CN114835600A - Method for extracting L-glutamine - Google Patents
Method for extracting L-glutamine Download PDFInfo
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- CN114835600A CN114835600A CN202110371318.0A CN202110371318A CN114835600A CN 114835600 A CN114835600 A CN 114835600A CN 202110371318 A CN202110371318 A CN 202110371318A CN 114835600 A CN114835600 A CN 114835600A
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Abstract
The invention provides an extraction method of L-glutamine, which comprises the following steps: and carrying out primary concentration crystallization, crystal dissolving and decoloring, electrodialysis desalination, anion exchange and secondary concentration crystallization on the fermentation filtered clear liquid containing the L-glutamine to obtain the L-glutamine. The extraction method provided by the invention improves the purity and yield of the L-glutamine product, and simultaneously, the wastewater generated in the extraction process can be recycled, so that the environmental protection load is reduced, and the extraction cost is reduced.
Description
Technical Field
The invention belongs to the technical field of L-glutamine, relates to an extraction method of L-glutamine, and particularly relates to a method for extracting L-glutamine from L-glutamine-containing fermentation liquor.
Background
Glutamine is the most abundant free amino acid in muscle, accounting for about 60% of the total amount of free amino acid in human body, and can be synthesized by glutamic acid, valine and isoleucine in human body, and the fasting plasma glutamine concentration is 500-; under stress conditions of diseases, poor nutritional state or high-intensity exercise, the demand of the body for glutamine increases, so that self-synthesis cannot meet the demand. Glutamine has a number of effects on the body: 1. growing the muscle; 2. glutamine has a powerful effect; 3. the important fuel of the immune system can enhance the function of the immune system; 4. involved in the synthesis of glutathione, an important antioxidant; 5. the basic energy source of gastrointestinal tract lumen cells maintains the structure and function of the intestinal barrier; 6. improving brain function, and improving oxidation resistance of organism; 7. the glutamine-enriched nutrition support has the functions of improving the metabolism of the organism, balancing nitrogen, promoting protein synthesis and increasing the total number of lymphocytes; 8. glutamine can maintain intestinal permeability of patients with severe pancreatitis, reduce intestinal bacterial translocation, inhibit inflammatory mediator release, reduce stress reaction degree of organism, and shorten hospitalization time; 9. timely and proper glutamine supplementation can effectively prevent the decomposition of muscle protein, increase the volume of cells through the hydration of the cells and promote the growth of muscles.
In recent years, with the progress and development of studies on glutamine in physiological, biochemical, clinical and other aspects, glutamine has been increasingly important for life activities. The small-batch industrial production of glutamine fermentation method has been started in China, and the technology of separation and purification as a downstream process is one of the important reasons for influencing the product quality and the cost. The main by-product in the glutamine fermentation process is glutamic acid, the molecular structures and chemical properties of glutamine and glutamic acid are similar, the separation is difficult, the glutamine is unstable, and the glutamine is easily converted into the glutamic acid under the acidic condition in the separation process, so the quality of the finished product of the glutamine is influenced. The extraction and separation method for producing glutamine by traditional fermentation method mainly comprises a primary concentration crystallization method, an ice-out method and a double-column method for extracting and purifying glutamine. At present, most of extraction and separation methods mostly adopt a cation-anion double-column ion exchange method to extract glutamine, however, the cation-anion double-column separation process has the problems of large consumption of exchange resin and high consumption of acid and alkali in the elution and regeneration processes, and glutamine is easily converted into glutamic acid in a strong acid or strong alkali environment, so that the yield is low.
Therefore, it is necessary to provide a novel process for extracting L-glutamine.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the L-glutamine extraction method, the purity and the yield of the L-glutamine product are improved, and meanwhile, the wastewater generated in the extraction process can be recycled, so that the environmental protection load is reduced, and the extraction cost is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides an extraction method of L-glutamine, which comprises the following steps:
and carrying out primary concentration crystallization, crystal dissolving and decoloring, electrodialysis desalination, anion exchange and secondary concentration crystallization on the fermentation filtered clear liquid containing the L-glutamine to obtain the L-glutamine.
The invention utilizes the cooperation of electrodialysis desalination and a single column method (anion exchange column) to separate glutamine and glutamic acid, can reduce the consumption of exchange resin, reduce the elution process, avoid that the glutamine is easily converted into the glutamic acid in a strong acid or strong base environment, and improve the yield of the glutamine.
In order to further reduce the cost and reduce the environmental load, the method for primary concentration crystallization comprises the following steps: concentrating the fermented filtered clear liquid by using a membrane and concentrating in vacuum to obtain a concentrated solution containing L-glutamine.
The invention uses membrane concentration technology to reduce energy consumption of vacuum concentration, and on the other hand, water removed by membrane concentration can be reused to reduce water consumption, if vacuum concentration is directly used, energy is wasted, the solvent distilled in vacuum can not be reused, and environmental protection load is increased.
In a preferred embodiment of the present invention, the membrane concentration removes 40-60% of the water in the fermentation filtrate supernatant, such as 45%, 50%, 55%, etc. If the water removed by membrane concentration is less, the energy consumed by vacuum concentration is larger; if more water needs to be removed for membrane concentration, the time required for membrane concentration is longer, which in turn increases the overall extraction process time.
As a preferred technical scheme of the invention, the concentration pressure of the vacuum concentration is controlled to be-0.052 to-0.068 MPa, and the discharge temperature is 65 to 75 ℃.
In a preferred embodiment of the present invention, the concentration of L-glutamine in the concentrated solution is 60 to 65%, for example, 61%, 62%, 63%, 64%.
As a preferred embodiment of the present invention, the crystallization method comprises: cooling the concentrated solution to separate out crystals, stirring for crystal growth, stirring at a rotating speed of 40-50r/min for 20-24h, growing the crystals at 35 ℃ for 1 h, continuously cooling for a certain time, slowly cooling to 15 ℃, and then performing centrifugal separation by using a low-speed centrifuge.
As a preferred technical scheme of the invention, the decolorization is carried out by using activated carbon, the light transmittance of the decolorized filtrate reaches more than 95%, and the adding amount of the activated carbon is about 5kg per ton of L-glutamine fermentation liquor.
The preparation method of the fermentation filtered clear liquid containing the L-glutamine comprises the following steps: and filtering the fermentation liquor containing the L-glutamine by using a ceramic membrane and a nanofiltration membrane to obtain the fermentation filtered clear liquid containing the L-glutamine.
As a preferable technical scheme of the invention, the concentration of the L-glutamine in the fermentation liquor is about 5-20%, and the content is 80-100 g/L.
The invention sequentially utilizes the ceramic membrane and the nanofiltration membrane to filter the fermentation liquor, and removes residual sugar, mycoprotein and part of acid radical ions in the fermentation liquor. In the invention, the nanofiltration step is preferably carried out before the fermentation and filtration clear liquid is concentrated, and the nanofiltration is firstly carried out to obtain the filtered clear liquid, and then the post-treatment such as concentration and crystallization is carried out, so that the clear liquid contains less impurities, the crystallization amount can be increased during the concentration and crystallization, the content of glutamine in the mother liquid can be reduced, and the yield of the final glutamine can be increased.
The mother liquor refers to the mother liquor, after primary concentration and crystallization, crystals and solution are separated, and the separated solution is called the mother liquor.
In a preferred embodiment of the present invention, when the fermentation broth is filtered by a ceramic membrane, the volume ratio of the clear filtrate to the concentrated phase is controlled to (5-7: 1), for example, 5.5:1, 6:1, 6.5:1, etc.
In a preferred embodiment of the present invention, when the fermentation liquid is filtered by a nanofiltration membrane, the volume ratio of the clear filtered liquid to the concentrated phase is controlled to be (8-10: 1), for example, 8.5:1, 9:1, 9.5:1, etc.
When the fermentation liquor is filtered, the amount of the dialysis water needs to be controlled, so that the yield is ensured, and the waste of energy is avoided.
In a preferred embodiment of the present invention, the fermentation broth containing L-glutamine has a temperature of 55 to 65 deg.C, for example, 60 deg.C. The fermentation liquor can be subjected to heat exchange before filtration, and membrane filtration treatment is carried out when the temperature reaches 55-65 ℃, so that the flux stability and efficiency of a membrane system can be ensured within the temperature range.
The pH value of the solution is adjusted to 4-6 before the anion exchange is carried out.
As a preferable technical scheme of the invention, the anion exchange is carried out by using D330 anion exchange resin, and the conductivity of the solution after the ion exchange is less than or equal to 200 mu s/cm.
The invention adjusts the pH value of the solution to 5-6 before the electrodialysis is carried out.
The electrodialysis desalination of the invention comprises the following steps: adjusting pH of the decolorized solution to 5-6, adding 1% thiamine aqueous solution and 0.25mol/L Na 2 SO 4 Removing salt from the aqueous solution by direct current, wherein SO is mainly removed 4 2- And (4) acid radical ions.
The secondary concentration crystallization is preferably performed by vacuum concentration and then temperature reduction crystallization. The vacuum concentration comprises: the vacuum concentration is utilized for concentration, the pressure of the vacuum concentration is-0.055 to-0.07 MPa, the discharging temperature is 65-70 ℃, and the discharging concentration is 65-68%. And the cooling crystallization comprises the steps of cooling and crystallizing the concentrated solution, then stirring and crystallizing, stirring at the rotating speed of 40-50r/min for 20-24h, growing the crystals at 35 ℃ for 1 h, continuously cooling and growing the crystals for a certain time, slowly cooling to 15 ℃, and then carrying out centrifugal separation on the finished product crystal slurry to obtain the finished wet crystals.
As a specific embodiment of the present invention, the extraction method includes the steps of:
(1) filtering the fermentation liquor containing L-glutamine at the temperature of 45-60 ℃ by using a ceramic membrane, controlling the volume ratio of the filtered clear liquid to the concentrated phase to be (5-7):1, then filtering by using a nanofiltration membrane, controlling the volume ratio of the filtered clear liquid to the concentrated phase to be (8-10):1, and obtaining the fermented filtered clear liquid containing L-glutamine;
(2) performing membrane concentration on the fermentation filtered clear liquid containing L-glutamine, removing 40-60% of water in the fermentation filtered clear liquid, and then performing vacuum concentration to obtain a concentrated solution with the concentration of L-glutamine of 60-65%;
(3) and (3) cooling, crystallizing, dissolving crystals and decoloring the concentrated solution, then adjusting the pH value of the solution to 5-6, performing electrodialysis desalination, adjusting the pH value of the solution to 4-6, performing anion exchange by using D330 anion exchange resin, finally performing secondary concentration, crystallization and drying to obtain the L-glutamine.
As a preferable embodiment of the present invention, the L-glutamine-containing fermentation liquid is obtained by fermentation using Corynebacterium glutamicum.
As a preferable technical scheme of the invention, the fermentation temperature is 30-35 ℃, the pH value is 6.2-7.2, and the fermentation period is about 60 hours.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the fermentation liquor is preferably filtered by adopting a ceramic membrane and a nanofiltration membrane, and then the filtrate is subjected to post-treatment, so that the impurities contained in the clear liquid are less, the crystallization amount can be increased during concentration and crystallization, the content of glutamine in the mother liquor is reduced, and the final yield of glutamine can be increased;
(2) according to the invention, the membrane concentration is preferably adopted for carrying out pre-concentration and then carrying out vacuum concentration for one-time concentration crystallization, and the concentration mode can reduce energy consumption, and simultaneously, water obtained by membrane concentration can be recycled, so that the water consumption is reduced, and the environmental protection load is reduced;
(3) the extraction method of the L-glutamine can improve the purity and the yield of the L-glutamine product, wherein the yield of the product is more than 83.5 percent, and the purity is more than 99.8.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the specific embodiments are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
This example provides a method for extracting L-glutamine.
(1) Carrying out heat exchange on L-glutamine fermentation liquor from a fermentation workshop through a plate heat exchanger to ensure that the temperature of the fermentation liquor reaches 60 ℃, then carrying out ceramic membrane filtration, controlling the volume ratio of clear liquor to concentrated phase to be 5:1 during filtration, and then carrying out nanofiltration membrane filtration to ensure that the volume ratio of the nanofiltration clear liquor to the concentrated phase is controlled to be 9:1, thus obtaining fermentation filtration clear liquor containing L-glutamine;
(2) performing membrane concentration on the fermentation filtered clear liquid containing the L-glutamine, removing 50% of water in the fermentation filtered clear liquid, then performing vacuum concentration, controlling the pressure to be about-0.055 MPa and the discharge temperature to be 70 ℃, and pumping the concentrated liquid with the concentration of the L-glutamine of 65% into a stock solution crystallization tank;
(3) cooling the concentrated solution to separate out crystals, stirring for crystal growth, stirring at a rotating speed of 45r/min for 24h, growing the crystals at 35 ℃ for 1 h, continuously cooling for crystal growth for a certain time, slowly cooling to 15 ℃ for centrifugal separation, feeding wet crystals into a decoloring tank, and refluxing mother liquor;
(4) dissolving wet crystals, decolorizing with active carbon (5 kg/ton L-glutamine fermentation liquor), regulating pH of decolorized filtrate to about 5.5, adding 1% thiamine water solution and 0.25mol/L Na 2 SO 4 Introducing direct current into the aqueous solution for desalting, filtering, adjusting the pH value to about 4.5 again, performing ion exchange through a D330 anion exchange resin column, wherein the conductivity of the solution after ion exchange is less than or equal to 200 mus/cm;
(5) pumping the solution after ion exchange into a vacuum concentration system, evaporating and concentrating again, controlling the pressure to be about-0.06 MPa, the discharging temperature to be 70 ℃, and the discharging concentration to be 65%;
(6) pumping the concentrated solution into a finished product crystallizing tank for cooling crystallization, then stirring for crystal growth, stirring at the rotating speed of 45r/min for 24 hours, growing the crystal at 35 ℃ for 1 hour, continuously cooling for a certain time, slowly cooling to 15 ℃, then performing centrifugal separation on the finished product crystal slurry, and drying and packaging the finished product wet crystal.
Example 2
This example provides a method for extracting L-glutamine.
(1) Carrying out heat exchange on L-glutamine fermentation liquor from a fermentation workshop through a plate heat exchanger to ensure that the temperature of the fermentation liquor reaches 65 ℃, then carrying out ceramic membrane filtration, controlling the volume ratio of clear liquor to concentrated phase to be 7:1 during filtration, and then carrying out nanofiltration membrane filtration to ensure that the volume ratio of the nanofiltration clear liquor to the concentrated phase is controlled to be 8:1, thus obtaining fermentation filtration clear liquor containing L-glutamine;
(2) performing membrane concentration on the fermentation filtered clear liquid containing the L-glutamine, removing 60 percent of water in the fermentation filtered clear liquid, then performing vacuum concentration, controlling the pressure to be about-0.055 MPa and the discharge temperature to be 70 ℃, and pumping the concentrated solution with the concentration of the L-glutamine of 60 percent into a stock solution crystallization tank;
(3) cooling the concentrated solution to separate out crystals, stirring for crystal growth, stirring at a rotating speed of 45r/min for 24h, growing the crystals at 35 ℃ for 1 h, continuously cooling for crystal growth for a certain time, slowly cooling to 15 ℃ for centrifugal separation, feeding wet crystals into a decoloring tank, and refluxing mother liquor;
(4) dissolving wet crystals, decolorizing with active carbon (5 kg/ton L-glutamine fermentation liquor), regulating pH of decolorized filtrate to about 6, adding 1% thiamine water solution and 0.25mol/L Na 2 SO 4 Introducing direct current into the aqueous solution for desalting, filtering, adjusting the pH value to about 5 again, performing ion exchange by using a D330 anion exchange resin column, wherein the conductivity of the solution after ion exchange is less than or equal to 200 mus/cm;
(5) pumping the solution after ion exchange into a vacuum concentration system, evaporating and concentrating again, controlling the pressure to be about-0.07 MPa, the discharging temperature to be 65 ℃ and the discharging concentration to be 68%;
(6) pumping the concentrated solution into a finished product crystallizing tank for cooling crystallization, then stirring for crystal growth, stirring at the rotating speed of 45r/min for 24 hours, growing the crystal at 35 ℃ for 1 hour, continuously cooling for a certain time, slowly cooling to 15 ℃, then performing centrifugal separation on the finished product crystal slurry, and drying and packaging the finished product wet crystal.
Comparative example 1
This comparative example provides a method for extracting L-glutamine.
The difference from example 1 is that in this comparative example, step (2) omits the membrane concentration process and directly performs vacuum concentration, specifically:
vacuum concentrating the fermented and filtered clear liquid containing L-glutamine under the pressure of about-0.055 MPa and the discharge temperature of 70 ℃ to obtain a concentrated solution with the concentration of the L-glutamine of 65 percent, and pumping the concentrated solution into a stock solution crystallizing tank.
Comparative example 2
This comparative example provides a method for extracting L-glutamine.
The difference from example 1 is that in this comparative example, nanofiltration was set up after anion exchange, the specific steps were as follows:
(1) carrying out heat exchange on L-glutamine fermentation liquor from a fermentation workshop through a plate heat exchanger to ensure that the temperature of the fermentation liquor reaches 60 ℃, then carrying out ceramic membrane filtration, controlling the volume ratio of clear liquor to concentrated phase to be 5:1 during filtration to obtain fermented filtered clear liquor containing L-glutamine, wherein the concentration of the L-glutamine is controlled to be the same as that of the L-glutamine in the embodiment 1;
(2) - (4) same as steps (2) to (4) of example 1;
(5) nanofiltration is carried out on the solution after ion exchange, then the solution is pumped into a vacuum concentration system, evaporation concentration is carried out again, the pressure is controlled to be about-0.06 MPa, the discharging temperature is 70 ℃, and the discharging concentration is 65%;
(6) same as in step (6) of example 1.
Comparative example 3
This comparative example provides a method for extracting L-glutamine using a two-column method.
(1) Ceramic membrane filtration: feeding L-glutamine fermentation liquor from a fermentation workshop into a ceramic membrane for circulating filtration to obtain fermentation filtration clear liquid, and cooling ceramic membrane circulation feed liquid by using circulating water in the circulating process to keep the temperature of the fermentation liquor below 70 ℃;
(2) primary crystallization: concentrating the concentrated feed liquid at 50 deg.C and 80rpm under vacuum, cooling the concentrated liquid product to 15 deg.C with circulating water under vacuum degree of-0.098 MPa, growing crystal for 4 hr at stirring speed of 20rpm, and centrifuging at 1200rpm to obtain wet product crystal;
(3) and (3) re-dissolving the crude product: dissolving wet products by reverse osmosis water at 70 ℃ and 40rpm, adding crude products according to the amount of 10 percent of product content, and adjusting the pH value to 3.5 by using hydrochloric acid to obtain crude product dissolved solution;
(4) ion exchange: allowing crude dissolving solution at 40 deg.C to pass through 732 cation exchange column with volume of resin 1 times per hour, and then passing through 330 anion exchange column at the same rate to obtain ion exchange solution;
(5) and (4) nanofiltration: allowing the ion exchange liquid to enter a nanofiltration device at normal temperature for circular filtration, and cooling with circulating water to keep the temperature of the liquid below 50 ℃ to obtain nanofiltration dialysis liquid;
(6) decoloring and removing impurities: heating the nanofiltration dialysis liquid to 70 ℃, adding 767 medicinal active carbon of 0.3%, keeping the temperature for 30min, stirring at 60rpm, and circularly filtering through a filter to remove the active carbon in the liquid when the transmittance reaches more than 95% to obtain a decolorized liquid;
(7) reverse osmosis concentration: cooling the decolorized solution to 40 deg.C, concentrating by reverse osmosis concentration circulator until the content reaches 15%, and adjusting pH of the feed solution to 6.0-6.5 with H-type 732 cation exchange resin;
(8) secondary crystallization: and (3) utilizing a single-effect concentration crystallization tank, keeping the stirring speed at 20rpm when the temperature is less than or equal to 50 ℃, the vacuum degree is-0.098 MPa, the stirring speed is 60rpm, when the content of the concentrated solution is more than 60%, cooling to 15 ℃ by using circulating water at the cooling speed of 15 ℃/h, growing crystals for 4h, obtaining wet product crystals by using a centrifuge, drying and packaging.
Performance testing
The initial L-glutamine fermentation liquids used in the examples and comparative examples of the present invention were the same fermentation liquids, and the volume was 100L, and the L-glutamine content was 90.0 g/L.
Energy consumption in examples and comparative examples was counted, finished crystals obtained in examples and comparative examples were weighed, purity thereof was checked and yield thereof was calculated, and the results are shown in table 1:
TABLE 1
As can be seen from Table 1, the extraction method of L-glutamine provided by the invention can reduce energy consumption and improve the yield and purity of the product, wherein the purity of the product can reach more than 99.8%, and the yield is more than 83.5%.
As can be seen from the comparison between example 1 and comparative example 1, the invention adopts the combination of membrane concentration and vacuum concentration, which can reduce energy consumption and product cost; as can be seen from the comparison between example 1 and comparative example 2, the present invention combines nanofiltration with ceramic membrane filtration to filter the fermentation broth first, which can further improve the yield of the product.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A method for extracting L-glutamine, which is characterized by comprising the following steps:
and carrying out primary concentration crystallization, crystal dissolving and decoloring, electrodialysis desalination, anion exchange and secondary concentration crystallization on the fermentation filtered clear liquid containing the L-glutamine to obtain the L-glutamine.
2. The extraction method according to claim 1, wherein the primary concentration and crystallization method comprises: concentrating the fermented filtered clear liquid by using a membrane and concentrating in vacuum to obtain a concentrated solution containing L-glutamine.
3. The extraction process according to claim 2, wherein the membrane concentration removes 40-60% of the water in the fermentation filtrate supernatant.
4. The extraction method according to claim 2 or 3, wherein the concentration of L-glutamine in the concentrated solution is 60 to 65%.
5. The extraction process according to any one of claims 1 to 4, wherein the preparation process of the L-glutamine containing fermentation filtrate comprises: and filtering the fermentation liquor containing the L-glutamine by using a ceramic membrane and a nanofiltration membrane to obtain the fermentation filtered clear liquid containing the L-glutamine.
6. The extraction method according to claim 5, wherein when the fermentation liquor is filtered by using the ceramic membrane, the volume ratio of the clear filtered liquid to the concentrated phase is controlled to be (5-7): 1;
and/or when the fermentation liquor is filtered by a nanofiltration membrane, controlling the volume ratio of the clear filtered liquid to the concentrated phase to be (8-10) to 1.
7. The extraction process according to claim 5 or 6, wherein the fermentation broth containing L-glutamine has a temperature of 55-65 ℃.
8. The extraction process according to any one of claims 1 to 7, characterized in that, before the anion exchange is carried out, the pH of the solution is adjusted to a value of 4 to 6;
and/or, the anion exchange is performed using a D330 anion exchange resin.
9. The extraction process according to any one of claims 1 to 8, characterized in that the solution pH is adjusted to 5 to 6 before the electrodialysis is carried out.
10. The extraction method according to any one of claims 1 to 9, characterized in that it comprises the steps of:
(1) filtering the fermentation liquor containing L-glutamine at the temperature of 45-60 ℃ by using a ceramic membrane, controlling the volume ratio of the filtered clear liquid to the concentrated phase to be (5-7):1, then filtering by using a nanofiltration membrane, controlling the volume ratio of the filtered clear liquid to the concentrated phase to be (8-10):1, and obtaining the fermented filtered clear liquid containing L-glutamine;
(2) performing membrane concentration on the fermentation filtered clear liquid containing L-glutamine, removing 40-60% of water in the fermentation filtered clear liquid, and then performing vacuum concentration to obtain a concentrated solution with the concentration of L-glutamine of 60-65%;
(3) cooling and crystallizing the concentrated solution, dissolving crystals and decoloring, then adjusting the pH value of the solution to 5-6, performing electrodialysis desalination, adjusting the pH value of the solution to 4-6, performing anion exchange by using D330 anion exchange resin, finally performing secondary concentration crystallization, and drying to obtain the L-glutamine;
preferably, the fermentation broth containing L-glutamine is obtained by fermentation using Corynebacterium glutamicum.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755586A (en) * | 2013-12-24 | 2014-04-30 | 山东民强生物科技股份有限公司 | Preparation method of L-glutamine |
| CN108285913A (en) * | 2017-12-09 | 2018-07-17 | 新疆阜丰生物科技有限公司 | A kind of technique preparing extraction L-Glutamine |
| CN111057727A (en) * | 2019-12-16 | 2020-04-24 | 新疆阜丰生物科技有限公司 | Method for producing, separating and extracting L-glutamine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755586A (en) * | 2013-12-24 | 2014-04-30 | 山东民强生物科技股份有限公司 | Preparation method of L-glutamine |
| CN108285913A (en) * | 2017-12-09 | 2018-07-17 | 新疆阜丰生物科技有限公司 | A kind of technique preparing extraction L-Glutamine |
| CN111057727A (en) * | 2019-12-16 | 2020-04-24 | 新疆阜丰生物科技有限公司 | Method for producing, separating and extracting L-glutamine |
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