CN104672190B - Method for recrystallizing gibberellin mother liquor - Google Patents
Method for recrystallizing gibberellin mother liquor Download PDFInfo
- Publication number
- CN104672190B CN104672190B CN201410761337.4A CN201410761337A CN104672190B CN 104672190 B CN104672190 B CN 104672190B CN 201410761337 A CN201410761337 A CN 201410761337A CN 104672190 B CN104672190 B CN 104672190B
- Authority
- CN
- China
- Prior art keywords
- gibberellins
- solution
- extraction
- recrystallized
- mother solution
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D307/93—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems condensed with a ring other than six-membered
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention discloses a method for recrystallizing a gibberellin mother liquor, and relates to the field of production of biochemical pesticides. The method specifically comprises the following steps: back extraction: adding a back extraction agent to the gibberellin mother liquor at the volume ratio of 1 to (2-5), stirring evenly, adding an alkaline solution, adjusting the pH value to be 4.0-7.0, and separating to obtain a water phase; extraction: adding an acid solution to the water phase containing gibberellin, adjusting the pH to be 1.5-3.5, adding an organic ester extraction agent according to the volume ratio of 1 to (0.7-1.2), extracting and separating to obtain an organic ester phase; dehydration: adding a dehydrating agent to the extracted organic ester phase and removing moisture; and concentration and crystallization: filtering and removing the dehydrating agent, carrying out vacuum concentration on the dehydrated organic ester phase, crystallizing and drying to obtain a gibberellin product. According to the method, the yield of the gibberellin powder can be maximized; great consumption of an organic solvent and an emulsifier required in the preparation process of missible oil can also be reduced; and the ecological environment and the personnel health are effectively protected.
Description
Technical field
The invention belongs to biofermentation --- biochemical pesticides production field, it is related to carrying for a plant growth regulators
Take method.
Background technology
Gibberellins, are the class phytohormone being widely present in plant.Its chemical constitution belongs to Diterpeneses acid, by Fourth Ring bone
Frame derives and obtains.It is a broad spectrum activity plant growth regulator, crop growth can be promoted, is allowed to ripe ahead of time, improves and produce
Amount, improvement quality；The dormancy of the organs such as seed, tuber and bulb, stratification can rapidly be broken；Reduce flower bud, flower, bell, fruit
Come off, improve fruit fruiting rate or formed stenospermocarpy.Gibberellins are widely used in agricultural production, with preferably effect
Really.
For a long time, the mother solution after gibberellins crystallization is configured to be used after cream typically by addition solvent and auxiliary agent.
Gibberellins market demand than larger, in recent years due to the requirement by environmental conservation, and gibberellins market supply and demand structure situation
Change, the Requirement Increasess of gibberellins crystal powder, and gibberellin emulsion sentiment undertone progressively glides, demand is fewer and feweri.
Gibberellin emulsion market demand is reduced, and in a large number storage is overstock to cause mother solution, is gone down to badly influence production for a long time and is looked forward to
Industry economic benefit, while environmental conservation is also had influence on, therefore it is extremely important to crystallizing the control of Mother liquor, from gibberellins mother solution
Carry out again isolating and purifying crystallization, obtain recrystallization powder and there is larger economic benefit and social benefit.
The content of the invention
The present invention is directed to defect described above, there is provided a kind of side of the big gibberellins mother solution recrystallization of gibberellins powder yield
Method.
The purpose of the present invention is achieved through the following technical solutions.
A kind of method of gibberellins mother solution recrystallization, it is characterised in that：It is made up of following steps successively：
（1）Back extraction：Gibberellins mother solution by volume 1：2 ~ 5 add strippant, strippant to may be selected from as carbonate
Aqueous solution or aqueous phosphatic, after stirring, add alkaline solution that its pH value is adjusted to into 4.0 ~ 7.0, in this pH value range
In the form of gibberellins salt, because gibberellins salt is soluble in water, and dissolubility in organic solvent is less, leads to for inner gibberellin
Crossing back extraction can make the gibberellins in mother solution be transformed into salt, and enter water phase, isolated water phase from organic faciess.
（2）Extraction：Acid solution is added toward the water phase containing gibberellins, pH to 1.5 ~ 3.5 is adjusted, in this pH value range
Inner gibberellin is insoluble in water in the form of gibberellins free acid because gibberellins free acid is soluble in organosilane ester solvent,
So by volume 1.0：0.7 ~ 1.2 addition organosilane ester extractant is extracted, and extracts back the gibberellins in water phase organic
Ester phase, separates to obtain organic ester phase.
（3）Dehydration：Add dehydrant toward the organic ester phase after extraction, remove moisture.Dehydrant preferentially elects anhydrous chlorine as
One or more of change calcium or anhydrous sodium sulfate or anhydrous magnesium sulfate.
（4）Condensing crystallizing：Dehydrant is filtered to remove, the organic ester after dehydration is mutually carried out concentrating under reduced pressure, after crystallizing and drying
Obtain gibberellins product.
Step（1）The water phase of resulting separation after middle addition strippant, can add enzyme material the water is mutually carried out it is pre-
Process, enzyme material may be selected from one or more for saccharifying enzyme, amylase, Lactose enzyme.
Step（1）Described strippant can further be optimized for 0.8 ~ 3.0% sodium bicarbonate solution or 0.8 ~ 3.0% carbonic acid
Sodium solution or 0.8 ~ 3.0% diammonium phosphate and ammonium dihydrogen phosphate or 0.8 ~ 3.0% disodium hydrogen phosphate and sodium dihydrogen phosphate composition
Buffer solution.Described alkaline solution may be selected from one or more for NaOH solution or KOH solution or ammonia spirit.Described
PH value can further optimize and be adjusted to as 4.8 ~ 6.5.
Step（2）Described organosilane ester extractant can further be optimized for the one of ethyl ester class or butyl ester class or isoamyl esters
Plant or several.Described acid solution may be selected from one or more for sulfuric acid solution or hydrochloric acid solution or phosphoric acid solution.It is described
PH value can further optimize and be adjusted to as 2.0 ~ 3.0.
Step（4）Described in concentrating under reduced pressure, its vacuum preferably be -0.08 ~ -0.095Mpa, chuck circulating water temperature
Degree is preferably 65 ~ 75 DEG C, and material temperature is preferably 30 ~ 40 DEG C.
Back extraction of the present invention and extraction step are carried out at normal temperatures.Organic faciess of this technique after back extraction
Organic faciess capable of circulation after simple process to apply mechanically, if product yield is low after condensing crystallizing, after can separating to back extraction
Carry out second back extraction-extraction-condensing crystallizing process, or the water after esters extract and separate is mutually carried out second extraction-
Condensing crystallizing process, extracts through back extraction again or again the two processes, and solution impurity content is reduced, is easy to concentration knot
Crystalline substance, gibberellins total yield of products is up to more than 90%.For the high mother solution of sugar content, the water after back extraction is mutually by adding enzyme
Class material carries out pretreatment, reduces solution viscosity, improves extraction yield, improving product purity and yield.
Beneficial effects of the present invention are：From the angle of gibberellins mother solution, by using back extraction recrystallize technique from
Powder product is extracted in mother solution, the technique for overcoming mother liquor cream is limited to, maximize gibberellins powder yield, improve enterprise
Industry economic benefit, meets wilderness demand of the client to gibberellins powder.And because GA content is significantly reduced in mother solution,
So that being also significantly reduced by the quantity of mother liquor cream, cream production is reduced with while usage amount, can be reduced cream and be matched somebody with somebody
It is strong to personnel during a large amount of consumption of required organic solvent and emulsifying agent, reduction preparation, storage, transport, use during system
Health and the infringement of ecological environment, reduce carrying cost and fire danger, effective protection ecological environment and personnel health, its Ecological Effect
Benefit and social benefit also highly significant.
Specific embodiment
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.
Embodiment 1.
Gibberellins mother solution 100ml is taken, the sodium bicarbonate solution 300ml of strippant 1.0% is added, after stirring, is added
Its pH is adjusted to 4.8 by 30%NaOH solution, and after back extraction is separated, water is added sulfuric acid solution and adjusts after pH to 2.0, and by volume 1.0：
1.0 addition ethyl acetate are extracted, and the organic faciess addition dehydrant anhydrous calcium chloride after extraction removes moisture, is filtered to remove de-
Organic faciess after dehydration are carried out concentrating under reduced pressure by water preparation, and concentrating under reduced pressure vacuum is -0.08Mpa, and chuck circulating water temperature is 75
DEG C, material temperature is 40 DEG C, and gibberellins product is obtained after crystallizing and drying, and product yield is 83%.
Embodiment 2.
Gibberellins mother solution 100ml is taken, the sodium carbonate liquor 250ml of strippant 0.8% is added, after stirring, 30% is added
Its pH is adjusted to 5.45 by NaOH solution, and after back extraction is separated, water is added sulfuric acid solution and adjusts after pH to 2.5, and by volume 1.0：
0.8 addition butyl acetate is extracted, and the organic faciess addition dehydrant anhydrous magnesium sulfate after extraction removes moisture, is filtered to remove de-
Organic faciess after dehydration are carried out concentrating under reduced pressure by water preparation, and concentrating under reduced pressure vacuum is -0.085Mpa, and chuck circulating water temperature is
72 DEG C, material temperature is 38 DEG C, and gibberellins product is obtained after crystallizing and drying, and product yield is 81%.After separating to n-butyl acetate extraction
Water mutually carries out second extraction-condensing crystallizing process, and operating procedure repeats the above method, and gibberellins total yield of products can
Up to 88%.
Embodiment 3.
Gibberellins mother solution 500ml is taken, the sodium bicarbonate solution 1500ml of strippant 1.5% is added, after stirring, is added
Its pH is adjusted to 5.85 by 30%NaOH solution, and after back extraction is separated, water is added sulfuric acid solution and adjusts after pH to 2.7, and by volume 1.0：
1.0 addition isoamyl acetates are extracted, and the organic faciess addition dehydrant anhydrous sodium sulfate after extraction removes moisture, is filtered to remove
Organic faciess after dehydration are carried out concentrating under reduced pressure by dehydrant, and concentrating under reduced pressure vacuum is -0.09Mpa, and chuck circulating water temperature is
68 DEG C, material temperature is 36 DEG C, and gibberellins product is obtained after crystallizing and drying, and product yield is 85%.
Embodiment 4.
Gibberellins mother solution 500ml is taken, the diammonium phosphate of strippant 2.0% and ammonium dihydrogen phosphate is added（Volume ratio 2:1）It is slow
Solution 2000ml is rushed, after stirring, adds 30% ammonia that its pH is adjusted to into 6.3, after back extraction is separated, water is added hydrochloric acid solution
After adjusting pH to 3.0, by volume 1.0：0.9 addition ethyl acetate is extracted, and the organic faciess addition dehydrant after extraction is anhydrous
Calcium chloride removes moisture, is filtered to remove dehydrant, and the organic faciess after dehydration are carried out into concentrating under reduced pressure, concentrating under reduced pressure vacuum for-
0.09Mpa, chuck circulating water temperature is 70 DEG C, and material temperature is 37 DEG C, and gibberellins product is obtained after crystallizing and drying, and product yield is
84%。
Embodiment 5.
Gibberellins mother solution 500ml is taken, the sodium carbonate liquor 2000ml of strippant 1.0% is added, after stirring, 30% is added
Its pH is adjusted to 5.5 by NaOH solution, and after back extraction is separated, water is added phosphoric acid solution and adjusts after pH to 2.5, and by volume 1.0： 1.0
Ethyl acetate is added to be extracted, the organic faciess addition dehydrant anhydrous sodium sulfate after extraction removes moisture, is filtered to remove dehydration
Organic faciess after dehydration are carried out concentrating under reduced pressure by agent, and concentrating under reduced pressure vacuum is -0.093Mpa, and chuck circulating water temperature is 65
DEG C, material temperature is 30 DEG C, and gibberellins product is obtained after crystallizing and drying, and product yield is 85%.
Embodiment 6.
Gibberellins mother solution 1000ml is taken, the sodium carbonate liquor 3000ml of strippant 1.2% is added, after stirring, is added
Its pH is adjusted to 5.8, after back extraction is separated by 30%NaOH solution, and water is added 2.5 ‰ Lactose enzymes and carries out pretreatment, digests after vulcanization
Acid solution is adjusted after pH to 2.1, and by volume 1.0：1.2 addition ethyl acetate are extracted, and the organic faciess addition after extraction is de-
Water preparation anhydrous calcium chloride removes moisture, is filtered to remove dehydrant, and the organic faciess after dehydration are carried out into concentrating under reduced pressure, and concentrating under reduced pressure is true
Reciprocal of duty cycle is -0.092Mpa, and chuck circulating water temperature is 68 DEG C, and material temperature is 35 DEG C, and gibberellins product, product are obtained after crystallizing and drying
Yield is 88%.
Embodiment 7.
Gibberellins mother solution 1000ml is taken, the sodium bicarbonate solution 4000ml of strippant 1.0% is added, after stirring, is added
Its pH is adjusted to 5.45, after back extraction is separated by 30%NaOH solution, and water is added 3 ‰ saccharifying enzyme and carries out pretreatment, enzymolysis after vulcanization acid
Solution is adjusted after pH to 2.7, and by volume 1.0：0.9 addition butyl acetate is extracted, the organic faciess addition dehydrant after extraction
Anhydrous magnesium sulfate removes moisture, is filtered to remove dehydrant, and the organic faciess after dehydration are carried out into concentrating under reduced pressure, concentrating under reduced pressure vacuum
For -0.09Mpa, chuck circulating water temperature is 65 DEG C, and material temperature is 30 DEG C, and gibberellins product, product yield are obtained after crystallizing and drying
For 87%.
Embodiment 8.
Gibberellins mother solution 1000ml is taken, the sodium bicarbonate solution 4000ml of strippant 1.2% is added, after stirring, is added
Its pH is adjusted to 5.5, after back extraction is separated by 30%NaOH solution, and water is added 2.5 ‰ amylase and saccharifying enzyme and carries out pretreatment, enzyme
Solution after vulcanization acid solution is adjusted after pH to 2.5, and by volume 1.0：1.0 addition ethyl acetate are extracted, the organic faciess after extraction
Addition dehydrant anhydrous sodium sulfate removes moisture, is filtered to remove dehydrant, and the organic faciess after dehydration are carried out into concentrating under reduced pressure, reduces pressure
Concentration vacuum is -0.09Mpa, and chuck circulating water temperature is 67 DEG C, and material temperature is 33 DEG C, and gibberellins product is obtained after crystallizing and drying
Product, product yield is 90%.
Embodiment 9.
Gibberellins mother solution 1000ml is taken, the disodium hydrogen phosphate of strippant 2.0% and sodium dihydrogen phosphate is added（Volume ratio 2:1）
Buffer solution 3000ml, after stirring, adds 30%NaOH solution that its pH is adjusted to into 6.3, after back extraction is separated, and water is added sulfur
Acid solution is adjusted after pH to 3.0, and by volume 1.0：0.9 addition ethyl acetate is extracted, the organic faciess addition dehydration after extraction
Agent anhydrous calcium chloride removes moisture, is filtered to remove dehydrant, and the organic faciess after dehydration are carried out into concentrating under reduced pressure, concentrating under reduced pressure vacuum
Spend for -0.08Mpa, chuck circulating water temperature is 68 DEG C, and material temperature is 35 DEG C, gibberellins product is obtained after crystallizing and drying, product is received
Rate is 85%.
Embodiment 10.
Gibberellins mother solution 1000ml is taken, the sodium carbonate liquor 4000ml of strippant 1.8% is added, after stirring, is added
Its pH is adjusted to 6.5 by 30%KOH solution, and after back extraction is separated, water is added sulfuric acid solution and adjusts after pH to 2.5, and by volume 1.0：
0.9 addition butyl acetate is extracted, and the organic faciess addition dehydrant anhydrous magnesium sulfate after extraction removes moisture, is filtered to remove de-
Organic faciess after dehydration are carried out concentrating under reduced pressure by water preparation, and concentrating under reduced pressure vacuum is -0.09Mpa, and chuck circulating water temperature is 65
DEG C, material temperature is 30 DEG C, and gibberellins product is obtained after crystallizing and drying, and product yield is 84%.
Embodiment 11.
Gibberellins mother solution 1000ml is taken, the sodium bicarbonate solution 2000ml of strippant 3.0% is added, after stirring, is added
Its pH is adjusted to 5.0 by 20% ammonia, and after back extraction is separated, water is added sulfuric acid solution and adjusts after pH to 3.5, and by volume 1.0： 0.7
Butyl acetate is added to be extracted, the organic faciess addition dehydrant anhydrous magnesium sulfate after extraction removes moisture, is filtered to remove dehydration
Organic faciess after dehydration are carried out concentrating under reduced pressure by agent, and concentrating under reduced pressure vacuum is -0.09Mpa, and chuck circulating water temperature is 65
DEG C, material temperature is 30 DEG C, and gibberellins product is obtained after crystallizing and drying, and product yield is 80%.In view of this technique by anti-for the first time
Its product yield is low after extraction, extraction, condensing crystallizing, and only 80%, thus the organic faciess after separating to back extraction carry out second
Secondary back extraction-extraction-condensing crystallizing process, operating procedure repeats the above method, and gibberellins total yield of products is reachable
90%。
Claims (8)
1. a kind of method that gibberellins mother solution is recrystallized, it is characterised in that comprise the steps of successively：
（1）Back extraction：Gibberellins mother solution by volume 1：2 ~ 5 add strippants, after stirring, add alkaline solution by its
PH value is adjusted to 4.8 ~ 6.5, makes the gibberellins in crystalline mother solution enter water phase, isolated water phase, to the water phase by back extraction
Addition enzyme material carries out pretreatment；Described enzyme material is selected from one or more of saccharifying enzyme, amylase, Lactose enzyme；
（2）Extraction：Add acid solution toward the water phase containing gibberellins, after adjusting pH to 1.5 ~ 3.5, by volume 1.0：
0.7 ~ 1.2 addition organosilane ester extractant is extracted, and makes the gibberellins in water phase extract back organic ester phase, separates to obtain organic ester
Phase；
（3）Dehydration：Add dehydrant toward the organic ester phase after extraction, remove moisture；
（4）Condensing crystallizing：Dehydrant is filtered to remove, the organic ester after dehydration is mutually carried out concentrating under reduced pressure, obtained after crystallizing and drying
Gibberellins product.
2. the method that a kind of gibberellins mother solution according to claim 1 is recrystallized, it is characterised in that：Step（1）Described
Strippant is carbonate solution or phosphate solution.
3. the method that a kind of gibberellins mother solution according to claim 2 is recrystallized, it is characterised in that：Step（1）Described
Strippant is 0.8 ~ 3.0% sodium bicarbonate solution, 0.8 ~ 3.0% sodium carbonate liquor, 0.8 ~ 3.0% diammonium phosphate and di(2-ethylhexyl)phosphate
One or more of the buffer solution of hydrogen ammonium, 0.8 ~ 3.0% disodium hydrogen phosphate and sodium dihydrogen phosphate composition.
4. the method that a kind of gibberellins mother solution according to claim 1 is recrystallized, it is characterised in that：Step（2）Described
Organosilane ester extractant is selected from one or more for ethyl ester class, butyl ester class, isoamyl esters.
5. the method that a kind of gibberellins mother solution according to claim 1 is recrystallized, it is characterised in that：Step（3）Described
Dehydrant is selected from one or more for anhydrous calcium chloride, anhydrous sodium sulfate, anhydrous magnesium sulfate.
6. the method that any one the gibberellins mother solution according to claim 1 ~ 5 is recrystallized, it is characterised in that：Step（1）Institute
The alkaline solution stated is selected from one or more for NaOH solution, KOH solution, ammonia spirit；Step（2）Described acid solution
Selected from for sulfuric acid solution, hydrochloric acid solution, phosphoric acid solution one or more.
7. the method that any one the gibberellins mother solution according to claim 1 ~ 5 is recrystallized, it is characterised in that：Step（2）Institute
The pH value stated, is adjusted to 2.0 ~ 3.0.
8. the method that any one the gibberellins mother solution according to claim 1 ~ 5 is recrystallized, it is characterised in that：Described step
（4）Described in concentrating under reduced pressure, its vacuum is -0.08 ~ -0.095Mpa, and chuck circulating water temperature is 65 ~ 75 DEG C, and material temperature is
30~40℃。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410761337.4A CN104672190B (en) | 2014-12-12 | 2014-12-12 | Method for recrystallizing gibberellin mother liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410761337.4A CN104672190B (en) | 2014-12-12 | 2014-12-12 | Method for recrystallizing gibberellin mother liquor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104672190A CN104672190A (en) | 2015-06-03 |
| CN104672190B true CN104672190B (en) | 2017-04-19 |
Family
ID=53307832
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410761337.4A Active CN104672190B (en) | 2014-12-12 | 2014-12-12 | Method for recrystallizing gibberellin mother liquor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104672190B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108184846A (en) * | 2018-01-18 | 2018-06-22 | 四川龙蟒福生科技有限责任公司 | A kind of gibberellic acid missible oil and preparation method thereof |
Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB819110A (en) * | 1957-07-02 | 1959-08-26 | Pfizer & Co C | Recovery process for gibberellins |
| GB821733A (en) * | 1957-04-05 | 1959-10-14 | Ici Ltd | Isolation process |
| US2980700A (en) * | 1958-01-21 | 1961-04-18 | Lilly Co Eli | Process of gibberellic acid purification |
| US3057878A (en) * | 1959-03-09 | 1962-10-09 | Abbott Lab | Process for making crystalline potassium salt of gibberellic acid |
| US3118909A (en) * | 1960-11-17 | 1964-01-21 | Applic Biochimique Soc Et | Purification of gibberellins |
| US3496194A (en) * | 1966-11-03 | 1970-02-17 | Ici Ltd | Process for the separation of gibberellins |
| ES8106555A1 (en) * | 1979-09-27 | 1981-08-16 | Inst Chemii Przemyslowej | Procedure to insulate giberelines of the liquor of stimulated crystalization of ethyl acetate. (Machine-translation by Google Translate, not legally binding) |
| CN1063309A (en) * | 1991-01-11 | 1992-08-05 | 北京清华大学 | The solvent extraction method concentration process of gibberellin fermented filtrate |
| CN1111286A (en) * | 1995-03-16 | 1995-11-08 | 北京农业大学 | Method for stage extraction gibberellin A4 and A7 from gibberellin mixture |
| CN1222575A (en) * | 1998-01-05 | 1999-07-14 | 中生北方生物工程开发研究所 | Gibberela fujikuroi strain used for industrial fermentation production of gibberellin A4 and A7 |
| CN101134751A (en) * | 2007-03-12 | 2008-03-05 | 江苏丰源生物化工有限公司 | Method for extracting gibberellic acid GA4+7 from gibberellic acid fermentation liquor |
| CN101421400A (en) * | 2003-03-06 | 2009-04-29 | 戴弗萨公司 | Amylases, nucleic acids encoding them and methods for making and using them |
| CN101849018A (en) * | 2007-08-22 | 2010-09-29 | 纳幕尔杜邦公司 | Process for concentrated biomass saccharification |
| CN102942547A (en) * | 2012-11-16 | 2013-02-27 | 南京工业大学 | Separation and purification method of GA4 (gibberellin A4) and/or GA7 (gibberellin A7) |
| CN103764836A (en) * | 2011-08-12 | 2014-04-30 | 诺维信公司 | Reduction of culture viscosity by manganese addition |
-
2014
- 2014-12-12 CN CN201410761337.4A patent/CN104672190B/en active Active
Patent Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB821733A (en) * | 1957-04-05 | 1959-10-14 | Ici Ltd | Isolation process |
| GB819110A (en) * | 1957-07-02 | 1959-08-26 | Pfizer & Co C | Recovery process for gibberellins |
| US2980700A (en) * | 1958-01-21 | 1961-04-18 | Lilly Co Eli | Process of gibberellic acid purification |
| US3057878A (en) * | 1959-03-09 | 1962-10-09 | Abbott Lab | Process for making crystalline potassium salt of gibberellic acid |
| US3118909A (en) * | 1960-11-17 | 1964-01-21 | Applic Biochimique Soc Et | Purification of gibberellins |
| US3496194A (en) * | 1966-11-03 | 1970-02-17 | Ici Ltd | Process for the separation of gibberellins |
| ES8106555A1 (en) * | 1979-09-27 | 1981-08-16 | Inst Chemii Przemyslowej | Procedure to insulate giberelines of the liquor of stimulated crystalization of ethyl acetate. (Machine-translation by Google Translate, not legally binding) |
| CN1063309A (en) * | 1991-01-11 | 1992-08-05 | 北京清华大学 | The solvent extraction method concentration process of gibberellin fermented filtrate |
| CN1111286A (en) * | 1995-03-16 | 1995-11-08 | 北京农业大学 | Method for stage extraction gibberellin A4 and A7 from gibberellin mixture |
| CN1222575A (en) * | 1998-01-05 | 1999-07-14 | 中生北方生物工程开发研究所 | Gibberela fujikuroi strain used for industrial fermentation production of gibberellin A4 and A7 |
| CN101421400A (en) * | 2003-03-06 | 2009-04-29 | 戴弗萨公司 | Amylases, nucleic acids encoding them and methods for making and using them |
| CN101134751A (en) * | 2007-03-12 | 2008-03-05 | 江苏丰源生物化工有限公司 | Method for extracting gibberellic acid GA4+7 from gibberellic acid fermentation liquor |
| CN101849018A (en) * | 2007-08-22 | 2010-09-29 | 纳幕尔杜邦公司 | Process for concentrated biomass saccharification |
| CN103764836A (en) * | 2011-08-12 | 2014-04-30 | 诺维信公司 | Reduction of culture viscosity by manganese addition |
| CN102942547A (en) * | 2012-11-16 | 2013-02-27 | 南京工业大学 | Separation and purification method of GA4 (gibberellin A4) and/or GA7 (gibberellin A7) |
Non-Patent Citations (2)
| Title |
|---|
| 关于赤霉素生产的一些技术问题;黄元康;《植物生理学通讯》;19650630(第6期);第16-39页 * |
| 酶在制糖工业中的应用;惇一小原 等;《甜菜糖业》;19801231(第5期);第42-50页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104672190A (en) | 2015-06-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP4151645A3 (en) | Separation of 2'-fl from a fermentation broth | |
| CN104473120A (en) | Monosodium glutamate production technology | |
| CN107207552B (en) | Crystal of N-acetylneuraminic acid ammonium salt anhydride and process for producing the same | |
| CN103950899B (en) | A kind of preparation method of calcium peroxide | |
| CN104910178B (en) | A kind of preparation method of Piperacillin acid | |
| CN104387355A (en) | Ethyl maltol crystallization mother liquor recovery method | |
| CN104672190B (en) | Method for recrystallizing gibberellin mother liquor | |
| US20140303406A1 (en) | Process for Preparing Xanthophyll Crystal | |
| CN102875404B (en) | Production method and application of lysine hydrochloride crystals | |
| CN106883274A (en) | Sialic acid process for purification | |
| CN104291288B (en) | Method for preparing monoammonium phosphate and co-producing special compound fertilizer for potatoes | |
| CN106430282B (en) | A kind of preparation method of basic copper sulfate | |
| CN105152930A (en) | Preparation method and application of sodium stearyl lactate | |
| CN103351412A (en) | Method for improving yield of crystalline xylose by virtue of biological treatment | |
| CN103819352B (en) | Valine continuous crystallization method | |
| CN103922532A (en) | Imidazolidine tail liquid treatment technology | |
| CN103014077B (en) | A kind of novel process of production of Propionic Acid by Fermentation Process calcium | |
| CN105503680A (en) | Method for improving flour extraction rate of monosultap centrifugal mother liquor | |
| CN104212869A (en) | Method for producing ultra-low moisture threonine | |
| CN110894170A (en) | Ammonium bicarbonate mixed crystal and preparation method thereof | |
| CN102382000A (en) | Production method of D- para hydroxybenzene glycine | |
| CN104291299B (en) | A kind of method preparing sodium dihydrogen phosphate coproduction cowpea composite fertilizer special | |
| CN108047288A (en) | A kind of preparation method of Gardenoside | |
| WO2018094757A1 (en) | Method for preparing anhydrous trisodium citrate | |
| CN103708501B (en) | A kind of method that membrane crystallization refines the thick sulphur ammonium of coking |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: Ji'an City Chengnan Industrial Zone 331399 Jiangxi Xingan Patentee after: Jiangxi new Ruifeng biochemical Limited by Share Ltd Address before: Ji'an City Chengnan Industrial Zone 331399 Jiangxi Xingan Patentee before: Jiangxi Xinruifeng Biochemical Co., Ltd. |
|
| CP01 | Change in the name or title of a patent holder |