CN1213043C - Preparation method for cnidium fruit - Google Patents
Preparation method for cnidium fruit Download PDFInfo
- Publication number
- CN1213043C CN1213043C CN 03134435 CN03134435A CN1213043C CN 1213043 C CN1213043 C CN 1213043C CN 03134435 CN03134435 CN 03134435 CN 03134435 A CN03134435 A CN 03134435A CN 1213043 C CN1213043 C CN 1213043C
- Authority
- CN
- China
- Prior art keywords
- preparation
- crystallization
- osthole
- alcohol
- alkali lye
- 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.)
- Expired - Fee Related
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention relates to a preparation method of the raw materials of a biological preparation, particularly to a preparation method of osthol, which is characterized in that alkaline liquid is used for impurity removal, wash and crystallization in the preparation process; the alkaline liquid and activated carbon are used for impurity removal in the preparation process; the alkaline liquid is NaOH. The preparation method of osthol has the characteristics of easy preparation, high production quantity, low cost and good safety.
Description
Technical field: the present invention relates to a kind of preparation method of biotechnological formulation raw material, particularly about a kind of preparation method of osthole.
Background technology: the preparation method of existing osthole comprises following several:
1, " natural medicinal component extraction separation and preparation " document ISBN7-5067-0885-X/R8226 of Sun Wenji chief editor; 0789).It gets Fructus Cnidii fruit meal 1kg, and with 5 times of amount alcohol immersion 3 times, pure immersion liquid merges, and is evaporated on a small quantity, is divided into oil reservoir and water layer.Oil reservoir is separated out mass crystallization with placing behind the petroleum ether extraction 3 times, through dehydrated alcohol recrystallization repeatedly, the brilliant about 7g of white blocks, be osthole.
Precious traditional Chinese medical science traditional Chinese medicines 1999. (10) 6 when 2, osthole extraction efficiency and several solvent concern the Liu Jiang qin in the Fructus Cnidii; (the Fructus Cnidii Study on extraction is executed arylidene layer Chinese medicine magazine 2000. (14) 1.When extracting research, think that with little polar solvents such as high density alcohol or acetone be good more.
3, utilize the carbon dioxide upercritical fluid extraction method to be prepared.
Above-mentioned preparation technology's shortcoming is:
When 1, extracting, the use repeatedly of solvent can increase extraction cost during use high density alcohol was unfavorable for producing in the production preparation process.
When 2, utilizing in the petroleum ether extraction oil reservoir osthole, because sherwood oil is limited to the solubleness of osthole, can not be transferred to osthole in the sherwood oil fully, and osthole can not all be separated out from sherwood oil, finally can cause all remaining result that osthole is arranged in oil reservoir, the sherwood oil, suitability for industrialized production is handled difficulty, easily causes waste.
3, osthole is dissolved in the sherwood oil that boils in theory, and insoluble in cold sherwood oil.It is solubleness and little in the sherwood oil that boils, so in the extraction process, in order to realize extraction " fully ", just must operate with a large amount of sherwood oils, the result also can make production cost increase.
4, sherwood oil belongs to flammable and explosive substance, at factory's mass production, brings potential safety hazard can for the links such as production, stock of factory in this mode.Promptly because factors such as safety are inapplicable in suitability for industrialized production.
5, sherwood oil easily causes production bottleneck because itself is little to the solubleness of osthole in the production preparation process, causes production output to amplify, and causes producing being in a kind of small-scale production pattern all the time.
6, carbon dioxide upercritical fluid extraction, because the restriction of production unit condition, each charging capacity is restricted, specific duty is difficult to improve, again because carbon dioxide upercritical fluid extraction equipment price costliness causes extraction cost too high.
Summary of the invention: the purpose of this invention is to provide a kind of preparation method of osthole, it has preparation easily, the turnout height, and cost is low, the characteristics that security is good.
Technical scheme of the present invention is: design a kind of preparation method of osthole, it is characterized in that: use the alkali lye removal of impurities in preparation process.
In preparation process, use alkali liquid washing, crystallization.
In preparation process, use alkali lye and gac impurity elimination.
Described alkali lye is NaOH.
Described alkali lye is KOH.
Described alkali lye is Ca (OH)
2
The Fructus Cnidii raw material extracts with the 70%-90% methanol eddy.
The Fructus Cnidii raw material is used the 70%-90% alcohol reflux.
Described alkali lye is NH
4OH.
The Fructus Cnidii raw material extracts with 80% methanol eddy, and extracting solution is merged to be evaporated to not to be had alcohol or do not have alcohol substantially, concentrated solution is placed and is spent the night, abandon supernatant liquor, add clear water, add alkali, fully stirring throw out placed 12 to 24 hours, abandon supernatant liquor, with the sig water wash crystallization for preparing in advance, clear water wash crystallization, it is dissolving crystallized to remove alkali lye alcohol, activated carbon decolorizing filtering gac, solution crystallization, goes out crystallization, wash crystallization, drying, finished product.
Characteristics of the present invention are:
1, in preparation process, uses the alkali lye removal of impurities.Because alkali lye can be dissolved in the most of impurity in the Fructus cnidii extract wherein, and osthole can form crystallization in alkaline solution, thereby replaced the ether extraction of existing preparation method PetroChina Company Limited., reduced cost of supplementary product, reduced the hidden danger in production, the library procedure; In preparation process, removed sherwood oil to the low production bottleneck of osthole solubleness after, be easy to industrialized production, turnout can amplify at any time according to the market requirement, produces in batches.
2, in preparation process, use alkali lye and gac impurity elimination.Can directly remove impurity such as wax in the raw material and chlorophyll, simple, the easy row that make that treating process becomes.
3, Fructus Cnidii raw material is used the 70%-90% alcohol reflux.During extraction, use the alcoholic solution of 70%-90% concentration, help the use repeatedly of solvent aborning, in the production preparation process, reduce extraction cost; During extraction, use the alcoholic solution of 70%-90% concentration, replace other solvents such as acetone, strengthened the security in production, the library procedure.
Embodiment: embodiment 1 gets Fructus Cnidii raw material 1kg, extracts three times with 80% methanol eddy in Backflow bottle, and the methyl alcohol volume is respectively 4500ml, 3000ml, 3000ml.Each reflux extracting time is one hour, and united extraction liquid is evaporated to 500ml with Rotary Evaporators, pour beaker into, placed 12 hours, abandon supernatant liquor, and, adding solid sodium hydroxide again to precipitating the clear water that adds 400ml, control sodium hydroxide final concentration is 0.025 volumetric molar concentration, fully stir, 10 to 15 minutes, place more than 12 hours, abandon supernatant liquor, wash the crystallization that settles out with 0.02 mol sodium that configures in advance, washing is divided into four times to be carried out, and each alkali lye volume is 200ml, after crystallizing and washing is clean, with clear water flush away alkali lye, remove moisture, crystallization is controlled at 70% with dissolve with ethanol (ethanolic soln is 250ml) with ethanolic soln concentration, fully after the dissolving, heated and stirred is placed crystallization (time requirement was greater than 24 hours), leaches crystallization, with a small amount of alcohol washing, remove solution, obtain faint yellow crystallization, oven dry, crystallization is weighed as 20.5g, and detecting purity is 60%.
Embodiment 2 Fructus Cnidii raw material 1kg, with 80% alcohol reflux three times, the ethanol volume is respectively 5000ml, 4500ml, 4000ml in Backflow bottle.Each extraction time is 1.2 hours, united extraction liquid, be evaporated to 700ml with Rotary Evaporators, pour beaker into and placed 14 hours, abandon supernatant liquor, and to precipitating the clear water that adds 600ml, add solid potassium hydroxide again, control potassium hydroxide final concentration is 0.027 volumetric molar concentration, fully stirs, 10 to 15 minutes, place more than 12 hours, abandon supernatant liquor, wash the crystallization that settles out with the 0.019 volumetric molar concentration potassium hydroxide solution that configures in advance, washing is divided into four times and carries out, each alkali lye volume is 200ml, after crystallizing and washing is clean, with clear water flush away alkali lye, remove moisture, crystallization is controlled at 75% to 80% with dissolve with methanol (methanol solution is 300ml) with concentration of methanol solution, adds gac (gac weight is 16g), thermal backflow decolouring 40 minutes, leach methanol solution, pour beaker into, and with a small amount of 80% methanol wash gac, add water in methanol solution, making the methyl alcohol final concentration is 50%.After fully stirring, place crystallization (time requirement was greater than 24 hours), leach crystallization,, remove solution, obtain white crystals with a small amount of alcohol washing, oven dry, crystallization is weighed as 13g, and detecting purity is 86%.Owing to used the gac impurity elimination, increased so obtain finished product purity.
Claims (5)
1, a kind of preparation method of osthole is characterized in that: in preparation process with the alkali lye removal of impurities of 0.025 mole or 0.027 volumetric molar concentration.
2, the preparation method of a kind of osthole according to claim 1 is characterized in that: in preparation process with alkali liquid washing, the crystallization of 0.019 volumetric molar concentration or 0.02 volumetric molar concentration.
3, the preparation method of a kind of osthole according to claim 1 is characterized in that: described alkali lye is NaOH.
4, the preparation method of a kind of osthole according to claim 1 is characterized in that: the Fructus Cnidii raw material, and use 70%--90% methyl alcohol or use the 70%--90% alcohol reflux.
5, the preparation method of a kind of osthole according to claim 1, it is characterized in that: the Fructus Cnidii raw material, extract with 80% methanol eddy, the extracting solution merging is evaporated to nothing alcohol or does not have alcohol substantially, concentrated solution is placed and is spent the night, abandon supernatant liquor, add clear water, add solid sodium hydroxide again, control sodium hydroxide final concentration is 0.025 volumetric molar concentration, fully stirs, 10 to 15 minutes, place more than 12 hours, abandon supernatant liquor, wash the crystallization that settles out with 0.02 mol sodium that configures in advance, after crystallizing and washing is clean, with clear water flush away alkali lye, remove moisture, activated carbon decolorizing filtering gac, solution crystallization, go out crystallization, wash crystallization, dry, finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03134435 CN1213043C (en) | 2003-07-16 | 2003-07-16 | Preparation method for cnidium fruit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03134435 CN1213043C (en) | 2003-07-16 | 2003-07-16 | Preparation method for cnidium fruit |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1482123A CN1482123A (en) | 2004-03-17 |
| CN1213043C true CN1213043C (en) | 2005-08-03 |
Family
ID=34154485
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03134435 Expired - Fee Related CN1213043C (en) | 2003-07-16 | 2003-07-16 | Preparation method for cnidium fruit |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1213043C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114890974A (en) * | 2022-06-09 | 2022-08-12 | 湖北医药学院 | Method for extracting osthole by response surface design method |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332603C (en) * | 2004-07-06 | 2007-08-22 | 江苏省农业科学院 | Fructus cnidii complex composition |
| JP4844955B2 (en) * | 2005-07-29 | 2011-12-28 | 独立行政法人国立がん研究センター | Antitumor agent |
| CN100356851C (en) * | 2005-10-28 | 2007-12-26 | 江苏省农业科学院 | Fructus cnidii thuricin complex insecticide |
| CN101948459B (en) * | 2010-11-02 | 2012-07-04 | 重庆市中药研究院 | Method for extracting osthole from traditional Chinese medicine fructus cnidii |
| CN101973977B (en) * | 2010-11-03 | 2012-02-08 | 西安应化生物技术有限公司 | Method for preparing osthole |
| CN102641314A (en) * | 2011-02-22 | 2012-08-22 | 广州大光制药有限公司 | Medicine composition for preventing and/or treating gynecological diseases |
-
2003
- 2003-07-16 CN CN 03134435 patent/CN1213043C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114890974A (en) * | 2022-06-09 | 2022-08-12 | 湖北医药学院 | Method for extracting osthole by response surface design method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1482123A (en) | 2004-03-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101704867B (en) | Method for preparing naringin or hesperidin | |
| CN101250106B (en) | Method for extracting chlorogenic acid | |
| CN101817853A (en) | Method for extracting tea saponin by adopting tea seed cake | |
| CN1213043C (en) | Preparation method for cnidium fruit | |
| CN102311468A (en) | Clean production method of hesperidin | |
| CN1053892C (en) | Preparation method of diversine | |
| CN107353183A (en) | A kind of method that high-content of resveratrol is extracted from giant knotweed | |
| CN1113893C (en) | Method for extracting hytosterol from vegitable oil asphalt or tall oil asphalt | |
| CN1817865A (en) | Preparation of sinomontanine and its hydrobromide | |
| CN103483403B (en) | A kind of circulation extracting method of hesperidine of purifying from tangerine slag | |
| CN100374529C (en) | Method for preparing biological diesel oil from saurauia tristyla var oldhamii oil | |
| CN105985315A (en) | Method for extracting nicotine from tobacco waste | |
| CN110128676A (en) | A kind of method and its application for slightly refining lignin in stalk using oxygen catalytic ethyl alcohol | |
| CN102344426A (en) | Method for extracting and purifying lovastatin | |
| CN101818184A (en) | Method for extracting rutin from sophora japonica | |
| CN1303078C (en) | Process for preparing effective constituent in tea | |
| CN101033175A (en) | Method of extracting veratric alcohol from peanut plant after harvesting peanut fruit | |
| CN1038427C (en) | Method for extracting grease and tea saponin by one-step leaching cake meal | |
| CN100358811C (en) | Process for extracting lignin by acid separation | |
| CN106967030A (en) | A kind of extraction and purification process of dihydromyricetin | |
| CN202011848U (en) | Diosmin production system | |
| CN104418852A (en) | Extracting method and application of high-purity coptisine | |
| CN1696130A (en) | Method for continuous extracting chlorophyll from silkworm dropping | |
| CN110105195A (en) | A method of extracting dihydroartemisinic acid from sweet wormwood wax oil | |
| CN1241930C (en) | Shaddock glycoside extracting and refining process from shaddock |
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 | ||
| ASS | Succession or assignment of patent right |
Owner name: ZHOU JIA Free format text: FORMER OWNER: XI N GREEN SPRING BIO-TECHNOLOGY CO., LTD. Effective date: 20080711 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20080711 Address after: Taibai Road, Beilin District in Shaanxi province Xi'an City, No. twenty-four West Village 22 floor No. 506 Patentee after: Zhou Jia Address before: Shaanxi city of Xi'an province high tech Zone Road No. 67 with light Jiayuan 10903 Patentee before: Xi'an Green Spring Bio-technology Co., Ltd. |
|
| ASS | Succession or assignment of patent right |
Owner name: DAI WEIZHENG Free format text: FORMER OWNER: ZHOU JIA Effective date: 20091002 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20091002 Address after: Xi'an City, Shaanxi province science and technology 2 new homes 11601 Maple Road Patentee after: Dai Weizheng Address before: Taibai Road, Beilin District in Shaanxi province Xi'an City, No. twenty-four West Village 22 floor No. 506 Patentee before: Zhou Jia |
|
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: SHAANXI LONGFU BIOLOGICAL CHEMICAL CO., LTD. Assignor: Dai Weizheng Contract fulfillment period: 2009.11.1 to 2011.10.31 contract change Contract record no.: 2009610000021 Denomination of invention: Preparation method for cnidium fruit Granted publication date: 20050803 License type: exclusive license Record date: 20091120 |
|
| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.11.1 TO 2011.10.31; CHANGE OF CONTRACT Name of requester: SHANXI LONGFU BIOCHEMICAL ENGINEERING CO., LTD Effective date: 20091120 |
|
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20050803 Termination date: 20110716 |