CN115626958A - Method for separating edible fungus polysaccharide based on silicon carbide ceramic membrane technology and application - Google Patents

Method for separating edible fungus polysaccharide based on silicon carbide ceramic membrane technology and application Download PDF

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CN115626958A
CN115626958A CN202211258352.8A CN202211258352A CN115626958A CN 115626958 A CN115626958 A CN 115626958A CN 202211258352 A CN202211258352 A CN 202211258352A CN 115626958 A CN115626958 A CN 115626958A
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silicon carbide
carbide ceramic
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polysaccharide
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郭庆彬
康继
李欣雪
王书军
王昌禄
胡新中
邵严辉
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Tianjin University of Science and Technology
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    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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Abstract

The invention discloses a method for separating edible fungus polysaccharide based on a silicon carbide ceramic membrane technology, which comprises the following steps: and (3) placing the supernatant of the water extract of the colloidal edible fungi leached by hot water into a feeding tank of the silicon carbide ceramic membrane, concentrating the feed liquid through cyclic concentration in the membrane process, then adding deionized water to wash and filter the feed liquid, and repeating for many times to finally obtain the relatively pure crude sugar of the colloidal edible fungi. The edible colloid fungus obtained by the method has low protein content, high total sugar content and high pigment removal rate. The method for separating the colloidal edible fungus polysaccharide by using the silicon carbide ceramic membrane has the advantages of simple operation, short separation period, high efficiency, low cost, less organic reagent consumption, greenness and environmental protection, and is suitable for industrial production of the colloidal edible fungus polysaccharide.

Description

Method for separating edible fungus polysaccharide based on silicon carbide ceramic membrane technology and application
Technical Field
The invention belongs to the technical field of polysaccharide extraction, and particularly relates to a method for separating edible fungus polysaccharide based on a silicon carbide ceramic membrane technology, and an application of the method.
Background
The edible fungi polysaccharide has various functional characteristics and biological activity. Domestic edible fungus industries are distributed in many places, have wide range and variety and have great development potential. The polysaccharide is one of the key bioactive components of black fungus, auricularia, and Tremella. The three edible fungi colloidal polysaccharides have various biological activities and pharmacological potentials, such as antioxidation, anti-tumor, blood sugar reduction, hypocholesterolemia, immunity improvement and the like. Meanwhile, the colloid edible fungi has good viscosity and gel characteristics, and can be used as a gelling agent and a thickening agent of food. In addition, the colloidal edible fungus polysaccharide can be used as a good prebiotic source, can simulate the texture of fat, and can generate beneficial health effects when combined with a suitable food.
The membrane technology for separating the edible colloid fungus polysaccharide mainly utilizes a screening mechanism to classify the polysaccharides with different molecular weights, selects reserved products according to requirements, and simultaneously removes non-target products with small molecular weights, such as salt contained in an original sample. The membrane technology can be used for separating and purifying biological products such as nutrient substances and active biological macromolecules. Because the membrane separation technology has the advantages of high efficiency and energy saving, the membrane separation technology is tried to replace the traditional alcohol precipitation technology in the production of the traditional Chinese medicine. The membrane separation has the advantages of no phase change, low energy consumption, simple and convenient operation, good selectivity and the like, and particularly has good selectivity to various potential active substances.
The colloid edible fungus polysaccharide is separated by using a membrane separation technology, so that the period, the steps, the organic reagent dosage and the like of the preparation process of the colloid edible fungus polysaccharide can be reduced, and the effects of high efficiency, energy conservation, environmental friendliness are achieved in the production process of the polysaccharide. Membrane separation techniques for separation of polysaccharides utilize pressure-driven processes. The polysaccharide sample solution can be purified and concentrated without causing thermal damage to the sample, without consuming energy for phase transition, and without containing harmful organic solvents. The device has the advantages of good mobility, simple structure, small requirement on space equipment and the like.
At present, most of the prior art adopts ethanol precipitation method or salting-out method to separate polysaccharide, but the prior art has the following defects:
1. the separation of polysaccharides can be achieved by ethanol precipitation. Adding ethanol with different concentrations into the concentrated water extract to obtain polysaccharides with different molecular weights.
However, it is generally difficult to obtain uniform polysaccharides by ethanol precipitation, and a large amount of protein is precipitated during ethanol precipitation, resulting in a mixture of components of the polysaccharide product, and the color of the polysaccharide sample obtained from a darker raw material is generally darker. The dialysis time is long and the process of extraction from the polysaccharide to the separation takes a lot of time.
2. The separation of polysaccharides can be achieved by salting out. In the salting-out method, ammonium sulfate is generally used as a salting-out agent, and polysaccharides of different components are separated out by utilizing the difference in solubility of the polysaccharides of different components in a salt solution.
Although the salting-out method can precipitate the polysaccharide, the salting-out method requires high conditions and is difficult to control, for example, the pH and temperature of the salt solution and the concentration of the polysaccharide solution need to be controlled in time. Meanwhile, dialysis is carried out for a long time after separation is finished, and the period is long.
Therefore, there is a need for new methods for isolating one or more polysaccharides.
Through searching, no patent publication related to the present patent application has been found.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method and application for separating edible fungus polysaccharide based on a silicon carbide ceramic membrane technology.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for separating edible fungus polysaccharide based on a silicon carbide ceramic membrane technology comprises the following steps:
rinsing the colloid edible fungi with running water, washing off impurities on the surface, putting the wiped sample into a blast oven for drying at 80 ℃, crushing the dried sample, and sieving with a 60-mesh sieve; sieving powder of colloid edible fungi and deionized water according to the mass ratio of feed liquid of 1:100, leaching for 2-2.5h at 95 ℃, centrifuging to obtain a supernatant, centrifuging and precipitating to repeat the leaching operation, combining the supernatants, and performing suction filtration to remove impurities to obtain an extracting solution for later use;
the obtained extracting solution is taken as a raw material solution, the extracting solution is placed in a silicon carbide ceramic membrane, the interior of the silicon carbide ceramic membrane is ensured to be in an isolated state with the external environment, impurities are prevented from entering, the first step of membrane separation, namely concentration, is carried out under the pressure of 0-0.5 MPa, and when the volume of the raw material solution is concentrated to 1/5 of the original volume; adding deionized water with 5 times of volume to wash and filter under the pressure of 0-0.5 MPa, washing and filtering to 1/5 of the original volume, repeating for 5 times, and finally concentrating the volume of the raw material liquid to 1/10 of the volume of the original raw material liquid; and (4) carrying out vacuum freeze drying on the trapped fluid to obtain the polysaccharide separated by the membrane.
Further, the diameter of the silicon carbide ceramic membrane is
Figure BDA0003890319150000021
Further, the colloid edible fungi are black fungus sporophore, auricularia fuscosuccinea sporophore and tremella sporophore.
Furthermore, the raw material liquid is placed in a raw material tank of the silicon carbide ceramic membrane separation equipment, and an inlet of the raw material liquid tank is sealed by a preservative film, so that the interior of the container is kept in an isolated state from the external environment.
The edible fungus polysaccharide colloid obtained by the method.
The method is applied to the separation of the edible fungi polysaccharide.
The invention has the advantages and positive effects that:
1. the method can improve the efficiency of preparing the edible fungus polysaccharide by the edible fungus and shorten the production period of the edible fungus polysaccharide.
2. The method can remove most of protein in the washing and filtering process while improving the production efficiency of the edible fungi polysaccharide with colloid, thereby playing a role in purifying products.
3. The method can reduce the use amount of organic solvent in the polysaccharide extraction process, and is environment-friendly and green in production.
4. The silicon carbide ceramic membrane used in the method has the advantages of excellent oxidation resistance, wear resistance, high temperature and high pressure resistance, acid and alkali corrosion resistance, heat and shock resistance, repeated utilization and long service life, and the polysaccharide concentrated solution does not have phase change.
5. The edible colloid fungus obtained by the method has low protein content and high total sugar content. The method for separating the colloidal edible fungus polysaccharide by using the silicon carbide ceramic membrane has the advantages of simple operation, short separation period, high efficiency, low cost, less organic reagent consumption, greenness and environmental protection, and is suitable for industrial production of the colloidal edible fungus polysaccharide.
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FIG. 1 is a flow chart of a production process of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
The various experimental procedures described in the specific examples are conventional in the art and are not specifically described herein, and one of ordinary skill in the art can refer to various conventional tool books, scientific literature, or related specifications, manuals, etc. before the filing date of the present application.
The silicon carbide ceramic membrane equipment is the prior art, can be silicon carbide ceramic membrane separation equipment DJM-01-1*2/1200, and is purchased from Hubei Dijie membrane science and technology, inc.
A method for separating edible fungus polysaccharide based on a silicon carbide ceramic membrane technology comprises the following steps:
flushing the colloid edible fungi with running water, washing off impurities on the surface, putting the wiped sample into a blast oven for drying at 80 ℃, crushing the dried sample, and sieving with a 60-mesh sieve; sieving powder of colloid edible fungi and deionized water according to the mass ratio of feed liquid of 1:100, leaching for 2-2.5h at 95 ℃, centrifuging to obtain a supernatant, centrifuging and precipitating to repeat the leaching operation, combining the supernatants, and performing suction filtration to remove impurities to obtain an extracting solution for later use;
the obtained extracting solution is taken as a raw material solution, the extracting solution is placed in a silicon carbide ceramic membrane, the interior of the silicon carbide ceramic membrane is ensured to be in an isolated state with the external environment, impurities are prevented from entering, the first step of membrane separation, namely concentration, is carried out under the pressure of 0-0.5 MPa, and when the volume of the raw material solution is concentrated to 1/5 of the original volume; adding 5 times of deionized water for washing and filtering under the pressure of 0-0.5 MPa, washing and filtering to 1/5 of the original volume, repeating for 5 times, and finally concentrating the volume of the raw material liquid to 1/10 of the volume of the original raw material liquid; and (4) carrying out vacuum freeze drying on the trapped fluid to obtain the polysaccharide separated by the membrane.
Preferably, the diameter of the silicon carbide ceramic film is
Figure BDA0003890319150000031
Preferably, the colloid edible fungi are black fungus sporophore, auricularia fuscosuccinea sporophore and tremella sporophore.
Preferably, the raw material liquid is placed in a raw material tank of the silicon carbide ceramic membrane separation equipment, and an inlet of the raw material liquid tank is sealed by a preservative film, so that the interior of the container is kept in an isolated state from the external environment.
The edible fungus polysaccharide colloid obtained by the method.
The method is applied to the separation of the edible fungi polysaccharide.
Specifically, the preparation and detection are as follows:
example 1
A method for separating edible fungus polysaccharide based on a silicon carbide ceramic membrane technology comprises the following steps:
rinsing the colloid edible fungus black fungus sporocarp with running water, washing off impurities on the surface, putting the wiped sample into a blast oven for drying at 80 ℃, crushing the dried sample, and sieving with a 60-mesh sieve.
Weighing 5L of deionized water, weighing 50g of black fungus fruiting body powder which is sieved by a 60-mesh sieve, adding the deionized water, stirring and leaching at 95 ℃ for 2.5h, centrifuging, repeatedly stirring and leaching precipitates, combining two supernatants, performing suction filtration to remove impurities, and then performing a silicon carbide ceramic membrane separation process. And placing the supernatant into a feed liquid tank of a silicon carbide ceramic membrane device with the diameter of 40nm, and sealing an inlet of the feed liquid tank with a preservative film to prevent external impurities from entering. The inside of the container is ensured to be in an isolation state with the external environment. Firstly, performing a membrane process concentration mode under the pressure of 0-0.5 MPa, closing a valve before a membrane, adding 10L of supernatant into a feed liquid tank, starting a pump, and concentrating 10L of feed liquid to 2L; then, under the pressure of 0-0.5 MPa, a membrane process washing and filtering mode is carried out, 10L of deionized water is added into a feed liquid tank, washing and filtering are started, 5L of deionized water is added when 1L of deionized water is washed, and the steps are repeated for 5 times. And finally, collecting 1L of the raw material solution after washing, filtering and concentrating, concentrating by using a reduced pressure concentrator, pouring into a flat plate, and freeze-drying to obtain the auricularia auricula polysaccharide. As shown in fig. 1.
The chemical components of the auricularia auricula polysaccharide intercepted by membrane separation are shown in the table 1.
Example 2
A method for separating edible fungus polysaccharide based on a silicon carbide ceramic membrane technology comprises the following steps:
rinsing the colloid edible fungi with running water, washing off impurities on the surface, putting the wiped sample into a blast oven for drying at 80 ℃, crushing the dried sample, and sieving with a 60-mesh sieve.
Weighing 5L of deionized water, weighing 50g of Auricularia fuscosuccinea fruiting body powder sieved by a 60-mesh sieve, adding deionized water, stirring and leaching at 95 ℃ for 2.5h, centrifuging, repeatedly stirring and leaching precipitates, mixing two supernatants, performing suction filtration to remove impurities, and performing membrane separation. And (3) placing the supernatant into a feed liquid tank of a silicon carbide ceramic membrane device with the diameter of 40nm, and sealing an inlet of the feed liquid tank by using a preservative film to ensure that the interior of the container is in an isolated state from the external environment. Firstly, performing a membrane process concentration mode under the pressure of 0-0.5 MPa, closing a valve before a membrane, adding 10L of supernatant into a feed liquid tank, starting a pump, and concentrating 10L of feed liquid to 2L; then, under the pressure of 0-0.5 MPa, a membrane process washing and filtering mode is carried out, 10L of deionized water is added into a feed liquid tank, washing and filtering are started, 5L of deionized water is added when 1L of deionized water is washed, and the steps are repeated for 5 times. And finally, collecting 1L of raw material liquid after washing, filtering and concentrating, concentrating by using a reduced pressure concentrator, pouring into a flat plate, and freeze-drying to obtain the auricularia polytricha polysaccharide. As shown in fig. 1.
The chemical components of the Auricularia fuscosuccinea polysaccharide trapped by membrane separation are shown in Table 1.
Example 3
A method for separating edible fungus polysaccharide based on a silicon carbide ceramic membrane technology comprises the following steps:
rinsing the tremella fruiting body of the colloid edible fungus with running water, washing off impurities on the surface, putting the wiped sample into a blast oven for drying at 80 ℃, and crushing the dried sample and sieving the crushed sample with a 60-mesh sieve.
Weighing 15L of deionized water, weighing 150g of tremella sporophore powder which is sieved by a 60-mesh sieve, adding the deionized water, stirring and leaching for 2.5h at the temperature of 95 ℃, centrifuging, repeatedly stirring and leaching precipitates, combining two supernatants, performing suction filtration to remove impurities, and performing a membrane separation process. And placing the supernatant into a feed liquid tank of a silicon carbide ceramic membrane device with the diameter of 40nm, and sealing an inlet of the feed liquid tank with a preservative film to prevent external impurities from entering. The inside of the container is ensured to be in an isolation state with the external environment. Firstly, under the pressure of 0-0.5 MPa, performing a membrane process concentration mode, closing a valve before membrane, adding 20L of supernatant into a feed liquid tank twice, starting a pump, and concentrating 20L of feed liquid to 4L twice; then, under the pressure of 0-0.5 MPa, the washing and filtering mode of the membrane process is carried out in two batches, 10L of deionized water is added into the feed liquid tank, the washing and filtering are started, 5L of deionized water is added when the volume is 1L, and the process is repeated for 5 times. And finally collecting 1L of raw material liquid obtained after two batches of washing, filtering and concentrating, concentrating by using a reduced pressure concentration instrument, pouring into a flat plate, and freeze-drying to obtain the tremella polysaccharide. As shown in fig. 1.
The chemical components of the tremella polysaccharide retained by the membrane separation are shown in table 1.
1. And (3) taking the index of the polysaccharide obtained by the traditional alcohol precipitation method as a reference to evaluate the effect of the polysaccharide separated by the membrane.
TABLE 1 comparison of chemical compositions of polysaccharides from edible fungi obtained by conventional alcohol precipitation method and membrane separation according to the present invention
Figure BDA0003890319150000051
Figure BDA0003890319150000061
As shown in Table 1, the total sugar content of the edible fungus polysaccharide extracted by the membrane separation method can be compared favorably with that of the conventional alcohol precipitation method, and the total sugar content of the tremella polysaccharide obtained by the membrane separation method is 10% higher than that obtained by the alcohol precipitation method.
The purity of the obtained polysaccharide was judged by protein content. The purity of the edible fungus polysaccharide obtained by membrane separation is obviously lower than that of the edible fungus polysaccharide obtained by alcohol precipitation, the content of the black fungus polysaccharide protein is reduced by 66.14%, the content of the Auricularia polytricha polysaccharide protein is reduced by 18.64%, the content of the tremella polysaccharide protein is reduced by 43.19%, and small molecular proteins can be removed in the process of washing and filtering.
The colloidal edible fungus polysaccharide is separated by the silicon carbide ceramic membrane, a large amount of protein can be removed, and the removal rate of the protein by the alcohol precipitation method is not ideal. Meanwhile, compared with an alcohol precipitation method, the silicon carbide ceramic membrane can avoid the use of a large amount of ethanol, and is environment-friendly. Therefore, when the colloid edible fungus polysaccharide is separated by the silicon carbide ceramic membrane, the efficiency of the polysaccharide preparation process can be improved, the purity of the colloid edible fungus polysaccharide is increased, and meanwhile, the production cost can be saved.
2. The synergistic effect of leaching for 2-2.5h and membrane separation for 5 times by using the silicon carbide ceramic membrane in the method
TABLE 2 synergistic effect of leaching for 2-2.5h and membrane separation for 5 times by using silicon carbide ceramic membrane in the method of the invention
Figure BDA0003890319150000062
Figure BDA0003890319150000071
The preparation methods of comparative example 1 and comparative example 4 in table 2 were the same as those of example 1 except for the differences shown in table 2, and the preparation methods of comparative example 2 and comparative example 3 in table 2 were the same as those of example 3 except for the differences shown in table 2.
As can be seen from Table 2, when the edible fungus polysaccharide is treated and separated under the conditions of leaching for 2-2.5 hours and membrane separation for 5 times by using the silicon carbide ceramic membrane, the total sugar content and the uronic acid content of the prepared edible fungus polysaccharide are obviously higher than the effect of the edible fungus polysaccharide treated under the two conditions which are not in the range, so that when the edible fungus polysaccharide is treated and separated under the conditions of leaching for 2-2.5 hours and membrane separation for 5 times by using the silicon carbide ceramic membrane, the two conditions have a synergistic effect, and the total sugar content and the uronic acid content of the edible fungus polysaccharide can be synergistically improved by leaching for 2-2.5 hours and membrane separation for 5 times by using the silicon carbide ceramic membrane. Meanwhile, as can be seen from table 2, the content of protein can be effectively reduced under the synergistic effect of two conditions of leaching for 2-2.5 hours and membrane separation for 5 times by using the silicon carbide ceramic membrane, and the purity of the chemical components of the edible fungi polysaccharide can be improved.
Therefore, it can be seen that, when the edible fungus polysaccharide is treated and separated by using the conditions of leaching for 2-2.5h and membrane separation for 5 times by using the silicon carbide ceramic membrane, the two conditions have synergistic effect.
Although the embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, alterations and modifications are possible without departing from the spirit and scope of this disclosure and appended claims, and accordingly, the scope of this disclosure is not limited to the embodiments disclosed.

Claims (6)

1. A method for separating edible fungus polysaccharide based on a silicon carbide ceramic membrane technology is characterized by comprising the following steps: the method comprises the following steps:
rinsing the colloid edible fungi with running water, washing off impurities on the surface, putting the wiped sample into a blast oven for drying at 80 ℃, crushing the dried sample, and sieving with a 60-mesh sieve; sieving colloid edible fungi powder and deionized water according to the mass ratio of feed liquid of 1:100, leaching for 2-2.5h at 95 ℃, centrifuging to obtain a supernatant, centrifuging and precipitating to repeat the leaching operation, combining the supernatants, and performing suction filtration to remove impurities to obtain an extracting solution for later use;
the obtained extracting solution is taken as a raw material solution, the extracting solution is placed in a silicon carbide ceramic membrane, the interior of the silicon carbide ceramic membrane is ensured to be in an isolation state with the external environment, the first step of membrane separation, namely concentration, is carried out under the pressure of 0-0.5 MPa, and when the volume of the raw material solution is concentrated to 1/5 of the original volume; adding deionized water with 5 times of volume to wash and filter under the pressure of 0-0.5 MPa, washing and filtering to 1/5 of the original volume, repeating for 5 times, and finally concentrating the volume of the raw material liquid to 1/10 of the volume of the original raw material liquid; and (4) carrying out vacuum freeze drying on the trapped fluid to obtain the polysaccharide separated by the membrane.
2. The method of claim 1, wherein: the diameter of the silicon carbide ceramic membrane is
Figure FDA0003890319140000011
3. The method of claim 1, wherein: the edible fungi include Auricularia fruiting body, auricularia fuscosuccinea fruiting body, and Tremella fruiting body.
4. A method according to any one of claims 1 to 3, characterized in that: the raw material liquid is placed in a raw material tank of the silicon carbide ceramic membrane equipment, and an inlet of the raw material liquid tank is sealed by a preservative film, so that the interior of the container is kept in an isolated state from the external environment.
5. A edible fungus mucilaginous polysaccharide obtained by the method according to any one of claims 1 to 4.
6. Use of a method according to any one of claims 1 to 4 for the isolation of edible fungus mucilaginose.
CN202211258352.8A 2022-10-14 2022-10-14 Method for separating edible fungus polysaccharide based on silicon carbide ceramic membrane technology and application Pending CN115626958A (en)

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