CN105949111B - A kind of preparation process of high-purity high light transmission L-Trp - Google Patents
A kind of preparation process of high-purity high light transmission L-Trp Download PDFInfo
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- CN105949111B CN105949111B CN201610346788.0A CN201610346788A CN105949111B CN 105949111 B CN105949111 B CN 105949111B CN 201610346788 A CN201610346788 A CN 201610346788A CN 105949111 B CN105949111 B CN 105949111B
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- tryptophan
- isoelectric point
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
- C07D209/04—Indoles; Hydrogenated indoles
- C07D209/10—Indoles; Hydrogenated indoles with substituted hydrocarbon radicals attached to carbon atoms of the hetero ring
- C07D209/18—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D209/20—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals substituted additionally by nitrogen atoms, e.g. tryptophane
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Indole Compounds (AREA)
Abstract
The present invention relates to a kind of preparation process of high-purity high light transmission L tryptophans, the preparation process includes the following steps：（1）Dissolution filter：Crude product tryptophan is added in lysate and is dissolved, while adjusting pH value；Again after activated carbon adsorption, filtering；（2）Crystallization：By lysate, low temperature slowly crystallizes under stiring, and by vacuumizing and adjusting isoelectric point that it is made fully to dissolve；（3）Centrifugation：By crystal solution centrifugal filtration, white crystal is obtained；（4）It is dry：By white crystal through pure water, after washing, dry sterling tryptophan.The advantage of the invention is that：The preparation process of the high-purity high light transmission L tryptophans of the present invention, by adjusting pH value in dissolving step, increases the solubility of tryptophan crude product by the improvement to dissolving and crystallisation step；In crystallisation step, by vacuumizing and adjusting isoelectric point simultaneously so that the light transmittance and yield of tryptophan increase, and purity is more than 99.8%, and light transmittance is up to 97.2% 97.5%, and yield is up to 92% 94%.
Description
Technical field
The present invention relates to a kind of preparation method of amino acid, more particularly to a kind of preparation work of high-purity high light transmission L-Trp
Skill.
Background technology
L-Trp scientific name tryptophane, relative molecular weight 204.23.White or yellowish foliaceous
Crystallization or powder, it is odorless or micro- smelly, it is dissolved in hot pyridine, is slightly soluble in ethyl alcohol, insoluble in chloroform, ether.It is molten in diluted acid or diluted alkaline
Solution, long-time illumination then colour.Heat generates a small amount of indoles altogether with water, such as in NaOH or CuSO4In the presence of heat, then generate a large amount of
Indoles.It heats unstable, relatively stablizes in lye, but there are easily decomposed when other amino acid or carbohydrate in the dark with acid.
L-Trp is one of essential amino acid in human body and animal life activity, to the growth and development of humans and animals,
Metabolism plays an important role, and is widely used in medicine, food and feed etc..L-Trp is some vegetable proteins
The middle amino acid relatively lacked with its condensed food and makees feed addictive to improving the utilization rate of phytoprotein with important
Effect, it be after methionine, lysine and threonine the fourth-largest feed addition amino acid.
The production of L-Trp relies primarily on protein Hydrolyze method and chemical synthesis earliest, but with to microbial method
It is to deepen continuously to produce L-Trp research, and microbial method has moved towards practical and has been in leading position.Currently, L-Trp
Production method is mainly fermentation method, and refining crystallization process mainly has isoelectric point method, solventing-out process and crystallisation by cooling method etc..L-
The solubility of tryptophan in water is smaller, and changes in acid condition less, so in L-Trp with the change of pH value
Isoelectric point crystallizing method is seldom used alone in industrial production.
It is found through retrieval, a kind of process for purification of L-Trp crude product is disclosed in 101531626 A of patent CN, it will be thick
Product are dissolved in the water of 20 times of quality, and the filtrate after decoloration is cooled to 5-15 DEG C, then the 80% of 15% volume ratio is added in filtrate
Acetic acid insulated and stirred crystallizes.This method expends a large amount of solvents, and acetic acid content is relatively low in final mother liquor, can not reuse.Specially
A kind of method of purification of L-Trp crude product is disclosed in sharp CN 101245047, and L-Trp crude product is pressed into mass concentration 1-
1.5% is dissolved in water, and is filtered again after activated carbon decolorizing, and filtrate is through being concentrated in vacuo to the 6-10% postcoolings of original volume to 3-
5 DEG C of crystallizations.Its deficiency is that the solubility of tryptophan in water is very low, a large amount of steam is expended when using condensing crystallizing, and water-soluble
Being concentrated in vacuo for a long time in liquid can cause L-Trp to decompose, and product yield and purity is caused to reduce.
To solve the above-mentioned problems, 104926709 A of patent CN propose a kind of process for purification of L-Trp, the essence
Method processed includes：Crude product is dissolved in the in the mixed solvent of water and acetic acid；Antioxidant is added, adjusts pH value；Activated carbon is added
It is filtered after decoloration；Crystal is collected by centrifugation in crystallisation by cooling, dries to obtain L-Trp；The L-Trp being refining to obtain using this method
Product purity is not less than 99.5%, up to 99.9%, and compared with being concentrated in vacuo method for recrystallizing and refining, saves most of steam
Energy consumption, single output increased 50% or more.But there are still certain defects for the preparation method：1. the preparation efficiency ratio of this method
It is relatively low；The light transmittance of 2.L- tryptophans generally can only achieve 95%, no more than 95%.
Therefore, research and develop a kind of purity that can improve production efficiency and product, light transmittance and yield high-purity high light transmission L-
The preparation process of tryptophan is necessary.
Invention content
The technical problem to be solved in the present invention is to provide a kind of purity that can improve production efficiency and product, light transmittance and
The preparation process of high-purity high light transmission L-Trp of yield.
In order to solve the above technical problems, the technical scheme is that：A kind of preparation work of high-purity high light transmission L-Trp
Skill, innovative point are：The preparation process includes the following steps：
（1）Dissolution filter：L-Trp crude product is added in lysate and is dissolved, while weak acid tune pH value is added, is made
It is fully dissolved；Again after activated carbon adsorption, filtering；
（2）Crystallization：Dissolved solution is slowly crystallized in the case where at the uniform velocity stirring, and is adjusted with lye by vacuumizing simultaneously
Isoelectric point makes its sufficient crystallising；
（3）Centrifugation：By crystal solution centrifugal filtration, white crystal is obtained；
（4）It is dry：By white crystal through pure water, after washing, dry straight color ammonia at a temperature of 60-75 DEG C
Acid.
Further, the step（1）In lysate be pure water and tryptophan mother liquor mixed liquor.
Further, the step（1）Middle pH value is adjusted to 4.0-5.5.
Further, the step（2）In the vacuum degree control that vacuumizes be 0.08-0.095MPa.
Further, the step（2）In while vacuumize, with the isoelectric point of lye tune isoelectric point to L-Trp
5.89。
The advantage of the invention is that：The preparation process of the high-purity high light transmission L-Trp of the present invention, by dissolving and crystallizing
The improvement of step increases the solubility of tryptophan crude product by adjusting pH value in dissolving step；In crystallisation step, lye is used
Isoelectric point is adjusted, the isoelectric point 5.89 of L-Trp is adjusted to, the solubility of tryptophan is minimum in isoelectric point, while true using taking out
Empty mode, makes the discharge rate of moisture increase, and can reduce crystallization time, improves efficiency；At the uniform velocity low temperature stirring and adjusting isoelectric point
It can make the preferable crystal form of product formation, be carried out at the same time with the mode vacuumized, you can ensure the quality and quantity of product, and can phase
To shortening the reaction time, efficiency is improved；By the preparation process, L-Trp obtained, purity is more than 99.8%, and light transmittance can
Up to 97.2%-97.5%, yield is up to 92%-94%.
Specific implementation mode
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among the embodiment described range.
Embodiment 1
The L-Trp crude product 50g of content 95%, light transmittance 38% is added tryptophan mother liquor 300ml, pure water 500ml, and leads to
Peracetic acid tune pH value makes it fully dissolve to 4.0；Then dissolved solution slowly crystallizes under stiring, and vacuumizes, vacuum
Degree is 0.08 MPa, while with the isoelectric point of lye tune isoelectric point to tryptophan 5.89, makes its sufficient crystallising；Again by crystal solution from
The heart filters, and obtains white crystal；Finally, it by white crystal through pure water, after washing, obtains within dry 3 hours at a temperature of 60 DEG C
Sterling L-Trp.
Embodiment 2
The L-Trp crude product 50g of content 95%, light transmittance 38% is added tryptophan mother liquor 300ml, pure water 500ml, and leads to
Peracetic acid tune pH value makes it fully dissolve to 5.5；Then dissolved solution slowly crystallizes under stiring, and vacuumizes, vacuum
Degree is 0.09 MPa, while with the isoelectric point of lye tune isoelectric point to tryptophan 5.89, makes its sufficient crystallising；Again by crystal solution from
The heart filters, and obtains white crystal；Finally, it by white crystal through pure water, after washing, obtains within dry 2 hours at a temperature of 75 DEG C
Sterling L-Trp.
Embodiment 3
The L-Trp crude product 50g of content 95%, light transmittance 38% is added tryptophan mother liquor 300ml, pure water 500ml, and leads to
Peracetic acid tune pH value makes it fully dissolve to 4.8；Then dissolved solution low temperature crystallization under stiring, and vacuumize, vacuum
Degree is 0.085 MPa, and temperature is 78 DEG C, while with the isoelectric point of lye tune isoelectric point to tryptophan 5.89, making its sufficient crystallising；
Again by crystal solution centrifugal filtration, white crystal is obtained；Finally, by white crystal through pure water, after washing, at a temperature of 68 DEG C
Obtain sterling L-Trp within dry 2.5 hours.
Following table is the index parameter table of tryptophan made from the preparation process of the high-purity high light transmission L-Trps of embodiment 1-3.
As can be seen from the above table, the preparation process of the high-purity high light transmission L-Trp of the present invention, by dissolving and crystallizing step
Rapid improvement increases the solubility of tryptophan crude product by adjusting pH value in dissolving step；In crystallisation step, with lye tune
Isoelectric point is saved, the isoelectric point 5.89 of L-Trp is adjusted to, the solubility of tryptophan is minimum in isoelectric point, while using and vacuumizing
Mode, so that the discharge rate of moisture is increased, can reduce crystallization time, improve efficiency；At the uniform velocity low temperature stirring and adjusting isoelectric point can
Make the preferable crystal form of product formation, be carried out at the same time with the mode vacuumized, you can ensures the quality and quantity of product, and can be opposite
Shorten the reaction time, improves efficiency；By the preparation process, L-Trp obtained, purity is more than 99.8%, and light transmittance is reachable
97.2%-97.5%, yield is up to 92%-94%.
The basic principles and main features and advantages of the present invention of the present invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (5)
1. a kind of preparation process of L-Trp, it is characterised in that：The preparation process includes the following steps：
（1）Dissolution filter：L-Trp crude product is added in lysate and is dissolved, while weak acid tune pH value is added, it is made to fill
Divide dissolving；Again after activated carbon adsorption, filtering；
（2）Crystallization：Dissolved solution is slowly crystallized in the case where at the uniform velocity stirring, and electric with lye adjusting etc. by vacuumizing simultaneously
Point makes its sufficient crystallising；
（3）Centrifugation：By crystal solution centrifugal filtration, white crystal is obtained；
（4）It is dry：By white crystal through pure water, after washing, dry sterling tryptophan at a temperature of 60-75 DEG C.
2. the preparation process of L-Trp according to claim 1, it is characterised in that：The step（1）In lysate
For the mixed liquor of pure water and tryptophan mother liquor.
3. the preparation process of L-Trp according to claim 1, it is characterised in that：The step（1）Middle pH value is adjusted
To 4.0-5.5.
4. the preparation process of L-Trp according to claim 1, it is characterised in that：The step（2）In vacuumize
Vacuum degree control is 0.08-0.095MPa.
5. the preparation process of L-Trp according to claim 1, it is characterised in that：The step（2）In vacuumize
Meanwhile with the isoelectric point of lye tune isoelectric point to L-Trp 5.89.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610346788.0A CN105949111B (en) | 2016-05-24 | 2016-05-24 | A kind of preparation process of high-purity high light transmission L-Trp |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106588681B (en) * | 2016-12-07 | 2018-04-03 | 河北科技大学 | A kind of method that L alanine is prepared using hydroxyproline waste water as raw material |
| CN114773251B (en) * | 2022-03-24 | 2024-05-24 | 天津大学 | L-tryptophan spherical crystal and preparation method and application thereof |
| CN116283711A (en) * | 2023-02-21 | 2023-06-23 | 黑龙江新和成生物科技有限公司 | Preparation method of high-purity cake-shaped L-tryptophan crystal and product thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101245047A (en) * | 2008-03-04 | 2008-08-20 | 汕头市紫光古汉氨基酸有限公司 | Purification method for tryptophane |
| CN102260722A (en) * | 2010-05-25 | 2011-11-30 | 陈士安 | Method for producing L-tryptophan |
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- 2016-05-24 CN CN201610346788.0A patent/CN105949111B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101245047A (en) * | 2008-03-04 | 2008-08-20 | 汕头市紫光古汉氨基酸有限公司 | Purification method for tryptophane |
| CN102260722A (en) * | 2010-05-25 | 2011-11-30 | 陈士安 | Method for producing L-tryptophan |
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