CN102001957B - Method for extracting L-threonine - Google Patents
Method for extracting L-threonine Download PDFInfo
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- CN102001957B CN102001957B CN 201010587819 CN201010587819A CN102001957B CN 102001957 B CN102001957 B CN 102001957B CN 201010587819 CN201010587819 CN 201010587819 CN 201010587819 A CN201010587819 A CN 201010587819A CN 102001957 B CN102001957 B CN 102001957B
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Abstract
The invention relates to the field of biochemical engineering, in particular to a method for extracting L-threonine. The method comprises the following steps of: (1) micro-filtrating L-threonine fermentation liquor, concentrating a filtrate to a solid-to-liquid ratio of 0.45-0.75 to 1 and centrifugating to obtain L-threonine crystals and mother liquor; (2) carrying out cross-adsorption on the mother liquor, then, eluting with ammonia with a pH value of 10-14 and collecting eluant from the start of elution to the Baume degree of 1; and (3) adding the L-threonine fermentation liquor to the eluant in the step (2), carrying out micro-filtration, concentrating the filtrate to the solid-to-liquid ratio of 0.45-0.75 to 1, centrifugating to obtain L-threonine crystals and mother liquor and repeating the step (2) to the mother liquor. The method of the invention is simple and convenient for operation without bleaching and can obtain high-quality L-threonine through separation by controlling the concentration times, and the crystallized mother liquor after the cross-adsorption is mixed and cycled with the L-threonine fermentation liquor to improve the purity of the subsequently extracted L-threonine.
Description
Technical field
The present invention relates to biological chemical field, a kind of method of the L-of extraction Threonine specifically is provided.
Background technology
Threonine, the formal name used at school 2 amino 3 hydroxybutyric acid, English Threonine Itaconic acid by name, molecular formula is C
4H
9O
3N, its proterties is white rhombic system or crystalline powder, odorless, it is little sweet, soluble in water to distinguish the flavor of, and is insoluble to ethanol, EC.Threonine is a kind of in 20 seed amino acids of constitutive protein matter, and two unsymmetrical carbons are arranged, and 4 kinds of isomer can be arranged, but natural existence and what organism was had physiological action is the L-Threonine.Because humans and animals self can not synthesize the L-Threonine, need absorb from food, so the L-Threonine is a kind of indispensable amino acid, is mainly used in aspects such as food fortifier, medicine, fodder additives.
As a kind of important food fortifier, the L-Threonine can intensified cereal, cake, milk-product, has to recover human-body fatigue, promote the effect of growing.
Pharmaceutically, contain hydroxyl owing in the structure of L-Threonine, so human body skin is had the water holding effect, hydroxyl can be combined with oligonucleotide chain simultaneously, plays the effect of protection cytolemma; The L-Threonine can also promote the synthetic and Fatty Acid Oxidation of phosphatide in vivo, has the human development of promotion and lipotropic medicinal function.In addition, the L-Threonine is again the raw material of making the efficiently low irritated microbiotic-monobactam of a class, and some character of L-Threonine can also disturb hiv virus, for new approach has been opened up in the development of development anti-AIDS drug.
Aspect livestock culture, the L-Threonine is the 4th stud bird poultry feed indispensable amino acid additive after methionine(Met), Methionin, tryptophane, to the growing of fowl poultry, strengthen fatten, improve fowl poultry meat, stimulating the secretion of milk, lay eggs etc. all has obvious facilitation.
The production method of L-Threonine mainly is to obtain the L-threonine fermentation liquid with producing strain fermentation at present, therefrom extracts the L-Threonine then.The quality height key of L-Threonine product is how to extract from its fermented liquid, Chinese patent publication number CN101293847A discloses a kind of method of being extracted Threonine by threonine fermentation liquid, wherein the L-threonine fermentation liquid through micro-filtration, decolouring, concentrate, obtain L-Threonine crystal behind the primary crystallization, and mother liquor and fermented liquid are mixed into next circulation extraction L-Threonine crystal, and its L-Threonine purity is more than 98.5%.But need fermented liquid is decoloured in this method, complex steps, operation inconvenience, and mother liquor has influenced the dna purity of follow-up L-Threonine without handling directly and fermented liquid mixing capsule usefulness after the crystallization.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of method of the L-of extraction Threonine, this method is easy and simple to handle, the dispense with decoloration step, concentrate directly separating obtained product of back, and mother liquor carries out the attached recycled of ion-exchange absorption after the crystallization, improves the dna purity of L-Threonine.
A kind of method of extracting the L-Threonine of the present invention comprises:
The solid-to-liquid ratio that step 1, L-threonine fermentation liquid micro-filtration, gained filtrate are concentrated into filtrate is 0.45-0.75: 1 back centrifugation obtains L-Threonine crystal and mother liquor;
Step 2, mother liquor carry out ion-exchange absorption, then with pH value be the ammoniacal liquor of 10-14 to resin elution, it is 1 elutriant that the collection wash-out begins to degree Beaume;
Step 3, add micro-filtration behind the L-threonine fermentation liquid in the described elutriant of step 2, the solid-to-liquid ratio that gained filtrate is concentrated into filtrate is 0.45-0.75: 1 back centrifugation obtains L-Threonine crystal and mother liquor, mother liquor repeating step 2.
Particular flow sheet is referring to Fig. 1.
Wherein, the L-threonine fermentation liquid is to obtain after producing bacterial strain and fermenting raw materials by industrial L-Threonine commonly used.
The present invention adopts micro-filtration technology can well remove tropina in the L-threonine fermentation liquid, and wherein to adopt the aperture be that 50nm, molecular weight are the ceramic membrane of 30KD to micro-filtration, and the volume ratio of the filtrate behind the micro-filtration and L-threonine fermentation liquid is 1: 4-6.
The present invention compared with prior art need not to use activated carbon decolorizing behind micro-filtration, directly concentrate, and the solid-to-liquid ratio that control concentrates rear filtrate is 0.45-0.75: 1, and most of impurity and pigment are included in the solution and are removed.Wherein said concentrating is specially:
Gained behind the micro-filtration is stated filtrate under-0.092Mpa pressure, under 50 ℃, 60 ℃, 70 ℃, 80 ℃, carry out preliminary concentrating four times according to the temperature incremental order respectively, the final degree Beaume that tentatively is concentrated into described filtrate is 7-9, then-to carry out the solid-to-liquid ratio that single is concentrated into filtrate under 0.092Mpa, the 55-58 ℃ be 0.45-0.75: 1.
The present invention utilizes the quadruple effect evaporation unit to carry out preliminary concentrating four times in actual production, the steam that the quadruple effect evaporation unit produces when each concentrating can recycle, this scheme that directly meets the requirements of cycles of concentration than once concentration will reduce the quantity of steam of loss, has saved the time of whole concentration process cost in addition.Though utilize the quadruple effect evaporation unit can save time and steam consumption, if but adopt quadruple effect or multi-effect evaporating device directly to be concentrated to the multiple of requirement, can cause line clogging, be unfavorable for follow-up extraction, carry out single again and concentrate to reach cycles of concentration so the present invention carries out four preliminary concentrating earlier.
Solid-to-liquid ratio after the present invention controls well and concentrates, directly centrifugation obtains L-Threonine crystal and mother liquor then, operates more easier than prior art.It is 1.5-3.0 that mother liquor after the separation is adjusted the pH value, carries out ion-exchange absorption then, the most Impurity removals in the mother liquor can be applied mechanically with L-threonine fermentation liquid mixed cycle then, has so not only improved L-Threonine purity, has also guaranteed total extraction yield.Wherein, described ion-exchange absorption can be adopted resin absorption such as 732 types, JK008 type or JK006 type.
In elution process, the present invention detects elutriant with Beaum and HPLC method, the result shows that beginning to the elutriant degree Beaume from wash-out is the elutriant of 1-1.5, its L-threonine content is generally more than 0.5%, for guaranteeing the L-Threonine purity of subsequent extracted, it is that 1 elutriant carries out recycled that the present invention collects that wash-out begins to the elutriant degree Beaume, only needs like this to use a Beaum just can collect elutriant fast and accurately in actual production.
The method of extraction L-Threonine provided by the present invention, step is easy, the dispense with decoloration step, the cycles of concentration of controlling well is the separable high-quality L-Threonine that obtains, mother liquor after the crystallization carried out ion-exchange absorption is attached to be applied mechanically with L-threonine fermentation liquid mixed cycle again, improved the L-Threonine purity of subsequent extracted.
Description of drawings
Figure 1 shows that the method flow diagram of extraction L-Threonine of the present invention.
Embodiment
The invention discloses a kind of method of the L-of extraction Threonine, those skilled in the art can use for reference this paper content, suitably improve processing parameter and realize.Special needs to be pointed out is that all similarly replace and change apparent to those skilled in the art, they all are regarded as being included in the present invention.Method of the present invention is described by preferred embodiment, and the related personnel obviously can change or suitably change and combination methods and applications as herein described in not breaking away from content of the present invention, spirit and scope, realizes and use the technology of the present invention.
According to the present invention, described a kind of method of extracting the L-Threonine comprises:
The solid-to-liquid ratio that step 1, L-threonine fermentation liquid micro-filtration, gained filtrate are concentrated into filtrate is 0.45-0.75: 1 back centrifugation obtains L-Threonine crystal and mother liquor;
Step 2, mother liquor carry out ion-exchange absorption, then with pH value be the ammoniacal liquor of 10-14 to resin elution, it is 1 elutriant that the collection wash-out begins to degree Beaume;
Step 3, add micro-filtration behind the L-threonine fermentation liquid in the described elutriant of step 2, the solid-to-liquid ratio that gained filtrate is concentrated into filtrate is 0.45-0.75: 1 back centrifugation obtains L-Threonine crystal and mother liquor, mother liquor repeating step 2.
Wherein, described micro-filtration is for being that 50nm, molecular weight are the ceramic membrane micro-filtration of 30KD with the aperture, and the volume ratio of gained filtrate and L-threonine fermentation liquid is 1 behind the micro-filtration: 4-6.
Of the present invention concentrating is specially:
Gained filtrate is under-0.092Mpa pressure behind the micro-filtration, under 50 ℃, 60 ℃, 70 ℃, 80 ℃, carry out preliminary concentrating four times according to the temperature incremental order respectively, the final degree Beaume that tentatively is concentrated into described filtrate is 7-9, then-carry out single under 0.092Mpa, the 55-58 ℃ to concentrate.
The L-Threonine that the method for the invention is extracted detects through the HPLC method, its purity is all more than 99%, improved about 1% than 98.5% of prior art, show that the method for the invention is not having still to obtain high-quality L-Threonine under the situation of decoloration process, also avoided the direct recycled of crystallization stepmother liquid to reduce the problem of L-Threonine purity.
Below in conjunction with embodiment, further set forth the present invention.
Embodiment 1: the method for extraction L-Threonine of the present invention
1, extracting method
The L-threonine fermentation liquid is filtered by ceramic membrane after sterilizing, and the ceramic membrane aperture is that 50nm, molecular weight are 30KD, working pressure 1.5bar, and transmembrane pressure 1bar, 25 ℃ of temperature, the volume ratio of filtrate and L-threonine fermentation liquid is 1: 4.
The L-Threonine filtrate that obtains enters the quadruple effect evaporation and tentatively concentrates, vacuum degree control is at-0.092Mpa, temperature is controlled to be 50 ℃, 60 ℃, 70 ℃, 80 ℃ respectively, and the Baume concentration of finally controlling filtrate reaches 7, enters single-effect evaporator then and further concentrates, 55 ℃ of control temperature, vacuum degree control is at-0.092Mpa, and mixing speed 80rpm is concentrated into the filtrate solid-to-liquid ratio and reaches 0.45: 1 and put jar, centrifugation obtains L-Threonine crystal and mother liquor.
The mother liquor adjust pH that obtains after the crystallization is 1.5, carry out ion-exchange absorption with 732 type resins, it is 10 ammoniacal liquor wash-out with the pH value, collecting that wash-out begins to the elutriant degree Beaume is 1 elutriant, adding the L-threonine fermentation liquid mixes and carries out that micro-filtration, quadruple effect tentatively concentrate, single-action concentrates, separate obtaining L-Threonine crystal and mother liquor then, mother liquor repeats above-mentioned steps.
2, product detects
With the HPLC method product is carried out content detection, the L-threonine content is 99.5%.Detected result shows, the method for the invention dispense with decoloration step, and the L-Threonine quality of extracting is higher, and the elutriant after ion-exchange absorption is handled has improved L-Threonine purity.
Embodiment 2: the method for extraction L-Threonine of the present invention
1, extracting method
The L-threonine fermentation liquid is filtered by ceramic membrane after sterilizing, and the ceramic membrane aperture is that 50nm, molecular weight are 30KD, working pressure 1.5bar, and transmembrane pressure 1bar, 25 ℃ of temperature, the volume ratio of filtrate and L-threonine fermentation liquid is 1: 6.
The L-Threonine filtrate that obtains enters the quadruple effect evaporation and tentatively concentrates, vacuum degree control is at-0.092Mpa, temperature is controlled to be 50 ℃, 60 ℃, 70 ℃, 80 ℃ respectively, and the Baume concentration of finally controlling filtrate reaches 8, enters single-effect evaporator then and further concentrates, 58 ℃ of control temperature, vacuum degree control is at-0.092Mpa, and mixing speed 80rpm is concentrated into the filtrate solid-to-liquid ratio and reaches 0.75: 1 and put jar, centrifugation obtains L-Threonine crystal and mother liquor.
The mother liquor adjust pH that obtains after the crystallization is 3.0, carry out ion-exchange absorption with JK008 type resin, it is 12 ammoniacal liquor wash-out with the pH value, collecting that wash-out begins to the elutriant degree Beaume is 1 elutriant, adding the L-threonine fermentation liquid mixes and carries out that micro-filtration, quadruple effect tentatively concentrate, single-action concentrates, separate obtaining L-Threonine crystal and mother liquor then, mother liquor repeats above-mentioned steps.
2, product detects
With the HPLC method product is carried out content detection, the L-threonine content is 99.2%.Detected result shows, the method for the invention dispense with decoloration step, and the L-Threonine quality of extracting is higher, and the elutriant after ion-exchange absorption is handled has improved L-Threonine purity.
Embodiment 3: the method for extraction L-Threonine of the present invention
1, extracting method
The L-threonine fermentation liquid is filtered by ceramic membrane after sterilizing, and the ceramic membrane aperture is that 50nm, molecular weight are 30KD, working pressure 1.5bar, and transmembrane pressure 1bar, 25 ℃ of temperature, the volume ratio of filtrate and L-threonine fermentation liquid is 1: 5.
The L-Threonine filtrate that obtains enters the quadruple effect evaporation and tentatively concentrates, vacuum degree control is at-0.092Mpa, temperature is controlled to be 50 ℃, 60 ℃, 70 ℃, 80 ℃ respectively, and the Baume concentration of finally controlling filtrate reaches 9, enters single-effect evaporator then and further concentrates, 57 ℃ of control temperature, vacuum degree control is at-0.092Mpa, and mixing speed 80rpm is concentrated into the filtrate solid-to-liquid ratio and reaches 0.6: 1 and put jar, centrifugation obtains L-Threonine crystal and mother liquor.
The mother liquor adjust pH that obtains after the crystallization is 2, carry out ion-exchange absorption with JK006 type resin, it is 14 ammoniacal liquor wash-out with the pH value, collecting that wash-out begins to the elutriant degree Beaume is 1 elutriant, adding the L-threonine fermentation liquid mixes and carries out that micro-filtration, quadruple effect tentatively concentrate, single-action concentrates, separate obtaining L-Threonine crystal and mother liquor then, mother liquor repeats above-mentioned steps.
2, product detects
With the HPLC method product is carried out content detection, the L-threonine content is 99.1%.Detected result shows, the method for the invention dispense with decoloration step, and the L-Threonine quality of extracting is higher, and the elutriant after ion-exchange absorption is handled has improved L-Threonine purity.
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. a method of extracting the L-Threonine is characterized in that, comprising:
The solid-to-liquid ratio that step 1, L-threonine fermentation liquid micro-filtration, gained filtrate are concentrated into filtrate is centrifugation behind the 0.45-0.75:1, obtains L-Threonine crystal and mother liquor;
Step 2, mother liquor carry out ion-exchange absorption, then with pH value be the ammoniacal liquor of 10-14 to resin elution, it is 1 elutriant that the collection wash-out begins to degree Beaume;
Step 3, add micro-filtration behind the L-threonine fermentation liquid in the described elutriant of step 2, the solid-to-liquid ratio that gained filtrate is concentrated into filtrate is centrifugation behind the 0.45-0.75:1, obtains L-Threonine crystal and mother liquor, mother liquor repeating step 2.
2. according to the described method of claim 1, it is characterized in that described micro-filtration is for being that 50nm, molecular weight are the ceramic membrane micro-filtration of 30KD with the aperture.
3. according to the described method of claim 1, it is characterized in that the volume ratio of gained filtrate and L-threonine fermentation liquid is 1:4-6 behind the micro-filtration.
4. according to the described method of claim 1, it is characterized in that described the concentrating of step 1 and step 3 is specially:
Gained filtrate is under-0.092Mpa pressure behind the micro-filtration, under 50 ℃, 60 ℃, 70 ℃, 80 ℃, carry out preliminary concentrating four times according to the temperature incremental order respectively, the final degree Beaume that tentatively is concentrated into described filtrate is 7-9, then-carry out single under 0.092Mpa, the 55-58 ℃ to concentrate.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102351723A (en) * | 2011-08-30 | 2012-02-15 | 无锡荣丰生物工程有限公司 | Triple-effect internal circulation continuous evaporative crystallization process of threonine |
| CN102578385B (en) * | 2011-12-30 | 2013-11-13 | 通辽梅花生物科技有限公司 | Preparation method of feed with low content of L-threonine |
| CN102911070A (en) * | 2012-11-13 | 2013-02-06 | 河南巨龙生物工程股份有限公司 | Technology for separating and extacting L-threonine from fermentation broth |
| CN110051634A (en) * | 2019-05-29 | 2019-07-26 | 绥化象屿金谷生化科技有限公司 | A kind of L-threonine processes for wet granulation |
| CN118359511B (en) * | 2024-06-19 | 2024-09-03 | 东晓生物科技股份有限公司 | Extraction method for removing peculiar smell of feed-grade threonine product |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3616217A (en) * | 1966-08-04 | 1971-10-26 | Kiyoshi Watanabe | Process for preparing l-threonine |
| US7598062B2 (en) * | 2001-04-03 | 2009-10-06 | Evonik Degussa Gmbh | Process for the production of L-amino acids using strains of the family enterobacteriaceae that contain an attenuated fruR gene |
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2010
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3616217A (en) * | 1966-08-04 | 1971-10-26 | Kiyoshi Watanabe | Process for preparing l-threonine |
| US7598062B2 (en) * | 2001-04-03 | 2009-10-06 | Evonik Degussa Gmbh | Process for the production of L-amino acids using strains of the family enterobacteriaceae that contain an attenuated fruR gene |
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