liquid, eluting, drying is made Radix Fissistigmatis Oldhamii total alkali extract, and makes various folk prescription/compound preparations with this.
2, the preparation of Radix Fissistigmatis Oldhamii extracts active ingredients according to claim 1 and preparation is characterized in that alcohol extraction/acid extraction to adopt the ethanol of 60-95% is the solvent alcohol extraction or is that solvent acid is carried with the acid of 0.2-10%.Alcohol extract reclaims ethanol, and adjust pH 2-3 filters, filtrate adjust pH 9-10 filtration/centrifugal, collecting precipitation is made Radix Fissistigmatis Oldhamii total extract or acid water extracting liquid adjust pH 9-10, filters, collecting precipitation is made the Radix Fissistigmatis Oldhamii total extract, and makes various folk prescription/compound preparations with this.
3, the preparation of Radix Fissistigmatis Oldhamii extracts active ingredients according to claim 1 and preparation is characterized in that Radix Fissistigmatis Oldhamii extracting solution upper prop eluting, adopts cation exchange resin column/macroporous resin column.
4, the preparation of Radix Fissistigmatis Oldhamii extracts active ingredients according to claim 1 and preparation, it is characterized in that the cation exchange resin eluting can adopt the acid of 2-20%, any in the ammonia alcohol (adding ammonia to adjust pH 9-10 in ethanol), macroporous resin can adopt the ethanol elution of 50-90%.
5, the preparation of Radix Fissistigmatis Oldhamii extracts active ingredients according to claim 1 and preparation, it is characterized in that the Radix Fissistigmatis Oldhamii total alkali can make Radix Fissistigmatis Oldhamii total alkali freeze-dried powder, Radix Fissistigmatis Oldhamii total alkali capsule, Radix Fissistigmatis Oldhamii total alkali sheet, Radix Fissistigmatis Oldhamii total extract tablet, Radix Fissistigmatis Oldhamii total extract capsule, Radix Fissistigmatis Oldhamii total extract low-sugar type syrup, Radix Fissistigmatis Oldhamii total extract Sugarless type oral liquid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA03118278XA CN1537573A (en) | 2003-04-15 | 2003-04-15 | Extraction of active ingredient of Zuanshanfeng, and method for preparing its prepn. |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA03118278XA CN1537573A (en) | 2003-04-15 | 2003-04-15 | Extraction of active ingredient of Zuanshanfeng, and method for preparing its prepn. |
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| CN1537573A true CN1537573A (en) | 2004-10-20 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101979069A (en) * | 2010-11-10 | 2011-02-23 | 江西天施康中药股份有限公司 | Method for preparing drill yamakaze syrup |
| CN105079204A (en) * | 2015-09-18 | 2015-11-25 | 陈昌泉 | Medicine for treating rheumatic and rheumatoid arthritis and preparation method of medicine |
| CN105434565A (en) * | 2015-12-28 | 2016-03-30 | 南昌理工学院 | Root of oldham fissistigma liniment |
| CN105641005A (en) * | 2015-11-11 | 2016-06-08 | 海南师范大学 | Fissistigma tungfangense extract, preparation method and applications thereof |
-
2003
- 2003-04-15 CN CNA03118278XA patent/CN1537573A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101979069A (en) * | 2010-11-10 | 2011-02-23 | 江西天施康中药股份有限公司 | Method for preparing drill yamakaze syrup |
| CN101979069B (en) * | 2010-11-10 | 2013-05-22 | 江西天施康中药股份有限公司 | Method for preparing drill yamakaze syrup |
| CN105079204A (en) * | 2015-09-18 | 2015-11-25 | 陈昌泉 | Medicine for treating rheumatic and rheumatoid arthritis and preparation method of medicine |
| CN105079204B (en) * | 2015-09-18 | 2018-11-06 | 陈昌泉 | A kind of drug and preparation method thereof for treating rheumatic and rheumatoid arthritis |
| CN105641005A (en) * | 2015-11-11 | 2016-06-08 | 海南师范大学 | Fissistigma tungfangense extract, preparation method and applications thereof |
| CN105641005B (en) * | 2015-11-11 | 2019-10-08 | 海南师范大学 | East melon Radix Fissistigmatis Oldhamii extract and the preparation method and application thereof |
| CN105434565A (en) * | 2015-12-28 | 2016-03-30 | 南昌理工学院 | Root of oldham fissistigma liniment |
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