CN106977442A - A kind of extraction process of hydroxyproline - Google Patents
A kind of extraction process of hydroxyproline Download PDFInfo
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- CN106977442A CN106977442A CN201710290318.1A CN201710290318A CN106977442A CN 106977442 A CN106977442 A CN 106977442A CN 201710290318 A CN201710290318 A CN 201710290318A CN 106977442 A CN106977442 A CN 106977442A
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- China
- Prior art keywords
- hydroxyproline
- exchange resin
- efflux
- extraction process
- anion exchange
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/04—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
- C07D207/10—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/16—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention provides a kind of extraction process of hydroxyproline, thalline is removed by the way that hydroxyproline zymotic fluid is crossed into ceramic membrane, then filtrate pH is adjusted to less than 6.5, anion exchange resin is crossed, the pH of efflux is adjusted to more than 6.5, crosses cationic ion-exchange resin, after efflux is evaporated to dryness under reduced pressure, washed out with absolute ethyl alcohol, supersonic oscillations 30min, hydroxyproline crystal is finally obtained by vacuum filtration again；Methods described needs not move through ultrafiltration and activated carbon decolorizing, can significantly reduce useless dirty intractability, while rotary evaporated to dryness is dry, reduce the residual quantity of hydroxyproline in mother liquor so that product yield is high, purity is high, steady quality.
Description
Technical field
The present invention relates to technical field of biochemical industry, especially a kind of extraction process of hydroxyproline.
Background technology
Hydroxyproline is the main constituents of collagen, and it is widely used in medicine, chemical industry, animal feed and beauty
In terms of.The method of production hydroxyproline mainly has chemical synthesis, biological extraction method and microbe fermentation method.Chemical synthesis
Cost is high, is not suitable for industrialized production.Current domestic production hydroxyproline main method is biological extraction method, but is utilized
Biological extraction method directly extracts hydroxyproline from gelatin, collagen, pigskin, and all kinds of corrupt practices creep in, the step of not only producing and purify
Many, low yield, raw material availability are low, and need to add substantial amounts of chemical reagent in process of production, and environmental pollution is big, and waste water gives up
Slag is difficult.Using Production by Microorganism Fermentation hydroxyproline, cost of material can be not only reduced, production efficiency, Er Qieyong is improved
Renewable resource replaces the non-renewable resources such as chemical, reduces the pollution to environment.Therefore, given birth to using microbe fermentation method
Produce hydroxyproline significant.
At present, hydroxyproline extraction process is that zymotic fluid is obtained after filtrate by micro-filtration and ultrafiltration in zymotic fluid, crosses ion
Exchanger resin, is afforded after the filtrate containing hydroxyproline, adds 0.5% activated carbon decolorizing, then by being filtered by vacuum and must filter
Liquid, by the 1/7-1/8 of filtrate rotary evaporation concentration volume to stoste, vacuum filtration obtains hydroxyproline crystal.Due to this method
Activated carbon is needed to use to carry out decolorization, in industrialized production, substantial amounts of activated carbon can cause useless dirty intractability, pollution
Environment；In rotary evaporation, remaining a small amount of liquid can make part hydroxyproline dissolving wherein, cause product yield relatively low.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of extraction process of hydroxyproline.
In order to solve the above technical problems, the technical scheme is that：
A kind of extraction process of hydroxyproline, is comprised the following steps that：
(1) hydroxyproline zymotic fluid (normal fermentation liquid) is crossed into ceramic membrane removing thalline and obtains filtrate；
(2) filtrate pH is adjusted to 5.5-6.0 with hydrochloric acid solution, crosses anion exchange resin and collect first time efflux；
(3) first time efflux pH is adjusted to 7.0-7.5 with ammoniacal liquor, crosses cationic ion-exchange resin, collected second and flow out
Liquid；
(4) it is second of efflux rotary evaporated to dryness is dry, washed out with absolute ethyl alcohol, supersonic oscillations 30min；
(5) vacuum filtration obtains hydroxyproline crystal.
It is preferred that, the extraction process of above-mentioned hydroxyproline, the anion exchange resin is to be made the transition by hydrochloric acid or sulfuric acid
For chlorine type weak anion exchange resin or sulfate radical type anion exchange resin.
It is preferred that, the extraction process of above-mentioned hydroxyproline, the cationic ion-exchange resin is to pass through NaCl solution or ammoniacal liquor
It is transformed into sodium form weak cation exchange resin or ammonium ion type cationic ion-exchange resin.
Structure of the present invention has the advantages that：
The extraction process of above-mentioned hydroxyproline, compared with traditional handicraft, it is not necessary to pass through ultrafiltration and activated carbon decolorizing, can show
The useless dirty intractability of reduction is write, useless dirty processing load is alleviated, while rotary evaporated to dryness is dry, reduces hydroxyproline in mother liquor
Residual quantity so that product yield is high, purity is high, steady quality is reliable；Whole technical process is simple to operate, and cost is relatively low, and ten
Divide and be applied to industrialized production.
Embodiment
To further illustrate the present invention, now by the way that example is embodied, the present invention will be described in detail.
A kind of hydroxyproline novel technology for extracting, comprises the following steps：
Take hydroxyproline zymotic fluid (being 37.7g/L containing hydroxyproline) to cross ceramic membrane removing thalline and obtain filtrate, by filtrate pH
5.5-6.0 is adjusted to, weak anion exchange resin SQD817 (filtrate for crossing 30 times of bed volumes) is crossed, except depigmentaton and albumen, obtains
Hydroxyproline efflux, 7.0-7.5 is adjusted to by efflux pH, is crossed weak cation exchange resin D152 and (is crossed the filter of 100 times of bed volumes
Liquid), pigment and albumen are carried out it is secondary remove, efflux is concentrated by evaporation to drying using Rotary Evaporators at 75 DEG C or so, so
Washed out afterwards with absolute ethyl alcohol, supersonic oscillations 30min washes away residual pigment, it is brilliant to obtain hydroxyproline finally by vacuum filtration
Body.Calculating is obtained, from rotary evaporation to a step yield of hydroxyproline product is obtained up to 92%, with former technique (from rotary evaporation
To a step yield of hydroxyproline product is obtained 70%) to compare, 31.4% is improved.Product purity is up to 99.6%.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (3)
1. a kind of extraction process of hydroxyproline, it is characterised in that：Comprise the following steps that：
(1) hydroxyproline zymotic fluid is crossed into ceramic membrane removing thalline and obtains filtrate；
(2) filtrate pH is adjusted to 5.5-6.0, crosses anion exchange resin, collect first time efflux；
(3) first time efflux pH is adjusted to 7.0-7.5, crosses cationic ion-exchange resin, collects second of efflux；
(4) it is second of efflux rotary evaporated to dryness is dry, washed out with absolute ethyl alcohol, supersonic oscillations 30min；
(5) vacuum filtration obtains hydroxyproline crystal.
2. the extraction process of hydroxyproline according to claim 1, it is characterised in that：The anion exchange resin is logical
Persalt or sulfuric acid are transformed into chlorine type weak anion exchange resin or sulfate radical type anion exchange resin.
3. the extraction process of hydroxyproline according to claim 1, it is characterised in that：The cationic ion-exchange resin is warp
Cross NaCl solution or ammoniacal liquor is transformed into sodium form weak cation exchange resin or ammonium ion type cationic ion-exchange resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710290318.1A CN106977442A (en) | 2017-04-28 | 2017-04-28 | A kind of extraction process of hydroxyproline |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710290318.1A CN106977442A (en) | 2017-04-28 | 2017-04-28 | A kind of extraction process of hydroxyproline |
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| Publication Number | Publication Date |
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| CN106977442A true CN106977442A (en) | 2017-07-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201710290318.1A Pending CN106977442A (en) | 2017-04-28 | 2017-04-28 | A kind of extraction process of hydroxyproline |
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| CN (1) | CN106977442A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107513030A (en) * | 2017-10-19 | 2017-12-26 | 福建师范大学 | A kind of method that L hydroxyprolines are isolated and purified in the hydroxyproline zymotic fluid from L |
| WO2020113289A1 (en) * | 2018-12-07 | 2020-06-11 | Atp Institute Pty Ltd | Formulations comprising non-animal derived hydroxyproline and their use |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07289274A (en) * | 1994-04-26 | 1995-11-07 | Sankyo Co Ltd | Production of trans-4-hydroxy-l-proline |
| EP0547898B1 (en) * | 1991-12-17 | 1999-02-17 | Sankyo Company Limited | Microbial process for the production of trans-4-hydroxy-L-proline |
| CN105420303A (en) * | 2015-12-09 | 2016-03-23 | 浙江绿创生物科技有限公司 | Fermentation process for producing trans-4-hydroxyl-L-proline |
| CN105506019A (en) * | 2015-12-31 | 2016-04-20 | 天津市敬业精细化工有限公司 | Method for industrially producing L-hydroxyproline through fermentation method |
| CN105777603A (en) * | 2016-04-01 | 2016-07-20 | 天津市敬业精细化工有限公司 | Method for extracting L-hydroxyproline from L-hydroxyproline fermentation liquor |
| CN107827803A (en) * | 2017-11-28 | 2018-03-23 | 绍兴厚普生物科技有限责任公司 | A kind of method that L hydroxyprolines are extracted from zymotic fluid |
-
2017
- 2017-04-28 CN CN201710290318.1A patent/CN106977442A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0547898B1 (en) * | 1991-12-17 | 1999-02-17 | Sankyo Company Limited | Microbial process for the production of trans-4-hydroxy-L-proline |
| JPH07289274A (en) * | 1994-04-26 | 1995-11-07 | Sankyo Co Ltd | Production of trans-4-hydroxy-l-proline |
| CN105420303A (en) * | 2015-12-09 | 2016-03-23 | 浙江绿创生物科技有限公司 | Fermentation process for producing trans-4-hydroxyl-L-proline |
| CN105506019A (en) * | 2015-12-31 | 2016-04-20 | 天津市敬业精细化工有限公司 | Method for industrially producing L-hydroxyproline through fermentation method |
| CN105777603A (en) * | 2016-04-01 | 2016-07-20 | 天津市敬业精细化工有限公司 | Method for extracting L-hydroxyproline from L-hydroxyproline fermentation liquor |
| CN107827803A (en) * | 2017-11-28 | 2018-03-23 | 绍兴厚普生物科技有限责任公司 | A kind of method that L hydroxyprolines are extracted from zymotic fluid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107513030A (en) * | 2017-10-19 | 2017-12-26 | 福建师范大学 | A kind of method that L hydroxyprolines are isolated and purified in the hydroxyproline zymotic fluid from L |
| WO2020113289A1 (en) * | 2018-12-07 | 2020-06-11 | Atp Institute Pty Ltd | Formulations comprising non-animal derived hydroxyproline and their use |
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