CN103833559A - Extraction process of ephedrine - Google Patents
Extraction process of ephedrine Download PDFInfo
- Publication number
- CN103833559A CN103833559A CN201210489938.5A CN201210489938A CN103833559A CN 103833559 A CN103833559 A CN 103833559A CN 201210489938 A CN201210489938 A CN 201210489938A CN 103833559 A CN103833559 A CN 103833559A
- Authority
- CN
- China
- Prior art keywords
- ephedra
- ephedrine
- oxalic acid
- dimethylbenzene
- extraction
- 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
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to an extraction process of ephedrine, and belongs to the technical field of extraction of effective components in traditional Chinese medicines. The process provided by the invention comprises the following steps: pretreatment of ephedra; alkalization; extraction with xylene; extraction; concentration; and the like. By adopting the processes such as alkalization, extraction with xylene and extraction with oxalic acid, tedious processes in the prior art can be simplified, and high purity ephedrine can be quickly and effectively extracted.
Description
Technical field
The present invention relates to the extraction process of effective constituent in a kind of Chinese medicine, more particularly, the present invention relates to a kind of extraction process of ephedrine, belong to extracts active ingredients technical field in Chinese medicine.
Background technology
Chinese ephedra is Chinese medicine or claims the wind-cold-dispersing medicinal in Chinese medicine; Ancient times is called imperial sand, inferior phase.Include the plant of three kinds of Ephedras: ephedra sinica (Ephedra sinica), ephedra equisetina (Ephedra equisetina) and epheday intermedia (Ephedra intermedia), employing position is herb stem.Ephedra sinica ephedra sinica is undershrub, is often draft shape, the high 20-40 centimetre of stem.Branch is less, and woody stems is short and small, the shape of crawling; Sprig circle, to raw or verticillate, the long 2.5-6 centimetre of internode, 2 millimeters of diameters.
Main effective constituent in Chinese ephedra is alkaloid, example hydrochloric acid ephedrine, pseudoephedrine hydrochloride and N-Methylephedrine and demethyl ephedrine.
It is 200410042762.4 that State Intellectual Property Office discloses an application number in 2007.6.6, name is called the patent of invention of " Zeo-karb separates ephedrine method with expanding bed integrated technology single step purification ", this patent provides a kind of purification process of eco-friendly ephedrine, concrete steps are as follows: 2-3 times of buffer A diluted through conventional Chinese ephedra plant extraction method, synthesis method, the original liquid of the hydrochloric ephedrine through the processing of 0.05M dilute hydrochloric acid that microbe fermentation method or cell culture method obtain, adopt the one step absorption ephedrine hydrochloride of the expanding bed with particular design liquid distributor of polystyrene resin cation (R.C.) 001 × 7 Styrene DVB filling, adopt the 0.01M phosphate buffered saline buffer of the pH7.2 that contains 0.1M NaCl and 1.0M NaCl to carry out two step step elutes, collect the elutriant of second elution peak, obtain the ephedrine hydrochloride of purifying.Present method has been avoided the use of organic solvent dimethylbenzene, and the more traditional organic solvent extractionprocess of yield of product has improved 22%, reaches 86%, and product purity reaches 85%.
The method for purifying and separating of above-mentioned ephedrine cannot extract ephedrine efficiently, and technique is loaded down with trivial details, and cost is high.
Summary of the invention
The present invention is intended to solve in above-mentioned prior art and cannot extracts efficiently ephedrine, and technique is loaded down with trivial details, and the problem that cost is high provides a kind of extraction process of ephedrine, can extract fast and effectively the ephedrine in Chinese ephedra.
In order to realize foregoing invention object, its concrete technical scheme is as follows:
An extraction process for ephedrine, is characterized in that: comprise following processing step:
A, Chinese ephedra pre-treatment
Chinese ephedra is carried out to drying treatment, and removal of impurities is also pulverized, and obtains Ephedra;
B, alkalization
Ephedra is immersed in saturated sodium hydroxide, soaks 1-3 hour, filter, obtain the Ephedra that alkalizes;
C, dimethylbenzene extract
In the alkalization Ephedra obtaining in step B, add dimethylbenzene, described alkalization Ephedra and the mass volume ratio of dimethylbenzene are 1:2-5(g/ml), reflux, extracts 2-3 time, obtains dimethylbenzene extracting solution;
D, extraction
Think to add 2% oxalic acid in dimethylbenzene extracting solution, mix, in the water-bath of 50-80 DEG C, heat, obtain oxalic acid extraction liquid simultaneously;
E, concentrated
The oxalic acid extraction liquid concentrating under reduced pressure that step D is obtained, crystallisation by cooling obtains ephedrine solid extract.
Preferably, the present invention is in steps A, and described drying treatment is dry 2-5 hour at 70-80 DEG C.
Preferably, the present invention is in step C, and described Heating temperature is 80-105 DEG C.
Preferably, the present invention is in step C, and the described reflux time is 2-8 hour.
Preferably, the present invention is in step D, and the volume of 2% described oxalic acid is the 1/20-1/35 of dimethylbenzene extracting solution.
Preferably, the present invention, in step D, when described oxalic acid extraction liquid pH value is neutral, adds 2% oxalic acid, makes pH value remain 3-5.
The useful technique effect that the present invention brings:
1, alkalization, the dimethylbenzene that the present invention adopts extracts, the technique of oxalic acid extraction, can simplify loaded down with trivial details technique of the prior art, and fast and effeciently extract highly purified ephedrine.
2, before extraction, just Ephedra is immersed in saturated sodium hydroxide, soaks 1-3 hour, filters, and the alkalization process of this step can make Chinese ephedra technique in the time of extraction and purifying more smooth and easy, improves extraction yield and purification effect.
3, the processing parameter that the present invention adopts in step C and the processing parameter adopting in step D can effectively and stably extract in conjunction with dimethylbenzene and two steps of oxalic acid extraction, make two kinds of extraction effects reach best, improve follow-up purification effect.
Embodiment
embodiment 1
An extraction process for ephedrine, comprises following processing step:
A, Chinese ephedra pre-treatment
Chinese ephedra is carried out to drying treatment, and removal of impurities is also pulverized, and obtains Ephedra;
B, alkalization
Ephedra is immersed in saturated sodium hydroxide, soaks 1 hour, filter, obtain the Ephedra that alkalizes;
C, dimethylbenzene extract
In the alkalization Ephedra obtaining in step B, add dimethylbenzene, described alkalization Ephedra and the mass volume ratio of dimethylbenzene are 1:2, and reflux is extracted 2 times, obtains dimethylbenzene extracting solution;
D, extraction
Think to add 2% oxalic acid in dimethylbenzene extracting solution, mix, in the water-bath of 50 DEG C, heat, obtain oxalic acid extraction liquid simultaneously;
E, concentrated
The oxalic acid extraction liquid concentrating under reduced pressure that step D is obtained, crystallisation by cooling obtains ephedrine solid extract.
embodiment 2
An extraction process for ephedrine, comprises following processing step:
A, Chinese ephedra pre-treatment
Chinese ephedra is carried out to drying treatment, and removal of impurities is also pulverized, and obtains Ephedra;
B, alkalization
Ephedra is immersed in saturated sodium hydroxide, soaks 3 hours, filter, obtain the Ephedra that alkalizes;
C, dimethylbenzene extract
In the alkalization Ephedra obtaining in step B, add dimethylbenzene, described alkalization Ephedra and the mass volume ratio of dimethylbenzene are 1:5, and reflux is extracted 3 times, obtains dimethylbenzene extracting solution;
D, extraction
Think to add 2% oxalic acid in dimethylbenzene extracting solution, mix, in the water-bath of 80 DEG C, heat, obtain oxalic acid extraction liquid simultaneously;
E, concentrated
The oxalic acid extraction liquid concentrating under reduced pressure that step D is obtained, crystallisation by cooling obtains ephedrine solid extract.
embodiment 3
An extraction process for ephedrine, comprises following processing step:
A, Chinese ephedra pre-treatment
Chinese ephedra is carried out to drying treatment, and removal of impurities is also pulverized, and obtains Ephedra;
B, alkalization
Ephedra is immersed in saturated sodium hydroxide, soaks 2 hours, filter, obtain the Ephedra that alkalizes;
C, dimethylbenzene extract
In the alkalization Ephedra obtaining in step B, add dimethylbenzene, described alkalization Ephedra and the mass volume ratio of dimethylbenzene are 1:3.5, and reflux is extracted 3 times, obtains dimethylbenzene extracting solution;
D, extraction
Think to add 2% oxalic acid in dimethylbenzene extracting solution, mix, in the water-bath of 65 DEG C, heat, obtain oxalic acid extraction liquid simultaneously;
E, concentrated
The oxalic acid extraction liquid concentrating under reduced pressure that step D is obtained, crystallisation by cooling obtains ephedrine solid extract.
embodiment 4
On the basis of embodiment 1-3:
Preferably, the present invention is in steps A, and described drying treatment is to be dried 2 hours at 70 DEG C.
Preferably, the present invention is in step C, and described Heating temperature is 80 DEG C.
Preferably, the present invention is in step C, and the described reflux time is 2 hours.
Preferably, the present invention is in step D, and the volume of 2% described oxalic acid is 1/35 of dimethylbenzene extracting solution.
Preferably, the present invention, in step D, when described oxalic acid extraction liquid pH value is neutral, adds 2% oxalic acid, makes pH value remain 3.
embodiment 5
On the basis of embodiment 1-3:
Preferably, the present invention is in steps A, and described drying treatment is to be dried 5 hours at 80 DEG C.
Preferably, the present invention is in step C, and described Heating temperature is 105 DEG C.
Preferably, the present invention is in step C, and the described reflux time is 8 hours.
Preferably, the present invention is in step D, and the volume of 2% described oxalic acid is 1/20 of dimethylbenzene extracting solution.
Preferably, the present invention, in step D, when described oxalic acid extraction liquid pH value is neutral, adds 2% oxalic acid, makes pH value remain 5.
embodiment 6
On the basis of embodiment 1-3:
Preferably, the present invention is in steps A, and described drying treatment is to be dried 3.5 hours at 75 DEG C.
Preferably, the present invention is in step C, and described Heating temperature is 90 DEG C.
Preferably, the present invention is in step C, and the described reflux time is 5 hours.
Preferably, the present invention is in step D, and the volume of 2% described oxalic acid is 1/30 of dimethylbenzene extracting solution.
Preferably, the present invention, in step D, when described oxalic acid extraction liquid pH value is neutral, adds 2% oxalic acid, makes pH value remain 4.
Claims (6)
1. an extraction process for ephedrine, is characterized in that: comprise following processing step:
A, Chinese ephedra pre-treatment
Chinese ephedra is carried out to drying treatment, and removal of impurities is also pulverized, and obtains Ephedra;
B, alkalization
Ephedra is immersed in saturated sodium hydroxide, soaks 1-3 hour, filter, obtain the Ephedra that alkalizes;
C, dimethylbenzene extract
In the alkalization Ephedra obtaining in step B, add dimethylbenzene, described alkalization Ephedra and the mass volume ratio of dimethylbenzene are 1:2-5, and reflux, extracts 2-3 time, obtains dimethylbenzene extracting solution;
D, extraction
Think to add 2% oxalic acid in dimethylbenzene extracting solution, mix, in the water-bath of 50-80 DEG C, heat, obtain oxalic acid extraction liquid simultaneously;
E, concentrated
The oxalic acid extraction liquid concentrating under reduced pressure that step D is obtained, crystallisation by cooling obtains ephedrine solid extract.
2. the extraction process of a kind of ephedrine according to claim 1, is characterized in that: in steps A, described drying treatment is dry 2-5 hour at 70-80 DEG C.
3. the extraction process of a kind of ephedrine according to claim 1, is characterized in that: in step C, described Heating temperature is 80-105 DEG C.
4. the extraction process of a kind of ephedrine according to claim 1, is characterized in that: in step C, the described reflux time is 2-8 hour.
5. the extraction process of a kind of ephedrine according to claim 1, is characterized in that: in step D, the volume of 2% described oxalic acid is the 1/20-1/35 of dimethylbenzene extracting solution.
6. the extraction process of a kind of ephedrine according to claim 1, is characterized in that: in step D, when described oxalic acid extraction liquid pH value is neutral, add 2% oxalic acid, make pH value remain 3-5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210489938.5A CN103833559A (en) | 2012-11-27 | 2012-11-27 | Extraction process of ephedrine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210489938.5A CN103833559A (en) | 2012-11-27 | 2012-11-27 | Extraction process of ephedrine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103833559A true CN103833559A (en) | 2014-06-04 |
Family
ID=50797500
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210489938.5A Pending CN103833559A (en) | 2012-11-27 | 2012-11-27 | Extraction process of ephedrine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103833559A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957234A (en) * | 2017-03-23 | 2017-07-18 | 陕西金冠牧业有限公司 | A kind of preparation method of pseudoephedrine hydrochloride |
| CN108823963A (en) * | 2018-07-24 | 2018-11-16 | 中国农业科学院麻类研究所 | A kind of Chinese fiber crops antibacterial fiber material preparation method |
| CN109251149A (en) * | 2018-09-13 | 2019-01-22 | 安徽佛子岭面业有限公司 | A method of extracting ephedrine from Chinese ephedra |
-
2012
- 2012-11-27 CN CN201210489938.5A patent/CN103833559A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957234A (en) * | 2017-03-23 | 2017-07-18 | 陕西金冠牧业有限公司 | A kind of preparation method of pseudoephedrine hydrochloride |
| CN108823963A (en) * | 2018-07-24 | 2018-11-16 | 中国农业科学院麻类研究所 | A kind of Chinese fiber crops antibacterial fiber material preparation method |
| CN109251149A (en) * | 2018-09-13 | 2019-01-22 | 安徽佛子岭面业有限公司 | A method of extracting ephedrine from Chinese ephedra |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20190210946A1 (en) | Method for preparing high-purity cannabidiol | |
| CN101830849B (en) | Method for preparing simplified high-purity bulleyaconitine A | |
| CN102351926B (en) | A kind of preparation method of arctinin | |
| CN103694364A (en) | Method for synchronously extracting, separating and purifying polysaccharides and flavones of cyclocarya paliurus | |
| CN102850219A (en) | Method for extracting rosmarinic acid from folia perillae acutae | |
| CN102146083A (en) | Method for separating and extracting cepharanthine | |
| CN103833559A (en) | Extraction process of ephedrine | |
| CN104447941B (en) | A kind of synchronous method of extracting of glucosidase procyanidins and Tea Saponin in oil-tea camellia husks | |
| CN102070527A (en) | Method for extracting high-purity huperzine A and huperzine B from medicinal plant phlegmariurus crutomerianus | |
| CN104072554A (en) | Method for extracting paederia scandens from fevervine | |
| CN103012518B (en) | Production process for simultaneously extracting asperuloside and chlorogenic acid from folium cortex eucommiae | |
| CN103274992A (en) | Method for preparing high-purity 1-deoxynojirimycin with combined membrane separation and column chromatography technology | |
| CN1927857A (en) | Extraction and purification process of buckwheat sprout total flavone | |
| CN103073561B (en) | Process of extracting artemisinin by biological enzyme-percolation method | |
| CN102643285A (en) | Method for preparing magnolin from magnolia flower | |
| CN100357251C (en) | Technique for producing purple common perilla rosemary acid | |
| CN102329209A (en) | Method for extracting emodin from giant knotweed rhizome | |
| CN104231011A (en) | Preparation method of verbascoside | |
| CN103833802A (en) | Preparation method of salidroside | |
| CN102675142B (en) | Method for purifying capsicine in hot pepper | |
| CN105367424A (en) | Method for preparing high-purity chlorogenic acid from eupatorium adenophorum Spreng | |
| CN107056872B (en) | The rapid extracting method of Radix Mussaendae thuja acid methyl esters | |
| CN104478842A (en) | Method for extracting jaceosidin and eupatilin from folium artemisiaeargyi | |
| CN107573312A (en) | Utilize the method for redpunjab sumac root extraction young fustic | |
| CN102241578A (en) | Extraction method of chimaphilin |
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: 20140604 |