CN114478813B - Method for extracting polysaccharide from hericium erinaceus spore powder - Google Patents
Method for extracting polysaccharide from hericium erinaceus spore powder Download PDFInfo
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Abstract
The invention relates to a method for extracting polysaccharide from hericium erinaceus spore powder, which comprises the following steps: (1) And (3) soaking the hericium erinaceus spore powder in a sodium chloride aqueous solution to enable sodium chloride to fully enter the spore powder to obtain the pretreated spore powder. (2) And (3) immersing the pretreated spore powder into deionized water to obtain the swollen spore powder. (3) Freeze-drying the swollen spore powder and then crushing to obtain the wall-broken spore powder. (4) And (3) putting the wall-broken spore powder into water, heating, carrying out ultrasonic extraction, carrying out solid-liquid separation after the solid-liquid separation is finished, and respectively collecting the extract to be extracted and solid residues. (5) And adding a modified adsorbent into the extract to perform decolorization treatment, then performing solid-liquid separation, and sequentially performing alcohol precipitation separation and drying treatment on the obtained decolorized solution to obtain a hericium erinaceus spore powder polysaccharide product. The method not only adopts the characteristics of the freeze-drying technology to effectively improve the wall breaking effect of the hericium erinaceus spore powder, but also realizes the decolorization treatment and improves the purity and the quality of the extracted polysaccharide substances.
Description
Technical Field
The invention relates to the technical field of hericium erinaceus spore powder processing, and particularly relates to a method for extracting polysaccharide from hericium erinaceus spore powder.
Background
The spore powder can be ejected out to be used as a propagation seed when the hericium erinaceus grows to a later stage, and the spore powder is developed into the hericium erinaceus in a proper environment, so that the hericium erinaceus is continuously continued. The hericium erinaceus spore powder contains various active substances such as hericium erinaceus polysaccharide and the like, has high nutritional value and medicinal efficacy, and researches show that the hericium erinaceus polysaccharide has obvious anticomplementary activity and the effect of promoting lymphocyte proliferation and has an important effect of improving the immunity of the organism.
The extraction of the hericium erinaceus spore powder is an effective way for obtaining polysaccharide components. However, the cell wall of the hericium erinaceus spore powder can seriously obstruct the release of polysaccharide substances in the hericium erinaceus spore powder in the leaching process, so that the polysaccharide acquisition rate is low, and the long-time heating leaching is beneficial to improving the release of the polysaccharide substances in the hericium erinaceus spore powder, but is easy to cause the problem of polysaccharide degradation, so that the efficacy of the obtained polysaccharide substances is influenced. Therefore, the wall breaking treatment of the hericium erinaceus spore powder before leaching is an effective way to solve the above problems. However, the existing wall breaking methods such as the wall breaking machine not only require long wall breaking time, but also have low wall breaking rate to the hericium erinaceus spore powder, have unsatisfactory wall breaking effect, and are still not beneficial to the extraction of polysaccharide substances in the hericium erinaceus spore powder.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for extracting polysaccharide from hericium erinaceus spore powder, which not only adopts the characteristics of the freeze-drying technology to effectively improve the wall breaking effect of the hericium erinaceus spore powder, but also realizes the decolorization treatment, and improves the purity and quality of the extracted polysaccharide substance. To achieve the above object, the present invention specifically provides the following.
A method for extracting polysaccharide from hericium erinaceus spore powder comprises the following steps:
(1) And (3) soaking the hericium erinaceus spore powder in a sodium chloride aqueous solution to enable sodium chloride to fully enter the spore powder to obtain pretreated spore powder for later use.
(2) And (3) immersing the pretreated spore powder into deionized water, and fully absorbing water and swelling the spore powder to obtain swollen spore powder for later use.
(3) Freeze-drying the swollen spore powder and then crushing to obtain wall-broken spore powder for later use.
(4) And (3) putting the wall-broken spore powder into water, heating, ultrasonically leaching, performing solid-liquid separation after completion, and respectively collecting the extract and solid residues for later use.
(5) And adding a modified adsorbent into the extract to perform decolorization treatment, then performing solid-liquid separation, and sequentially performing alcohol precipitation separation and drying treatment on the obtained decolorized solution to obtain a hericium erinaceus spore powder polysaccharide product.
The preparation method of the modified adsorbent comprises the following steps:
(i) And (4) drying the solid residue obtained in the step (4), crushing the dried solid residue into powder, uniformly mixing the powder with the chopped chrysotile asbestos, and then adding water and a binder for wet granulation to obtain a precursor.
(ii) And carbonizing the precursor, soaking the obtained carbonized product with oxidizing acid liquor, washing the carbonized product to be neutral after the carbonization is finished, and drying to obtain the modified adsorbent.
In a further scheme, in the step (1), the mass concentration of the sodium chloride aqueous solution is kept between 8 and 15 percent, and the hericium erinaceus spore powder is soaked in the sodium chloride aqueous solution to absorb water and permeate sodium chloride so as to keep high osmotic pressure in the spore powder.
In a further scheme, in the step (1), the soaking time is 2-3 h, so that the hericium erinaceus spore powder can absorb moisture and salt in sufficient time.
In a further scheme, in the step (2), the pretreated spore powder is immersed in deionized water and then kept for 50-90 min, salt in the pretreated spore powder is permeated outwards under the immersion of clear water, and meanwhile, the clear water enters the spore powder to swell the spore powder.
In a further scheme, in the step (3), the swollen spore powder is frozen to below-30 ℃, then the moisture is sublimated under the vacuum condition of-0.2 to-0.1 MPa, and then the obtained freeze-dried block is ground into powder, so that the wall-broken spore powder is obtained.
In a further scheme, in the step (4), the ratio of the sporoderm-broken spore powder to water is 1g: 50-70 ml, in the step, the polysaccharide in the wall-broken spore powder is dissolved in water to form a solution to be extracted, so as to further extract the polysaccharide substances in the solution.
In a further scheme, in the step (4), the leaching temperature is 40-55 ℃, the leaching time is 40-60 min, and preferably, water bath heating is adopted to ensure the leaching temperature. In the step, the low-temperature leaching is beneficial to leaching the polysaccharide in the sporozoite powder and avoiding the problem that the polysaccharide is degraded due to overhigh temperature.
In a further scheme, in the step (5), the adding amount of the modified adsorbent is 3-4.5% of the mass of the liquid to be extracted, the decoloring time is 35-50 min, and the decoloring is carried out under the stirring condition. Decolorizing the leach liquor helps to improve the purity and quality of the polysaccharide species ultimately extracted.
In a further embodiment, in step (5), the method for precipitating ethanol comprises: adding ethanol with the volume more than four times of that of the decolorized extract to the decolorized extract, wherein the concentration of the ethanol is not less than 95%, standing and precipitating for 20-24 h to fully separate out and precipitate polysaccharide substances in the extract, then carrying out solid-liquid separation, airing the obtained solid at room temperature for more than 1h to fully volatilize the residual ethanol, and thus obtaining the hericium erinaceus spore powder polysaccharide product.
In a further aspect, in step (i), the chrysotile asbestos, which is a natural material having a nanotube-like structure, is added in an amount of 10 to 17% by mass of the powder, and is used as an adsorbent component, not only to prevent the collapse of micropores in the adsorbent during carbonization, but also to contribute to the improvement of the performance of the adsorbent.
In a further aspect, in step (i), the chrysotile asbestos has a length of between 1 and 2mm to facilitate thorough mixing of the early solid residue powder.
In a further scheme, in the step (ii), the temperature of the carbonization treatment is 700-850 ℃ and the time is 1.5-3 h.
In a further embodiment, in step (ii), the oxidizing acid solution includes any one of a sulfuric acid solution and a nitric acid solution. After further treatment by the oxidizing acid liquor, the active carbon is not only beneficial to hole expanding treatment, but also can remove MgO components in the chrysotile asbestos, thereby modifying the chrysotile asbestos into a porous nano-tubular structure and opening micropores in the adsorbent and a pipe cavity of the chrysotile asbestos.
Further, in the step (ii), the soaking time is 30-45 min, and the stirring is continuously carried out in the soaking process; and (3) after the solid-liquid separation is finished, washing the obtained carbonized product with clear water until the washing liquid is neutral, and drying to obtain the modified adsorbent.
Compared with the prior art, the invention has the following beneficial effects:
just as in the foregoing, when polysaccharide components in hericium erinaceus spore powder are extracted, the wall-breaking effect of the spore powder has an important influence on the extraction rate of the polysaccharide, the traditional method has a poor wall-breaking effect on the hericium erinaceus spore powder, the polysaccharide content in the spore powder is limited, the hericium erinaceus spore powder is difficult to collect, and the hericium erinaceus spore powder is wasted due to the low extraction rate. Therefore, the invention provides a novel method for breaking the wall of hericium erinaceus spore powder, the wall breaking rate is as high as more than 97%, and the problems are effectively solved for the following reasons: according to the invention, firstly, the hericium erinaceus spore powder is soaked in a high-concentration sodium chloride solution, so that on one hand, the spore powder can be preliminarily swelled to increase the extrusion force on cell walls, and on the other hand, the sodium chloride infiltrated into the spore powder can keep the spore powder at high osmotic pressure, thereby facilitating further water absorption and swelling. On the basis, the spore powder is soaked in the clear water, the clear water can further permeate into the spore powder through cell walls due to the high-concentration sodium chloride contained in the spore powder, and the sodium chloride permeates into the clear water through the cell walls, so that the spore powder is further filled with water and swelled. Furthermore, the spore powder in the swelling state is subjected to freeze-drying treatment, so that the cell wall of the spore powder is completely broken, the cell wall of the spore powder is broken by extrusion due to the fact that liquid water in the spore powder forms ice and the volume of the spore powder is increased after the spore powder is frozen at low temperature, the spore powder in the swelling state is in a state that the cell wall is fully extruded, the liquid water forms ice and the volume of the spore powder is increased by freezing, the cell wall of the spore powder is broken by extrusion, and the cell wall of the spore powder cannot resist the breakage by transmitting extrusion force to other parts when the cell wall of the spore powder is extruded due to the fact that the ice in the spore powder is rigid solid, so that a good wall breaking effect can be brought. Further, ice in the spore powder is directly sublimated into water vapor under the subsequent vacuum condition and removed, and the broken cell walls are impacted by the water vapor again in the process, so that the wall breaking effect is further enlarged, and particularly, the wall breaking effect can be effectively enlarged by part of the broken cell walls which are cracked but have small degrees in the process.
In addition, the modified adsorbent is prepared to decolor the extract, so that the purity and appearance quality of the polysaccharide extract are effectively improved. This is because part of the pigment in the spore powder enters the leaching solution during the heating leaching process of the sporoderm-broken spore powder. Therefore, the spore powder residue separated after leaching is used as a raw material, and the chopped chrysotile asbestos is added into the raw material, so that on one hand, the chrysotile asbestos can be dispersed in the adsorbent to form a three-dimensional network structure, the chrysotile asbestos can play a role in solidifying the spore powder residue, the problem of micropore collapse of the adsorbent in the high-temperature carbonization process is effectively prevented, the good decoloring capacity of the adsorbent is ensured, and meanwhile, the chrysotile asbestos can also adapt to the high-temperature environment in the carbonization process. In addition, the chrysotile asbestos has the characteristic of a nano-tube structure, but because the chrysotile asbestos is doped in spore powder residues and then two ends are sealed, the chrysotile asbestos nano-tube structure cannot play a role in decoloring. On one hand, under the action of acid, mgO in the chrysotile asbestos is dissolved to enable the chrysotile asbestos to form a porous nanotube structure, namely, a lumen of the chrysotile asbestos is opened, micropores in the adsorbent are communicated with the lumen of the chrysotile asbestos, and micropores in the adsorbent blocked by the chrysotile asbestos are opened, so that the decoloring capacity of the adsorbent is improved. On the other hand, hydrophilic groups are formed on the surface of the adsorbent after strong oxidizing acid treatment, which is beneficial to improving the hydrophilicity of the adsorbent and is convenient for fully mixing with the to-be-extracted liquid. On the other hand, the acid treatment is also beneficial to reaming the adsorbent and improving the decoloring capacity of the adsorbent.
Detailed Description
It is to be understood that all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, unless otherwise defined. The reagents or starting materials used in the present invention can be purchased from conventional sources, and unless otherwise specified, the reagents or starting materials used in the present invention can be used in a conventional manner in the art or in accordance with the product specification.
In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are exemplary only. The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1
1. A preparation method of a modified adsorbent comprises the following steps:
(i) Heating and drying the residual solid residue after extracting the polysaccharide in the hericium erinaceus spore powder until the water content is below 5%, then grinding the solid residue into powder in a mortar, uniformly mixing the powder with chopped chrysotile asbestos, wherein the length of the chrysotile asbestos is between 1 and 2mm, the addition amount of the chrysotile asbestos is 13% of the mass of the powder, and then adding water and an adhesive into a granulator for wet granulation to obtain a precursor.
(ii) And putting the precursor into carbonization equipment, carbonizing at 800 ℃ for 2h under the protection of nitrogen, cooling to room temperature under the protection of atmosphere, and taking out the carbonized product for later use.
(iii) And (3) putting the carbonized product into a beaker, adding a nitric acid solution with the mass concentration of 30%, stirring for 40min, filtering and separating the carbonized product after the reaction is finished, washing the carbonized product with clear water until the washing liquid is neutral, and drying for 2h in vacuum at 60 ℃ to obtain the modified adsorbent.
2. A method for extracting polysaccharide from hericium erinaceus spore powder comprises the following steps:
(1) Putting the hericium erinaceus spore powder into a beaker, adding a sodium chloride aqueous solution with the mass concentration of 12% to soak for 3 hours, and filtering and separating out the spore powder after the soaking, so as to obtain the pretreated spore powder for later use.
(2) Soaking the pretreated spore powder in deionized water for 75min, and filtering to separate spore powder to obtain swelled spore powder.
(3) Freezing the swollen spore powder to-30 deg.C, maintaining for 20h, sublimating at-0.2 MPa and 40 deg.C for 20h, and grinding the obtained lyophilized block into powder to obtain wall-broken spore powder.
(4) 1g of spore powder and water: and (5) adding the wall-broken spore powder obtained in the step (3) into water according to a proportion of 65ml, heating to 45 ℃, leaching for 50min under an ultrasonic condition to dissolve polysaccharide in the wall-broken spore powder into the water, filtering after completion, performing solid-liquid separation, and collecting the extract and solid residues respectively for later use.
(5) And (5) adding the modified adsorbent prepared in the embodiment into the to-be-extracted liquid in the step (4) for decoloring, wherein the adding amount of the modified adsorbent is 4% of the mass of the to-be-extracted liquid, the decoloring time is 35min, then filtering and carrying out solid-liquid separation after the decoloring, and respectively collecting the decolored liquid and the modified adsorbent for adsorbing pigments for later use.
(6) And (3) adding ethanol (the concentration is 95%) which is 5 times the volume of the decolorized solution obtained in the step (5), standing and precipitating for 24 hours to separate out and precipitate polysaccharide substances in the extract, then filtering and carrying out solid-liquid separation, airing the obtained solid for more than 1 hour at room temperature, and fully volatilizing the residual ethanol to obtain the hericium erinaceus spore powder polysaccharide product.
Example 2
1. A preparation method of the modified adsorbent comprises the following steps:
(i) Heating and drying the solid residue obtained in the step (4) in the embodiment 1 until the water content is below 5%, grinding the solid residue into powder in a mortar, uniformly mixing the powder and chopped chrysotile asbestos, wherein the length of the chrysotile asbestos is between 1 and 2mm, the addition amount of the chrysotile asbestos is 10 percent of the mass of the powder, and then adding water and a bonding agent into a granulator for wet granulation to obtain a precursor.
(ii) And putting the precursor into carbonization equipment, carbonizing at 750 ℃ for 3h under the protection of nitrogen, cooling to room temperature in the protection atmosphere after the carbonization is finished, and taking out a carbonized product for later use.
(iii) And (3) placing the carbonized product in a beaker, adding a nitric acid solution with the mass concentration of 35%, stirring for 30min, filtering and separating the carbonized product after the reaction is finished, washing the carbonized product with clear water until the washing liquid is neutral, and drying for 2h in vacuum at 60 ℃ to obtain the modified adsorbent.
2. A method for extracting polysaccharide from hericium erinaceus spore powder comprises the following steps:
(1) Taking hericium erinaceus spore powder in a beaker, adding a sodium chloride aqueous solution with the mass concentration of 15% to soak for 2 hours, and filtering and separating out the spore powder after the soaking to obtain the pretreated spore powder for later use.
(2) Soaking the pretreated spore powder in deionized water for 90min, and filtering to separate spore powder to obtain swelled spore powder.
(3) Freezing the swollen spore powder to 35 ℃ below zero, keeping for 18h, sublimating for 20h under the conditions of-0.2 MPa and 40 ℃, and then putting the obtained freeze-dried block into a mortar and grinding into powder to obtain the wall-broken spore powder.
(4) 1g of spore powder and water: adding the wall-broken spore powder obtained in the step (3) into water at a ratio of 70ml, heating to 55 ℃, leaching for 40min under an ultrasonic condition to dissolve polysaccharide in the wall-broken spore powder in the water, filtering after completion, performing solid-liquid separation, and respectively collecting the extract and solid residues for later use.
(5) Adding the modified adsorbent prepared in the embodiment into the to-be-extracted liquid in the step (4) for decoloring, wherein the adding amount of the modified adsorbent is 4.5% of the mass of the to-be-extracted liquid, the decoloring time is 45min, filtering and carrying out solid-liquid separation after the decoloring, and respectively collecting the decolored liquid and the modified adsorbent for later use
(6) And (3) adding ethanol (the concentration is 95%) which is 5 times the volume of the decolorized solution obtained in the step (5), standing and precipitating for 20 hours to separate out and precipitate polysaccharide substances in the extract, then filtering and carrying out solid-liquid separation, and airing the obtained solid for more than 1 hour at room temperature to fully volatilize the residual ethanol to obtain the hericium erinaceus spore powder polysaccharide product.
Example 3
1. A preparation method of the modified adsorbent comprises the following steps:
(i) Heating and drying the solid residue obtained in the step (4) of the embodiment 2 until the water content is below 5%, then grinding the solid residue into powder in a mortar, uniformly mixing the powder and the chopped chrysotile asbestos, wherein the length of the chrysotile asbestos is between 1 and 2mm, the addition amount of the chrysotile asbestos is 17 percent of the mass of the powder, and then adding water and a bonding agent into a granulator for wet granulation to obtain a precursor.
(ii) And putting the precursor into carbonization equipment, carbonizing at 700 ℃ for 3h under the nitrogen protection atmosphere, cooling to room temperature under the protection atmosphere, and taking out the carbonized product for later use.
(iii) And (3) placing the carbonized product in a beaker, adding a sulfuric acid solution with the mass concentration of 30%, stirring for 45min, filtering and separating the carbonized product after the reaction is finished, washing the carbonized product with clear water until the washing liquid is neutral, and drying for 2h in vacuum at 60 ℃ to obtain the modified adsorbent.
2. A method for extracting polysaccharide from hericium erinaceus spore powder comprises the following steps:
(1) Taking hericium erinaceus spore powder in a beaker, adding a sodium chloride aqueous solution with the mass concentration of 8% to soak for 3 hours, and filtering and separating out the spore powder after the soaking to obtain the pretreated spore powder for later use.
(2) Soaking the pretreated spore powder in deionized water for 50min, and filtering to separate spore powder to obtain swelled spore powder.
(3) Freezing the swollen spore powder to-30 deg.C, maintaining for 20h, sublimating at-0.1 MPa and 40 deg.C for 20h, and grinding the obtained lyophilized block into powder to obtain wall-broken spore powder.
(4) 1g of spore powder and water: and (4) adding the wall-broken spore powder obtained in the step (3) into water according to the proportion of 50ml, heating to 40 ℃, leaching for 60min under the ultrasonic condition to dissolve polysaccharide in the wall-broken spore powder into the water, filtering after completion, carrying out solid-liquid separation, and respectively collecting the extract to be extracted and solid residues for later use.
(5) Adding the modified adsorbent prepared in the embodiment into the to-be-extracted liquid in the step (4) for decoloring, wherein the adding amount of the modified adsorbent is 3.5% of the mass of the to-be-extracted liquid, the decoloring time is 40min, filtering and carrying out solid-liquid separation after the decoloring, and respectively collecting the decolored liquid and the modified adsorbent for later use
(6) And (4) adding ethanol (the concentration is 95%) with the volume of 4 times of the decolorized solution obtained in the step (5), standing and precipitating for 20 hours to separate out and precipitate polysaccharide substances in the extract, then filtering and carrying out solid-liquid separation, airing the obtained solid for more than 1 hour at room temperature, and fully volatilizing the residual ethanol to obtain the hericium erinaceus spore powder polysaccharide product.
Example 4
1. A preparation method of the modified adsorbent comprises the following steps:
(i) Heating and drying the solid residue obtained in the step (4) of the embodiment 3 until the water content is below 5%, then grinding the solid residue into powder in a mortar, uniformly mixing the powder and the chopped chrysotile asbestos, wherein the length of the chrysotile asbestos is between 1 and 2mm, the addition amount of the chrysotile asbestos is 15 percent of the mass of the powder, and then adding water and a bonding agent into a granulator for wet granulation to obtain a precursor.
(ii) And putting the precursor into carbonization equipment, carbonizing at 850 ℃ for 1.5h in a nitrogen protective atmosphere, cooling to room temperature in the protective atmosphere after the carbonization is finished, and taking out a carbonized product for later use.
(iii) And (3) placing the carbonized product in a beaker, adding a sulfuric acid solution with the mass concentration of 30%, stirring for 40min, filtering and separating the carbonized product after the reaction is finished, washing the carbonized product with clear water until the washing liquid is neutral, and drying for 2h in vacuum at 60 ℃ to obtain the modified adsorbent.
2. A method for extracting polysaccharide from hericium erinaceus spore powder comprises the following steps:
(1) Putting the hericium erinaceus spore powder into a beaker, adding a sodium chloride aqueous solution with the mass concentration of 10% to soak for 2.5 hours, and filtering and separating out the spore powder after the soaking is finished to obtain the pretreated spore powder for later use.
(2) Soaking the pretreated spore powder in deionized water for 70min, and filtering to separate spore powder to obtain swelled spore powder.
(3) Freezing the swollen spore powder to-30 deg.C, maintaining for 20h, sublimating at-0.1 MPa and 40 deg.C for 20h, and grinding the obtained lyophilized block into powder to obtain wall-broken spore powder.
(4) 1g of spore powder and water: and (3) adding the wall-broken spore powder obtained in the step (3) into water according to a proportion of 60ml, heating to 50 ℃, leaching for 55min under an ultrasonic condition to dissolve polysaccharide in the wall-broken spore powder into the water, filtering after completion, performing solid-liquid separation, and respectively collecting the extract and solid residues for later use.
(5) Adding the modified adsorbent prepared in the embodiment into the to-be-extracted liquid in the step (4) for decoloring treatment, wherein the adding amount of the modified adsorbent is 3.0 percent of the mass of the to-be-extracted liquid, the decoloring time is 50min, then filtering and carrying out solid-liquid separation after the decoloring treatment is finished, and respectively collecting the decolored liquid and the modified adsorbent for later use
(6) And (3) adding absolute ethyl alcohol with the volume 4.5 times of that of the decolorized solution obtained in the step (5), standing and precipitating for 20 hours to separate out and precipitate polysaccharide substances in the extract, then filtering and carrying out solid-liquid separation, and airing the obtained solid for more than 1 hour at room temperature to fully volatilize the residual ethyl alcohol to obtain the hericium erinaceus spore powder polysaccharide product.
Example 5
1. Preparation of a modified adsorbent: and (3) carrying out microwave heating on the modified adsorbent adsorbing the pigment in the step (5) in the embodiment 1 to 300 ℃ for desorption to obtain the modified adsorbent for later use.
2. A method for extracting polysaccharide from Hericium erinaceus spore powder is similar to that of the first embodiment, except that the modified adsorbent prepared in this embodiment is used for decolorization in step (5).
Example 6
1. Preparation of a modified adsorbent: and (3) carrying out microwave heating on the modified adsorbent adsorbing the pigment in the step (5) in the embodiment 5 to 300 ℃ for desorption to obtain the modified adsorbent for later use.
2. A method for extracting polysaccharide from Hericium erinaceus spore powder is similar to that of the first embodiment, except that the modified adsorbent prepared in this embodiment is used for decolorization in step (5).
Example 7
1. A preparation method of the modified adsorbent comprises the following steps:
(i) Heating and drying the residual solid residue after extracting the polysaccharide in the hericium erinaceus spore powder until the water content is below 5%, then placing the solid residue in carbonization equipment, carbonizing at 850 ℃ for 1.5h in a nitrogen protective atmosphere, cooling to room temperature in the protective atmosphere after the carbonization is completed, and taking out the carbonized product for later use.
(ii) And (3) placing the carbonized product in a beaker, adding a sulfuric acid solution with the mass concentration of 30%, stirring for 40min, filtering and separating the carbonized product after the reaction is finished, washing the carbonized product with clear water until the washing liquid is neutral, and drying for 2h in vacuum at 60 ℃ to obtain the modified adsorbent.
2. A method for extracting polysaccharide from Hericium erinaceus spore powder is similar to that of the first embodiment, except that the modified adsorbent prepared in this embodiment is used for decolorization in step (5).
Example 8
1. A preparation method of a modified adsorbent comprises the following steps:
(i) Heating and drying the solid residue obtained in the step (4) of the embodiment 3 until the water content is below 5%, then grinding the solid residue into powder in a mortar, uniformly mixing the powder and the chopped chrysotile asbestos, wherein the length of the chrysotile asbestos is between 1 and 2mm, the addition amount of the chrysotile asbestos is 15 percent of the mass of the powder, and then adding water and a bonding agent into a granulator for wet granulation to obtain a precursor.
(ii) And putting the precursor into carbonization equipment, carbonizing at 850 ℃ for 1.5h in a nitrogen protective atmosphere, cooling to room temperature in the protective atmosphere after the carbonization is finished, and taking out a carbonized product to obtain the modified adsorbent.
2. A method for extracting polysaccharide from Hericium erinaceus spore powder is similar to that of the first embodiment, except that the modified adsorbent prepared in this embodiment is used for decolorization in step (5).
Example 9
A method for extracting polysaccharide from hericium erinaceus spore powder comprises the following steps:
(1) Putting the hericium erinaceus spore powder into a beaker, adding a sodium chloride aqueous solution with the mass concentration of 12% to soak for 3 hours, and filtering and separating out the spore powder after the soaking, so as to obtain the pretreated spore powder for later use.
(2) Soaking the pretreated spore powder in deionized water for 75min, and filtering to separate spore powder to obtain swelled spore powder.
(3) Freezing the swollen spore powder to-30 deg.C, maintaining for 20h, heating to 40 deg.C for thawing, and repeating the step for 5 times to obtain wall-broken spore powder.
(4) 1g of spore powder and water: and (5) adding the wall-broken spore powder obtained in the step (3) into water according to a proportion of 65ml, heating to 45 ℃, leaching for 50min under an ultrasonic condition to dissolve polysaccharide in the wall-broken spore powder into the water, filtering after completion, performing solid-liquid separation, and collecting the extract and solid residues respectively for later use.
(5) And (3) adding a modified adsorbent (same as the example 1) into the to-be-extracted liquid in the step (4) for decoloring, wherein the adding amount of the modified adsorbent is 4% of the mass of the to-be-extracted liquid, the decoloring time is 35min, filtering and carrying out solid-liquid separation after the decoloring, and respectively collecting the decolored liquid and the modified adsorbent for adsorbing pigments for later use.
(6) And (3) adding ethanol (the concentration is 95%) which is 5 times the volume of the decolorized solution obtained in the step (5), standing and precipitating for 24 hours to separate out and precipitate polysaccharide substances in the extract, then filtering and carrying out solid-liquid separation, airing the obtained solid for more than 1 hour at room temperature, and fully volatilizing the residual ethanol to obtain the hericium erinaceus spore powder polysaccharide product.
Example 10
A method for extracting polysaccharide from hericium erinaceus spore powder comprises the following steps:
(1) Putting the hericium erinaceus spore powder into a beaker, adding a sodium chloride aqueous solution with the mass concentration of 12% to soak for 3 hours, and filtering and separating out the spore powder after the soaking, so as to obtain the pretreated spore powder for later use.
(2) Freezing the swollen spore powder to-30 deg.C, maintaining for 20h, sublimating at-0.2 MPa and 40 deg.C for 20h, and grinding the obtained lyophilized block into powder to obtain wall-broken spore powder.
(3) 1g of spore powder and water: and (3) adding the wall-broken spore powder obtained in the step (2) into water according to a proportion of 65ml, heating to 45 ℃, leaching for 50min under an ultrasonic condition to dissolve polysaccharide in the wall-broken spore powder into the water, filtering after completion, performing solid-liquid separation, and collecting the extract and solid residues respectively for later use.
(4) And (3) adding a modified adsorbent (same as the example 1) into the to-be-extracted liquid in the step (3) for decoloring, wherein the adding amount of the modified adsorbent is 4% of the mass of the to-be-extracted liquid, the decoloring time is 35min, filtering and carrying out solid-liquid separation after the decoloring, and respectively collecting the decolored liquid and the modified adsorbent for adsorbing pigments.
(5) And (5) adding ethanol (the concentration is 95%) with the volume 5 times of that of the decolorized solution obtained in the step (4), standing and precipitating for 24 hours to separate out and precipitate polysaccharide substances in the extract, then filtering and carrying out solid-liquid separation, airing the obtained solid for more than 1 hour at room temperature, and fully volatilizing the residual ethanol to obtain the hericium erinaceus spore powder polysaccharide product.
Example 11
A method for extracting polysaccharide from hericium erinaceus spore powder comprises the following steps:
(1) Putting Hericium erinaceus spore powder into a beaker, soaking the spore powder in deionized water for 75min, and filtering to separate out spore powder to obtain swollen spore powder for later use.
(2) Freezing the swollen spore powder to-30 deg.C, maintaining for 20h, sublimating at-0.2 MPa and 40 deg.C for 20h, and grinding the obtained lyophilized block into powder to obtain wall-broken spore powder.
(3) 1g of spore powder and water: and (5) adding the wall-broken spore powder obtained in the step (3) into water according to a proportion of 65ml, heating to 45 ℃, leaching for 50min under an ultrasonic condition to dissolve polysaccharide in the wall-broken spore powder into the water, filtering after completion, performing solid-liquid separation, and collecting the extract and solid residues respectively for later use.
(4) And (3) adding a modified adsorbent (same as the example 1) into the to-be-extracted liquid in the step (3) for decolorization treatment, wherein the adding amount of the modified adsorbent is 4% of the mass of the to-be-extracted liquid, the decolorization time is 35min, filtering for solid-liquid separation after the decolorization treatment is finished, and collecting the decolorized liquid and the modified adsorbent for adsorbing pigments respectively for later use.
(5) And (3) adding ethanol (the concentration is 95%) which is 5 times the volume of the decolorized solution obtained in the step (4), standing and precipitating for 24 hours to separate out and precipitate polysaccharide substances in the extract, then filtering and carrying out solid-liquid separation, airing the obtained solid for more than 1 hour at room temperature, and fully volatilizing the residual ethanol to obtain the hericium erinaceus spore powder polysaccharide product.
The wall-breaking rate of the hericium erinaceus spore powder, the yield of the hericium erinaceus spore powder polysaccharide and the purity of the hericium erinaceus spore powder polysaccharide product in each example are tested, and the results are shown in the following table.
From the results in the table, it can be seen that examples 5 and 6 still maintain good decolorization ability after the modified adsorbent is used for many times, which indicates that the modified adsorbent has good stability and can be recycled. From the test results of example 7 and example 8, it can be seen that the decoloring effect was reduced in the modified adsorbent not doped with chrysotile asbestos and the modified adsorbent not subjected to acid treatment, resulting in the obtained hericium erinaceum spore powder polysaccharide product being rich in color and reduced in purity. The wall breaking effect is obviously reduced in the embodiment 9 of carrying out wall breaking on spore powder by adopting the traditional freeze-thaw treatment, the embodiment 10 of not adopting clear water treatment on the spore powder and the embodiment 11 of not adopting sodium chloride solution treatment on the spore powder, so that the extraction rate of polysaccharide in the hericium erinaceus spore powder is obviously reduced.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (14)
1. A method for extracting polysaccharide from hericium erinaceus spore powder is characterized by comprising the following steps:
(1) Soaking hericium erinaceus spore powder in a sodium chloride aqueous solution to enable sodium chloride to fully enter the spore powder to obtain pretreated spore powder for later use; the mass concentration of the sodium chloride aqueous solution is kept between 8 and 15 percent;
(2) Immersing the pretreated spore powder into deionized water to ensure that the spore powder fully absorbs water and swells to obtain swollen spore powder for later use;
(3) Freeze-drying the swollen spore powder and then crushing to obtain wall-broken spore powder for later use;
(4) Heating and ultrasonically leaching the wall-broken spore powder in water, performing solid-liquid separation after the completion, and respectively collecting the extract and solid residues for later use;
(5) Adding a modified adsorbent into the to-be-extracted solution for decolorization, then carrying out solid-liquid separation, and sequentially carrying out alcohol precipitation separation and drying treatment on the obtained decolorized solution to obtain a hericium erinaceus spore powder polysaccharide product;
the preparation method of the modified adsorbent comprises the following steps:
(i) Drying the solid residue obtained in the step (4), crushing the dried solid residue into powder, uniformly mixing the powder with chopped chrysotile asbestos, and then adding water and a bonding agent for wet granulation to obtain a precursor;
(ii) And carbonizing the precursor, soaking the obtained carbonized product with oxidizing acid liquor, washing the carbonized product to be neutral after the carbonization is finished, and drying to obtain the modified adsorbent.
2. The method for extracting polysaccharide from hericium erinaceus spore powder according to claim 1, wherein in the step (1), the soaking time is 2-3 hours.
3. The method for extracting polysaccharide from hericium erinaceus spore powder according to claim 1, wherein in the step (2), the pretreated spore powder is immersed in deionized water and then kept for 50-90 min.
4. The method for extracting polysaccharide from hericium erinaceus spore powder according to claim 1, wherein in the step (3), the swollen spore powder is frozen to below-30 ℃, then water is sublimated under a vacuum condition of-0.2 to-0.1 MPa, and then the obtained freeze-dried block is ground into powder, so that the wall-broken spore powder is obtained.
5. The method for extracting polysaccharide from hericium erinaceus spore powder according to claim 1, wherein in the step (4), the ratio of the wall-broken spore powder to water is 1g:50 to 70ml.
6. The method for extracting polysaccharide from hericium erinaceus spore powder according to claim 1, wherein in the step (4), the leaching temperature is 40-55 ℃ and the leaching time is 40-60 min.
7. The method for extracting polysaccharide from hericium erinaceus spore powder according to claim 6, wherein the extraction temperature is ensured by heating in a water bath.
8. The method for extracting polysaccharide from hericium erinaceus spore powder according to claim 1, wherein in the step (5), the modified adsorbent is added in an amount of 3-4.5% by mass of the liquid to be extracted, the decoloring time is 35-50 min, and the decoloring is performed under a stirring condition.
9. The method for extracting polysaccharide from hericium erinaceus spore powder according to claim 1, wherein in the step (5), the alcohol precipitation method comprises the following steps: and adding ethanol with the volume more than four times of that of the decolorized extract to the decolorized extract, wherein the concentration of the ethanol is not less than 95%, standing and precipitating for 20-24 h, performing solid-liquid separation after the completion, and airing the obtained solid at room temperature for more than 1h to obtain the hericium erinaceus spore powder polysaccharide product.
10. The method for extracting polysaccharide from hericium erinaceus spore powder according to any one of claims 1 to 9, wherein the chrysotile asbestos is added in an amount of 10 to 17% by mass of the powder in step (i).
11. The method for extracting polysaccharide from hericium erinaceus spore powder according to claim 10, wherein the chrysotile asbestos has a length of between 1 and 2 mm.
12. The method for extracting polysaccharide from hericium erinaceus spore powder according to any one of claims 1 to 9, wherein in the step (ii), the temperature of the carbonization treatment is 700 to 850 ℃ and the time is 1.5 to 3 hours.
13. The method for extracting polysaccharide from hericium erinaceus spore powder according to any one of claims 1 to 9, wherein in the step (ii), the oxidizing acid solution comprises any one of sulfuric acid solution and nitric acid solution.
14. The method for extracting polysaccharide from hericium erinaceus spore powder according to any one of claims 1 to 9, wherein in the step (ii), the soaking time is 30-45 min, and the stirring is continuously carried out during the soaking process; and (4) after the solid-liquid separation is finished, washing the obtained carbonized product with clear water until the washing liquid is neutral, thus obtaining the modified adsorbent.
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