CN1055738A - Gibberellin extraction process - Google Patents
Gibberellin extraction process Download PDFInfo
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- CN1055738A CN1055738A CN 90102217 CN90102217A CN1055738A CN 1055738 A CN1055738 A CN 1055738A CN 90102217 CN90102217 CN 90102217 CN 90102217 A CN90102217 A CN 90102217A CN 1055738 A CN1055738 A CN 1055738A
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- gibberellins
- extraction
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- plant hormones
- hormones regulators
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Abstract
The invention discloses a kind of Plant hormones regulators,gibberellins GA that from the solid fermentation substratum, extracts
3Method, it comprises the system dry medium, water is that medium is multistage continuously, adverse current, pressure, circulation extracting dry medium, resin absorption, desorb, steps such as extraction, charcoal take off, condensing crystal, processing method advantages of simple, reduced investment.Compare with existing solvent refinement method, product cost has reduced by 30%, refines yield and has improved 10%, and finished product is tired and improved 50r/mg, and the finished product color and luster is good, can reach the outgoing quality standard.In addition, energy consumption of the present invention and three wastes discharge amount are also much lower than prior art.
Description
The present invention relates to a kind of process for extracting of Plant hormones regulators,gibberellins, be specially adapted to from solid medium, refine Plant hormones regulators,gibberellins A
3(be called for short GA
3) production technique.
Plant hormones regulators,gibberellins (Gibberellin) claims " GA " again, and it is the meta-bolites of gibberella (Gibberella fujkuroi).Plant hormones regulators,gibberellins is a kind of plant growth hormones efficiently, along with science and technology development, has been widely used in agricultural, livestock industry, makeup industry, foodstuffs industry and pharmaceutical industries at present, and the world market sale price is very high, is a kind of very vital product.It is reported, known that the homologue of Plant hormones regulators,gibberellins has tens of kinds more than at present, wherein with GA
3(structural formula is
) biological activity best, the product of fermentation mainly also is with GA
3Be main mixture, what gibberellin extraction technology of the present invention referred to is exactly GA from solid medium
3Active ingredient is separated, concentrated, purge process.
Present most producer adopts the solvent extraction method, and its technological process of production as shown in Figure 1.The solvent extraction method is only applicable to the submerged fermentation culture method as suitability for industrialized production, and this technology unavoidably to exist investment big, the construction period is long, yield poorly, the cost height, consumption grain is big, power consumption is big, and three wastes treatment capacity is big, and low grade of economic and technical norms can't overcome the deficiency.With China's present circumstances, a newly-built year six tons Plant hormones regulators,gibberellins factory, need investment more than 2,000 ten thousand yuan, the construction period is taken 2 years.Need consume electricity 1666.7 ten thousand degree, 8380 tons in water, 3135.5 tons of steam by one ton of Plant hormones regulators,gibberellins of the every production of this method, 523.17 tons in coal, 82.42 tons in grain, 197.55 tons of cash crop such as peanut, soya beans etc., about 1800 yuan/kg of factory cost, and sale price 2500 yuan/kg only.9 days submerged fermentation cycles, fermentation unit 1200-1600r/ml refines yield 70%, and it is the unit of expression microbial metabolites biological activity power that finished product tires that 850r/mg(tires), do not reach export standard 900r/mg, a year waste discharge amount reaches 1248 tons of/ton products.And up to now, the solvent method is used for the refinement of solid fermentation culture method and did not meet report as yet.In view of the foregoing, situation that Plant hormones regulators,gibberellins market occurs that supply falls short of demand, also because of in this, the improvement of the refining technique of Plant hormones regulators,gibberellins has caused each producer's common concern.
Task of the present invention is to provide a kind of can overcome the insufficient gibberellin extraction process of above-mentioned prior art, and this production technique can not only be used for submerged fermentation, and can directly extract GA from the solid fermentation substratum
3, method is simple, and reduced investment greatly reduces production cost, has improved quality product.
According to the task that the present invention provides, the contriver is according to the physicochemical property of Plant hormones regulators,gibberellins:
1, GA
3Contain carboxyl, hydroxyl isopolarity group in the molecular structure, different solubility in the aqueous solution of different PH scopes changes with PH at water and the ester partition ratio in mutually.
2, the molecular weight of Plant hormones regulators,gibberellins is 346, therefore can select for use macroporous resin absorption with GA according to molecular size
3Be main Plant hormones regulators,gibberellins.
3, Plant hormones regulators,gibberellins is heat-sensitive substance, so the entire operation process should be carried out at low temperatures.And technological advantages such as comprehensive counter-flow water extracting, resin absorption, solvent extraction, a kind of Plant hormones regulators,gibberellins dry medium extraction process is disclosed, this processing method comprises:
1, solid medium (wet bent) is made particle, airing becomes dry medium.
2, adopt multistage continuously, adverse current, pressure, round-robin water extracting dry medium, dry medium and extract volume ratio are 1: 5～20, and are strict controlled under the low temperature and carry out.
3, behind the suspended impurity in the filtering extract, utilizing the active principle in the macroporous resin enrichment extract, is that strippant carries out desorb with organic solvent as 50～90% acetone or 60～95% aqueous ethanolic solution again.
4, stripping liquid repeatedly extracts with the lower acetate kind solvent that is slightly soluble in water after concentrating under reduced pressure reclaims strippant, and extraction liquid adds an amount of charcoal absorption impurity, filtration, concentrating under reduced pressure, crystallisation by cooling, filtration, vacuum-drying, promptly makes to contain GA
3Xln more than 90%.
When refining method of the present invention was used for the submerged fermentation culture method and refines, as long as save system dry medium and multistage water extraction steps, all the other steps were identical.
Compared with prior art, the present invention has following advantage:
1, reduced investment of the present invention, the construction period is short, builds up a Plant hormones regulators,gibberellins factory that produces 2000kg per year and only need invest 1,000,000 yuan, three months construction periods.
2, cost is low, and per kilogram Plant hormones regulators,gibberellins factory cost reduces by 30% than existing solvent method.
3, economic and technical norms height, the present invention refines yield and reaches more than 80%, and is higher by 10% than solvent method, finished product of the present invention is tired and is reached more than the 900r/mg, than the high 50r/mg of solvent method, the finished product color and luster is good, and grain consumption of the present invention, energy consumption and three wastes discharge amount are all much lower than existing technology.
Further describe the present invention below in conjunction with concrete production technique and embodiment.
The process flow diagram that solvent refinement method is produced is cultivated in Fig. 1, Plant hormones regulators,gibberellins submerged fermentation
Fig. 2, the present invention refine technological process of production block diagram (in the frame of broken lines be used for use on the submerged fermentation culture method processing step)
The processing step of embodiment following (with reference to Fig. 2)
One, the pre-treatment of raw material-system dry medium
Get wet song and tire, admix proper amount of gypsum (CaSO to the Plant hormones regulators,gibberellins solid medium 1000g more than the 5000r/g
4) mixing, make particle, granular size is advisable with φ 5～10mm, airing under the room temperature, it is standby promptly to make dry medium (tiring more than the 8000r/g).
Two, multi-stage countercurrent extracts:
The above-mentioned dry medium 80g that respectively packs in the glass column of four φ 35 * 270mm respectively gets 10 times of water-cooleds to 0 to dry medium～5 ℃ simultaneously, regulates PH2.0～6.0(3N H
2SO
4), with micropump respectively the dry medium in above-mentioned four glass columns do pressure, adverse current, recirculated water extracting, making in the post Plant hormones regulators,gibberellins tire to be step by step successively decreases, and the Plant hormones regulators,gibberellins in four groups of extracts is tired to be and is increased progressively step by step, along with the low song of tiring constantly withdraws from, and new bently constantly add, extract is tired and is constantly risen, standby to the discharging of tiring when reaching 1600r/ml of fourth stage extract, material liquid volume 800ml replenishes fresh water liquid and continues to reflux from the first step.According to this law, extraction efficiency can reach 94.33%, and the extracting yield reaches 85%.
Three, resin absorption, acetone desorb
1, absorption: above-mentioned extract is filtered through B, get clear filtrate, clear filtrate is passed through the SIP-1300 resin with the speed of 3ml/min, when the effluent discharge of resin absorption is tired greater than 200r/ml, shut-down operation washes resin with water, removes water-soluble impurity.
2, desorb: carry out desorb through washing clean saturated resin with 90% acetone, flow velocity 1ml/min, tiring when stripping liquid begins to collect when being higher than 500r/ml, and tiring when stripping liquid stops to collect when being lower than 500r/ml, collects stripping liquid 120ml.Tire according to this law operation peak desorb and to reach 56000r/ml.Absorption, separate specific absorption and reach 90%.
Four, stepwise solvent extraction, charcoal take off
Above-mentioned stripping liquid reclaims solvent (acetone) with rotary film evaporator, and more than the control vacuum tightness 650mmHg, 60～80 ℃ of bath temperatures are concentrated into original volume about 1/3rd, concentrated solution 3NH
2SO
4Solution regulate use behind pH to 1.5～3.0 divide with the isopyknic butylacetate of concentrated solution extract for five times, when the shut-down operation when being lower than 500r/ml of tiring of aqueous phase Plant hormones regulators,gibberellins, merge the ester phase, the gac of adding 0.5～1.0% decoloured 5～10 minutes, put into the refrigerator-freezer lyophilization, filter, must clarify light yellow filtrate.This step operational yield reaches 95%.
Five, finished product crystallization, drying
To go up step filtrate and reclaim solvent with rotary film evaporator, more than the control vacuum tightness 700mmHg, 80～90 ℃ of bath temperatures, being concentrated into partial crystallization separates out, be chilled to room temperature,, filter in refrigerator and cooled but 2～4 hours, crystallization is washed with amount of ethyl acetate, drain 50～60 ℃ of control loft drier temperature, the above vacuum-drying of vacuum tightness 700mmHg 4 hours, get crystallization 0.67g, 915r/mg tires.The crystalline mother solution preparation emulsion 10.4ml(40000r/ml that tires).
Total recovery reaches 80.39%(in extract total hundred million in the present embodiment), the yield height, quality is good, and method is simple and reliable, and Technology advanced person is the desirable process for extracting that the solid fermentation culture method is produced Plant hormones regulators,gibberellins.
Claims (6)
1, a kind of refinement Plant hormones regulators,gibberellins particularly extracts Plant hormones regulators,gibberellins GA from the solid fermentation substratum
3Novel process, it is characterized in that the technical process of this processing method is: raw material (wet bent) → particulate state dry medium → multistage water extracting → filtrations → macroporous resin absorption → desorb → concentrated → repeatedly extraction → charcoal takes off freezing and filtering → concentrating under reduced pressure → freezing → filtration washing → vacuum-drying → finished product.
2, technology according to claim 1 is characterized in that particulate state dry medium water content is 10-20%, tires 〉=8000r/g.
3, technology according to claim 1, it is characterized in that multistage water extract be adopt continuously, adverse current, pressure, round-robin level Four extraction process, the pH value of extract is 2.0-6.0.
4, technology according to claim 1 is characterized in that stripping liquid adopts the aqueous solution of acetone or alcohol.
5, technology according to claim 1 is characterized in that extraction agent adopts the lower acetate that is slightly soluble in water.
6, technology according to claim 1 is characterized in that the method for regulating pH value realizes that the extraction charcoal takes off, concentration and crystallization process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90102217 CN1055738A (en) | 1990-04-16 | 1990-04-16 | Gibberellin extraction process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90102217 CN1055738A (en) | 1990-04-16 | 1990-04-16 | Gibberellin extraction process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1055738A true CN1055738A (en) | 1991-10-30 |
Family
ID=4877426
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90102217 Pending CN1055738A (en) | 1990-04-16 | 1990-04-16 | Gibberellin extraction process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1300131C (en) * | 2005-04-27 | 2007-02-14 | 浙江钱江生物化学股份有限公司 | Separation method for purifying gibberellin GA3 |
| CN100447147C (en) * | 2006-12-20 | 2008-12-31 | 福州大学 | Aminoglycoside antibiotics enriching and purifying macroporous resin process |
| CN102241653A (en) * | 2011-07-08 | 2011-11-16 | 江西新瑞丰生化有限公司 | Membrane filtration and concentration technology of gibberellin |
| WO2017091956A1 (en) * | 2015-11-30 | 2017-06-08 | 南京工业大学 | Process for separating and purifying gibberellin ga3 by using magnetic resin |
| CN111499703A (en) * | 2020-05-07 | 2020-08-07 | 浙江新银象生物工程有限公司 | Extraction method of high-yield nisin |
-
1990
- 1990-04-16 CN CN 90102217 patent/CN1055738A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1300131C (en) * | 2005-04-27 | 2007-02-14 | 浙江钱江生物化学股份有限公司 | Separation method for purifying gibberellin GA3 |
| CN100447147C (en) * | 2006-12-20 | 2008-12-31 | 福州大学 | Aminoglycoside antibiotics enriching and purifying macroporous resin process |
| CN102241653A (en) * | 2011-07-08 | 2011-11-16 | 江西新瑞丰生化有限公司 | Membrane filtration and concentration technology of gibberellin |
| WO2017091956A1 (en) * | 2015-11-30 | 2017-06-08 | 南京工业大学 | Process for separating and purifying gibberellin ga3 by using magnetic resin |
| GB2552593A (en) * | 2015-11-30 | 2018-01-31 | Nanjing University Of Technology | Process for separating and purifying gibberellin GA3 by using magnetic resin |
| GB2552593B (en) * | 2015-11-30 | 2020-04-15 | Nanjing University Of Technology | Process for separation and purification of gibberellin GA3 using magnetic resin |
| CN111499703A (en) * | 2020-05-07 | 2020-08-07 | 浙江新银象生物工程有限公司 | Extraction method of high-yield nisin |
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