CN110283219B - Preparation method of sialic acid crystal - Google Patents
Preparation method of sialic acid crystal Download PDFInfo
- Publication number
- CN110283219B CN110283219B CN201910588753.1A CN201910588753A CN110283219B CN 110283219 B CN110283219 B CN 110283219B CN 201910588753 A CN201910588753 A CN 201910588753A CN 110283219 B CN110283219 B CN 110283219B
- Authority
- CN
- China
- Prior art keywords
- drying
- crystal
- sialic acid
- microwave
- crystallization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H7/00—Compounds containing non-saccharide radicals linked to saccharide radicals by a carbon-to-carbon bond
- C07H7/02—Acyclic radicals
- C07H7/033—Uronic acids
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to the field of medicine preparation, in particular to a preparation method of sialic acid crystals, which comprises the step of drying wet crystals obtained after crystallizing a sialic acid extracting solution, wherein the drying is vacuum microwave drying, the drying temperature is 30-80 ℃, the vacuum degree is not more than-0.08 MPa, and the microwave time is 35-150mins. By the method, free water and bound water in the sialic acid crystal are effectively removed on the basis of not influencing the crystal structure and ensuring the crystal quality, so that the water content in the final product can be less than 2%, the crystal content can reach 98-99.5%, the whiteness of the product is over 90, and the method can be widely applied to multiple fields of medicines, cosmetics, health products, infant food and the like. The method has the advantages of simple operation, low cost, clean production and no environmental pollution; and the drying time is short, the energy consumption is low, the large-scale production is easy, and the investment return is high.
Description
Technical Field
The invention relates to the field of medicine preparation, in particular to a preparation method of a sialic acid crystal.
Background
In the prior art, the problem of crystal moisture removal of sialic acid in the preparation process is always difficult to solve. In fact, in the course of our research, many drying methods have been tried, but it is very difficult to reduce the moisture content below 2% anyway using ordinary vacuum drying.
Due to uneven heating, the local overheating phenomenon can occur in spray drying, and the color and whiteness of the product are reduced to some extent; the time and energy consumption for freeze drying are too long, and the ideal effect is still not achieved; the water content was around 10% using a common drying method, as demonstrated in CN 109293612A.
CN 104046671A proposes a method for producing sialic acid by fermentation, wherein sialic acid (N-acetylneuraminic acid) crystal is vacuum freeze-dried to obtain product with purity of 94.8%. The method has high requirements on vacuum degree and temperature, high energy consumption, high final water content of the product and low purity, and can not meet the market requirements.
If an organic solvent dehydration method is adopted, such as shown in CN109265497A and CN 104628794A, the dihydrate is dehydrated into N-acetylneuraminic acid in ethanol, so that the purity of the product can be improved and the content of bound water can be reduced, but the method has the problems that the organic solvent is introduced into the finished product, the obtained wet crystal needs to be dehydrated by absolute ethanol, the treatment process is increased, the cost is increased, and a subsequent ethanol recovery system is also considered. And the subsequent vacuum drying oven is used for drying the product, so that the product drying time is longer and the energy consumption is higher.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method which can conveniently and efficiently improve the purity of sialic acid crystals and reduce the content of bound water on the basis of ensuring the quality of the crystals.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for preparing sialic acid (N-acetylneuraminic acid or SA) crystal comprises crystallizing sialic acid extractive solution, and drying wet crystal at 30-80 deg.C under vacuum of-0.08 MPa for 35-150mins.
Compared with other drying methods in the prior art, the vacuum microwave drying method for the SA crystals can efficiently reduce the water content of the crystals without introducing other substances, has uniform microwave drying effect, and can reduce the damage to the quality of the crystals.
Preferably, the vacuum microwave drying is divided into a first step microwave drying and a second step microwave drying, wherein the first step microwave drying comprises: setting the temperature at 50-80 deg.c, the vacuum degree not higher than-0.08 MPa and the microwave time at 15-60mins;
further preferably, the temperature is 65-75 ℃, and the microwave time is 20-45mins;
further preferably, the microwave power is 500-1000W.
Preferably, the second step of microwave drying: setting the temperature at 30-60 deg.c, the vacuum degree not higher than-0.08 MPa and the microwave time at 20-90mins;
further preferably, the temperature is 45-55 ℃, and the microwave time is 30-50mins;
further preferably, the microwave power is 200-500W.
Preferably, the moisture content of the wet crystals after the first microwave drying step is 3-8%.
In research and development, the invention discovers that aiming at the sialic acid crystal, free water and bound water in the crystal can be well removed by the step-by-step microwave drying method on the basis of not influencing the crystal structure and ensuring the crystal quality, other organic solvents are not required to be introduced in the process, the drying time is short, and the whole process is convenient and efficient.
Preferably, before drying, the moisture of the wet crystal is controlled to be 20-50%; preferably 20-30%.
Through controlling the moisture content of the wet crystal in the range before microwave drying, the time (about 10 mins-30 mins) of the first step of microwave drying can be controlled more reasonably, the influence of overlong microwave treatment on the crystal quality is avoided, and the finally prepared crystal quality can be further improved while the microwave drying effect is ensured, and the drying efficiency is improved.
Preferably, the drying is carried out by the step (1) until the crystal moisture is 4.5 to 5.3%.
The first microwave drying step is stopped under the moisture content, so that the drying effect and the crystal quality can be better ensured.
Preferably, the crystals are dried by the step (3) to have a moisture content of less than 2%, more preferably less than 1%.
When the water content of the crystal is in the range, the second step of microwave drying can be stopped, the SA crystal content is 98-99.5%, the whiteness of the product is above 90, the performance is excellent, the influence on the water content of the crystal is small by continuing the microwave drying, and the quality of the crystal is possibly influenced.
Preferably, the particle size of the semi-finished product is less than 60 mesh, preferably 100-200 mesh, before the second drying step.
The method for making the particle size of the semi-finished product less than 60 mesh can adopt crushing equipment such as a mechanical crusher, a jet mill, a cryogenic crusher, a ball mill and the like, and in the embodiment, the mechanical crusher is selected to crush the semi-finished product for the sake of cost and process convenience.
Preferably, the sialic acid extractive solution is one or more of sialic acid monomer extractive solution obtained by fermentation, sialic acid extractive solution obtained by hydrolysis after polysialic acid is obtained by fermentation, sialic acid extractive solution obtained by nidus Collocaliae extraction, and sialic acid extractive solution obtained by enzymatic synthesis.
Wherein the sialic acid monomer extracting solution prepared by fermentation is a sialic acid monomer-containing fermentation liquid prepared by microbial fermentation, and the sialic acid extracting solution is obtained by extraction and purification steps;
hydrolyzing after fermentation to obtain polysialic acid to obtain a sialic acid extracting solution, wherein the sialic acid extracting solution is a fermentation liquid containing polysialic acid obtained by microbial fermentation, and the sialic acid extracting solution is obtained by hydrolysis, extraction and purification steps;
the sialic acid extracting solution extracted from the cubilose is obtained by hydrolyzing natural cubilose by an enzyme or chemical means, and then extracting and purifying;
the sialic acid extract obtained by enzymatic synthesis is a sialic acid extract obtained by catalytic enzymatic synthesis in a system containing one or more enzymes of sialic acid aldolase, sialic acid synthetase and sialic acid kinase, and further extracting and purifying.
Preferably, before the crystallization, the concentration of the sialic acid extracting solution is controlled to be 300-600g/L; preferably 400 to 500g/L.
Preferably, the pH of the sialic acid extract is adjusted to 0.1 to 2 during the crystallization; preferably 0.9 to 1.2.
The pH adjuster is preferably hydrochloric acid, sulfuric acid, nitric acid, or the like, and more preferably hydrochloric acid.
Preferably, the crystallization temperature is from 0 to 10 ℃ and preferably from 0 to 4 ℃.
Preferably, the stirring speed for crystallization is 10 to 100rpm/min, preferably 50 to 70rpm/min.
Preferably, the crystallization time is from 4 to 20 hours, preferably from 14 to 15 hours.
When the crystallization is carried out under the above conditions (a better scheme can be obtained by optimizing the combination of the conditions), the content of the combined water in the crystals can be further controlled, so that the treatment effect of the microwave drying on the combined water is improved, and the quality of the prepared SA crystals is further improved.
As a preferable embodiment of the present invention, the method for producing a sialic acid crystal of the present invention comprises the steps of:
s1, crystallization: controlling the concentration of sialic acid extractive solution at 300-600g/L, adjusting pH to 0.1-2, crystallizing at 0-10 deg.C, stirring at 10-100rpm/min for 4-20 hr to obtain crude crystal;
s2, purification: and (3) centrifuging the coarse crystal at 4000-10000rpm/min for 20-60mins, washing for 30-60mins, and centrifuging at 4000-10000rpm/min to ensure that the water content of the crystal is 20% -50%.
S3, drying:
s3a, first-step microwave drying: setting the temperature at 50-80 deg.C, the vacuum degree at not more than-0.08 MPa, and the microwave time at 15-60mins, and drying the wet crystal until the water content is 3-8%; further preferable microwave power is 500-1000W;
s3b, crushing the semi-finished product obtained in the S3a to obtain powder with the particle size smaller than 60 meshes;
s3c, second-step microwave drying: and (3) drying the crushed crystal obtained in the step (S3 b) at the set temperature of 30-60 ℃, the vacuum degree of not more than-0.08 MPa and the microwave time of 20-90 mins. Further preferred microwave power is 200W-500W.
The invention has the following beneficial effects:
(1) The invention effectively removes free water and bound water in the sialic acid crystal by a microwave drying method on the basis of not influencing the crystal structure and ensuring the crystal quality. The water content in the final product can be lower than 2 percent and further lower than 1 percent by a step-by-step microwave drying method, so that the crystal content can reach 98-99.5 percent, the whiteness of the product is ensured to be more than 90 percent, and the method can be widely applied to a plurality of fields of medicines, cosmetics, health products, infant food and the like.
(2) The method has the advantages of simple operation, low cost, clean production and no environmental pollution; and the drying time is short, the energy consumption is low, the large-scale production is easy, and the investment return is high.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
A method for preparing a sialic acid crystal, comprising the steps of:
s1, crystallization: preparing a fermentation liquor containing sialic acid monomers by fermentation, extracting to obtain a sialic acid extracting solution, controlling the concentration of the sialic acid extracting solution to be 450g/L, adjusting the pH value to be 1, controlling the crystallization temperature to be 4 ℃, controlling the crystallization stirring speed to be 60rpm/min, and controlling the crystallization time to be 16 hours to obtain a crude crystal;
s2, purification: and centrifuging the crude crystal at 10000rpm/min for 20mins, washing for 30mins, and centrifuging at 10000rpm/min for 20mins to ensure that the water content of the crystal is 20%.
S3, drying:
s3a, first-step microwave drying: setting the temperature at 70 ℃, the vacuum degree at-0.1 MPa, the microwave power at 1000W and the time at 25mins, and drying the wet crystal until the moisture content is 5%;
s3b, crushing the semi-finished product obtained in the S3a to 100 meshes;
s3c, second-step microwave drying: and setting the temperature to be 50 ℃, the vacuum degree to be-0.08 MPa and the microwave power to be 400W, and drying the crushed crystal obtained in the step S3b for 40mins.
The obtained crystal has water content of 0.5%, crystal content of 99.2%, and whiteness of 92.5
Example 2
A method for preparing a sialic acid crystal, comprising the steps of:
s1, crystallization: hydrolyzing after preparing polysialic acid by fermentation to obtain a sialic acid extracting solution, controlling the concentration of the sialic acid extracting solution to be 600g/L, adjusting the pH value to be 2, controlling the crystallization temperature to be 10 ℃, controlling the crystallization stirring speed to be 100rpm/min, and controlling the crystallization time to be 4 hours to obtain a crude crystal;
s2, purification: and centrifuging the crude crystals at 4000rpm/min for 60mins, washing for 60mins, and centrifuging at 4000rpm/min for 60mins to ensure that the water content of the crystals is 30%.
S3, drying:
s3a, first-step microwave drying: setting the temperature at 80 ℃, the vacuum degree at-0.08 MPa, the microwave power at 1000W and the time at 15mins, and drying the wet crystal until the water content is 3 percent;
s3b, crushing the semi-finished product obtained in the S3a to 80 meshes;
s3c, second-step microwave drying: and setting the temperature to be 60 ℃, the vacuum degree to be-0.08 MPa and the microwave power to be 500W, and drying the crushed crystal obtained in the step S3b for 20mins.
The obtained crystal has the water content of 1.2 percent, the crystal content of 98.3 percent and the whiteness of the product of 93.7.
Example 3
A method for preparing a sialic acid crystal, comprising the steps of:
s1, crystallization: extracting sialic acid extract from nidus Collocaliae, controlling the concentration of sialic acid extract at 300g/L, adjusting pH to 0.1, crystallizing at 0 deg.C, stirring at 10rpm/min for 20 hr to obtain coarse crystal;
s2, purification: and centrifuging the crude crystal for 20mins at 10000pm/min, washing for 30mins, and centrifuging for 20mins at 10000rpm/min to ensure that the water content of the crystal is 25%.
S3, drying:
s3a, first-step microwave drying: setting the temperature at 50 ℃, the vacuum degree at-0.1 MPa, the microwave power at 500W and the time at 50mins, and drying the wet crystal until the moisture content is 8%;
s3b, crushing the semi-finished product obtained in the S3a to 60 meshes;
s3c, second-step microwave drying: and setting the temperature to be 30 ℃, the vacuum degree to be-0.1 MPa and the microwave power to be 200W, and drying the crushed crystal obtained in the step S3b for 60mins.
The obtained crystal has the water content of 1.7 percent, the crystal content of 98.0 percent and the whiteness of the product of 95.1.
Example 4
A method for preparing a sialic acid crystal, comprising the steps of:
s1, crystallization: synthesizing a sialic acid extracting solution through enzyme catalysis, controlling the concentration of the sialic acid extracting solution to be 400g/L, adjusting the pH value to be 0.1, controlling the crystallization temperature to be 0 ℃, controlling the crystallization stirring speed to be 10rpm/min, and controlling the crystallization time to be 20 hours to obtain a crude crystal;
s2, purification: and centrifuging the crude crystal at 8000pm/min for 30mins, washing for 40mins, and centrifuging at 8000rpm/min for 30mins to reach the crystal moisture content of 22%.
S3, drying:
s3a, first-step microwave drying: setting the temperature at 75 ℃, the vacuum degree at-0.08 MPa, the microwave power at 800W and the time at 20mins, and drying the wet crystal until the moisture content is 7%;
s3b, crushing the semi-finished product obtained in the S3a to 200 meshes;
s3c, second-step microwave drying: and setting the temperature to be 55 ℃, the vacuum degree to be-0.08 MPa and the microwave power to be 300W, and drying the crushed crystal obtained in the step S3b for 50mins.
The obtained crystal has the water content of 0.7 percent, the crystal content of 99 percent and the whiteness of 92.5 products.
Example 5
A method for preparing a sialic acid crystal, comprising the steps of:
s1, crystallization: hydrolyzing and extracting polysialic acid to obtain a sialic acid extracting solution, controlling the concentration of the sialic acid extracting solution to be 450g/L, adjusting the pH value to be 0.1, controlling the crystallization temperature to be 0 ℃, controlling the crystallization stirring speed to be 10rpm/min, and controlling the crystallization time to be 20 hours to obtain a crude crystal;
s2, purification: and centrifuging the crude crystal for 45mins at 5000pm/min, washing for 30mins, and centrifuging at 6000rpm/min for 20mins to ensure that the water content of the crystal is 23%.
S3, drying:
s3a, first-step microwave drying: setting the temperature at 65 ℃, the vacuum degree at-0.08 MPa, the microwave power at 1000W and the time at 45mins, and drying the wet crystal until the moisture content is 6.5 percent;
s3b, crushing the semi-finished product obtained in the S3a to 100 meshes;
s3c, second-step microwave drying: and setting the temperature to be 45 ℃, the vacuum degree to be-0.08 MPa and the microwave power to be 500W, and drying the crushed crystal obtained in the step S3b for 50mins.
The obtained crystal has the water content of 0.3 percent, the crystal content of 99.5 percent and the whiteness of the product of 93.1.
Example 6
A method for preparing a sialic acid crystal, comprising the steps of:
s1, crystallization: hydrolyzing and extracting polysialic acid to obtain a sialic acid extracting solution, controlling the concentration of the sialic acid extracting solution to be 450g/L, adjusting the pH value to be 0.1, the crystallization temperature to be 0 ℃, and the crystallization time to be 20 hours to obtain a crude crystal;
s2, purification: and centrifuging the crude crystal for 45mins at 5000pm/min, washing for 30mins, and centrifuging at 6000rpm/min for 20mins to ensure that the water content of the crystal is 23%.
S3, drying:
s3a, first-step microwave drying: setting the temperature at 65 ℃, the vacuum degree at-0.09 MPa, the microwave power at 1000W and the time at 45mins, and drying the wet crystal until the moisture content is 6.5%;
s3b, crushing the semi-finished product obtained in the S3a to 100 meshes;
s3c, second-step microwave drying: and setting the temperature to be 45 ℃, the vacuum degree to be-0.09 MPa and the microwave power to be 500W, and drying the crushed crystal obtained in the step S3b for 50mins.
The obtained crystal has the water content of 0.9 percent, the crystal content of 98.5 percent and the whiteness of 90 percent.
Example 7
This example differs from example 1 in that: the steps S3b and S3c are removed, and 40mins are processed under the condition of the step S3 a.
The crystal obtained had a moisture content of 3.1%, but due to prolonged exposure to high energy conditions, local overheating of the crystal destroyed sialic acid, the crystal content was 96.2%, and the product whiteness was 80%.
Example 8
The present example differs from example 1 in that: stopping the first microwave drying step when the water content of the crystal is 10%; the second step of microwave drying is carried out until the rate of decrease of the moisture content is less than 0.1% per half hour (the moisture content is not substantially affected any more).
It took 3 hours for the crystal to have a moisture content of 2%, but the local overheating of the crystal due to the long microwave destroyed the sialic acid structure, the crystal content was 97.1%, and the product whiteness was 78.
Example 9
This example differs from example 1 in the drying step:
s3, drying:
s3a, first-step microwave drying: setting the temperature at 50 ℃, the vacuum degree above-0.08 MPa, the microwave power at 600W and the time at 80mins, and drying the wet crystal until the water content is 10 percent;
s3b, crushing the semi-finished product obtained in the S3a to 100 meshes;
s3c, second-step microwave drying: and setting the temperature to be 50 ℃, the vacuum degree to be more than minus 0.08MPa and the microwave power to be 400W, and drying the crushed crystal obtained in the step S3b for 45mins.
The obtained crystal has the water content of 2.3 percent, the crystal content of 96.7 percent and the whiteness of the product of 85 percent.
Example 10
This example differs from example 1 in the drying step:
s3, drying:
s3a, first-step microwave drying: setting the temperature at 70 ℃, the vacuum degree at-0.1 MPa, the microwave power at 1000W and the time at 25mins, and drying the wet crystal until the water content is 5%;
s3b, crushing the semi-finished product obtained in the S3a to 100 meshes;
s3c, second-step microwave drying: and setting the temperature to be 35 ℃, the vacuum degree to be-0.08 MPa and the microwave power to be 400W, and drying the crushed crystal obtained in the step S3b for 125mins.
The obtained crystal has the water content of 1.7 percent, the crystal content of 97.1 percent and the whiteness of the product of 90 percent.
Example 11
This example differs from example 1 in that after the purification washing step before drying, direct filtration gives wet crystals with a moisture content of 60%.
The obtained crystal has the water content of 2.6 percent, the crystal content of 96.0 percent and the whiteness of the product of 92 percent.
After 150mins, the water content of the product is reduced at a rate of less than 0.1% per half hour, at which time the crystal water content is 2.2%, the crystal content is 96.9%, and the whiteness of the product is 83.
Comparative example 1
The present example differs from example 1 in that: the drying step is carried out at the temperature of 25 ℃, the vacuum degree of-0.1 MPa and the power of 200W, and the water content reduction speed is less than 0.05 percent per half hour after drying for 200 mins.
The obtained crystal has the water content of 10.3 percent, the crystal content of 87.5 percent and the whiteness of 92 percent.
Comparative example 2
This example differs from example 1 in that: the drying step is that the water content is reduced by less than 0.05 percent per half hour after drying for 30mins at the temperature of 100 ℃, the vacuum degree of-0.1 MPa and the power of 1200W.
The obtained crystal has the water content of 1.4 percent, the crystal content of 96.5 percent and the whiteness of 78 percent.
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, it is intended that all such modifications and alterations be included within the scope of this invention as defined in the appended claims.
Claims (10)
1. A process for producing a sialic acid crystal, which comprises crystallizing a sialic acid extract solution, and drying the resulting wet crystal,
before drying, controlling the moisture of the wet crystal to be 20-50%;
the drying is vacuum microwave drying; the vacuum microwave drying is divided into a first microwave drying step and a second microwave drying step,
wherein, the first step of microwave drying: setting the temperature to be 50-80 ℃, the vacuum degree to be not more than-0.08 MPa, the microwave power to be 500-1000W and the microwave time to be 15-60mins; after the first step of microwave drying, the moisture content of the wet crystal is 3-8%;
and the second step of microwave drying: setting the temperature at 30-60 ℃, the vacuum degree at not more than-0.08 MPa, the microwave power at 200-500W and the microwave time at 20-90mins;
before the second step of microwave drying, the grain diameter of the semi-finished product is less than 60 meshes.
2. The method of claim 1, wherein the wet crystals are controlled to have a moisture content of 20-30% prior to drying.
3. The method of claim 1, wherein the semi-finished product has a particle size of 100 to 200 mesh before the second microwave drying step.
4. The method according to claim 1, wherein the sialic acid extractive solution is one or more selected from the group consisting of a sialic acid monomer extractive solution obtained by fermentation, a sialic acid extractive solution obtained by hydrolysis after polysialic acid is obtained by fermentation, a sialic acid extractive solution obtained by extraction from bird's nest, and a sialic acid extractive solution obtained by enzymatic synthesis.
5. The method according to claim 1, wherein the pH of the sialic acid extract is adjusted to 0.1 to 2 during the crystallization.
6. The method according to claim 5, wherein the pH of the sialic acid extract is adjusted to 0.9 to 1.2 during the crystallization.
7. The process according to claim 1, wherein the crystallization temperature is 0-10 ℃.
8. The process according to claim 7, wherein the crystallization temperature is 0 to 4 ℃.
9. The method of claim 1, wherein the crystallization agitation speed is 10 to 100rpm/min.
10. The method according to claim 9, wherein the stirring speed for crystallization is 50 to 70rpm/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910588753.1A CN110283219B (en) | 2019-07-02 | 2019-07-02 | Preparation method of sialic acid crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910588753.1A CN110283219B (en) | 2019-07-02 | 2019-07-02 | Preparation method of sialic acid crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110283219A CN110283219A (en) | 2019-09-27 |
| CN110283219B true CN110283219B (en) | 2023-03-24 |
Family
ID=68021657
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910588753.1A Active CN110283219B (en) | 2019-07-02 | 2019-07-02 | Preparation method of sialic acid crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110283219B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113416222B (en) * | 2021-07-01 | 2023-06-20 | 嘉必优生物技术（武汉）股份有限公司 | Sialic acid particles and preparation method thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104628794A (en) * | 2015-03-10 | 2015-05-20 | 武汉中科光谷绿色生物技术有限公司 | Method for separating and purifying N-acetylneuraminic acid produced by microbiological fermentation |
| CN106173612A (en) * | 2015-04-24 | 2016-12-07 | 燕凰国际有限公司 | Instant brewing cubilose and preparation method thereof |
| CN106366136A (en) * | 2016-08-03 | 2017-02-01 | 江南大学 | Sialic acid, and preparation method and application thereof |
| CN106418490A (en) * | 2015-08-10 | 2017-02-22 | 江苏布诺堂健康生物科技有限公司 | Remodeled fast bird's nest and preparation method thereof |
| CN106748848A (en) * | 2016-11-23 | 2017-05-31 | 无锡晶海氨基酸股份有限公司 | A kind of technique for preparing branched-chain amino acid and its application |
| CN106883274A (en) * | 2015-12-15 | 2017-06-23 | 中科鸿基生物科技有限公司 | Sialic acid process for purification |
| CN108003202A (en) * | 2017-11-28 | 2018-05-08 | 广西佛斯肽生物科技有限公司 | A kind of method that Sialic acid is extracted from bird's nest |
| CN108902941A (en) * | 2018-06-28 | 2018-11-30 | 燕生（福建）生物工程有限公司 | A method of extracting Sialic acid from bird's nest |
| CN109180745A (en) * | 2018-11-16 | 2019-01-11 | 武汉中科光谷绿色生物技术有限公司 | A method of separating-purifying prepares N-acetyl-neuraminate from the material containing poly sialic acid |
| CN109627269A (en) * | 2018-11-16 | 2019-04-16 | 武汉中科光谷绿色生物技术有限公司 | A method of extracting N-acetyl-neuraminate |
-
2019
- 2019-07-02 CN CN201910588753.1A patent/CN110283219B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104628794A (en) * | 2015-03-10 | 2015-05-20 | 武汉中科光谷绿色生物技术有限公司 | Method for separating and purifying N-acetylneuraminic acid produced by microbiological fermentation |
| CN106173612A (en) * | 2015-04-24 | 2016-12-07 | 燕凰国际有限公司 | Instant brewing cubilose and preparation method thereof |
| CN106418490A (en) * | 2015-08-10 | 2017-02-22 | 江苏布诺堂健康生物科技有限公司 | Remodeled fast bird's nest and preparation method thereof |
| CN106883274A (en) * | 2015-12-15 | 2017-06-23 | 中科鸿基生物科技有限公司 | Sialic acid process for purification |
| CN106366136A (en) * | 2016-08-03 | 2017-02-01 | 江南大学 | Sialic acid, and preparation method and application thereof |
| CN106748848A (en) * | 2016-11-23 | 2017-05-31 | 无锡晶海氨基酸股份有限公司 | A kind of technique for preparing branched-chain amino acid and its application |
| CN108003202A (en) * | 2017-11-28 | 2018-05-08 | 广西佛斯肽生物科技有限公司 | A kind of method that Sialic acid is extracted from bird's nest |
| CN108902941A (en) * | 2018-06-28 | 2018-11-30 | 燕生（福建）生物工程有限公司 | A method of extracting Sialic acid from bird's nest |
| CN109180745A (en) * | 2018-11-16 | 2019-01-11 | 武汉中科光谷绿色生物技术有限公司 | A method of separating-purifying prepares N-acetyl-neuraminate from the material containing poly sialic acid |
| CN109627269A (en) * | 2018-11-16 | 2019-04-16 | 武汉中科光谷绿色生物技术有限公司 | A method of extracting N-acetyl-neuraminate |
Non-Patent Citations (1)
| Title |
|---|
| 中药提取物的微波真空干燥工艺研究;梁新丽等;《中成药》;20100620(第06期);92-100 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110283219A (en) | 2019-09-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106282266B (en) | Method for preparing enteromorpha prolifera oligosaccharide by using naringinase | |
| CN110283219B (en) | Preparation method of sialic acid crystal | |
| CN103766531B (en) | Prepare the method for high gamma-aminobutyric acid instant tea | |
| CN106579443A (en) | Method for extracting anthocyanin from mulberries | |
| CN103923140A (en) | Preparation method of acetylisovaleryltylosin tartrate | |
| CN104357518A (en) | Method for preparing nucleotide from waste beer yeast | |
| CN111978430A (en) | Preparation method of oat beta-glucan | |
| CN103804172B (en) | A kind of method improving organic acid production quality | |
| CN108048495B (en) | Biological extraction method of resveratrol | |
| WO2023134467A1 (en) | Method for preparing starch and non-thermal-denaturation protein powder by using rice as raw material | |
| CN103275047B (en) | Preparation method of griseofulvin | |
| CN104629967A (en) | Saccharification technology for brewing beer | |
| CN1281900A (en) | Extraction method of abamectin | |
| CN108997331B (en) | Process for extracting berberine from phellodendron based on enzyme method | |
| CN101891774B (en) | Production process of rhamnose | |
| CN108047288B (en) | Preparation method of geniposide | |
| CN110384195B (en) | Rice bran fresh-keeping method | |
| CN107778160B (en) | Preparation method of 3,4,5, 6-tetrafluorophthalic acid | |
| CN102040597A (en) | Improved production method of aztreonam | |
| CN107686853B (en) | Method for preparing ultrahigh maltose syrup by multi-enzyme method | |
| CN106543264B (en) | Method for multi-layer separation and component refining of biological components of caragana microphylla of leguminosae | |
| KR20080085377A (en) | Method for preparing l-ornithine salts | |
| CN110092729B (en) | Crystallization method of L-lysine hydrochloride | |
| CN109096275A (en) | A kind of hyoscine supercritical extraction process | |
| CN1314337A (en) | Method for producing 3,4,5 trimethoxybenzoic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |