CN112280814A - High-content medium-low molecular weight konjac glucomannan, preparation method thereof and functional composition thereof - Google Patents
High-content medium-low molecular weight konjac glucomannan, preparation method thereof and functional composition thereof Download PDFInfo
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Abstract
The invention discloses high-content medium and low molecular weight konjac glucomannan, a preparation method thereof and an efficacy composition thereof. Therefore, the glucomannan is degraded by an enzyme degradation method, and then a series of separation and purification methods are adopted to finally separate and obtain the medium molecular weight glucomannan (with the weight-average molecular weight of 15300-17600) and the low molecular weight glucomannan (with the weight-average molecular weight of 6800-8500) so as to improve the application possibility of the glucomannan.
Description
Technical Field
The invention relates to the technical field of daily necessities, in particular to high-content medium and low molecular weight konjac glucomannan, a preparation method and an efficacy composition thereof.
Background
Glucomannan is a water-soluble natural high-molecular polysaccharide, and is widely applied to the fields of environmental protection, medicine, biology and the like. Glucomannan is a medium molecular weight non-ionic mannan formed by bonding mannan and glucose in a molar ratio of 1.6 (1-4) through beta-1, 4-pyranoside linkages, and has an average molecular weight of 20-200 million with an acetyl group at every 19 sugar residues to aid solubility.
The molecular weight of the natural glucomannan is too large, so that the problems of high viscosity, low solubility and the like are caused, and the application of the glucomannan is severely limited.
Disclosure of Invention
Aiming at the problems, the invention provides high-content medium and low molecular weight konjac glucomannan, a preparation method thereof and an efficacy composition thereof, aiming at improving the application of the konjac glucomannan by enzymolysis.
The specific technical scheme is as follows:
the first aspect of the present invention provides a method for preparing medium molecular weight glucomannan, which is characterized by comprising the steps of: adding 10 parts of konjac refined powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 300-65U cellulase under the stirring state, carrying out enzymolysis for 48-60h under the conditions of the stirring rotation speed of 200-300r/min and the temperature of 60-65 ℃, carrying out enzyme deactivation in a boiling water bath for 15-20min, adding 10-15 parts of a gel-releasing agent, stirring for 3-5h, carrying out centrifugal separation, separating the obtained centrifugal liquid through a molecular sieve separation device, adding 30-50 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 3-5h, repeating 3-5 times of repeated precipitation-centrifugation-stirring as above, taking the precipitate obtained by the last centrifugation, and drying in a dryer to obtain the medium molecular weight glucomannan;
wherein, the height ratio of the separation column diameter of the molecular sieve equipment is 1 (30-50), the linear flow velocity is 8-10L/min, the particle diameter of the molecular sieve is 0.3-0.7mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1.2: 1.
The preparation method is also characterized in that the slow release solution is prepared from a citric acid solution and a sodium citrate solution with the concentration of 0.1 mol/L.
The second aspect of the present invention is to provide a medium molecular weight glucomannan prepared by the above preparation method.
The third aspect of the present invention is to provide a method for preparing low molecular weight glucomannan, characterized by comprising the steps of: adding 10 parts of konjac refined powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 300-65U cellulase under the stirring state, carrying out enzymolysis for 72-75h under the conditions of the stirring rotation speed of 200-300r/min and the temperature of 60-65 ℃, carrying out deactivation of enzyme in a boiling water bath for 15-20min, adding 7-10 parts of a gel-releasing agent, stirring for 3-5h, carrying out centrifugal separation, separating the obtained centrifugal liquid through a molecular sieve separation device, adding 30-50 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 3-5h, repeating 3-5 times of repeated precipitation-centrifugation-stirring as above, taking the precipitate obtained by the last centrifugation, and drying in a dryer to obtain the low-molecular-weight glucomannan;
wherein, the height ratio of the separation column diameter of the molecular sieve equipment is 1 (30-40), the linear flow velocity is 8-10L/min, the particle diameter of the molecular sieve is 0.3-0.5mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1: 1.
The preparation method is also characterized in that the slow release solution is prepared from a citric acid solution and a sodium citrate solution with the concentration of 0.1 mol/L.
The fourth aspect of the present invention is to provide a low molecular weight glucomannan produced by the above production method.
The fifth aspect of the invention provides an efficacy composition, which is characterized by comprising the following raw materials in parts by weight: 1 part of low molecular weight glucomannan, 1 part of medium molecular weight glucomannan and 2 parts of rose hydrosol.
The above effect composition also has the characteristic that the rose hydrosol is prepared by distilling fresh Damascus rose.
Because the glucomannan has the average molecular weight of 20-200 ten thousand, the viscosity is too high, the solubility is too low, and the application of the glucomannan is greatly limited, the glucomannan is degraded by an enzyme degradation method, and a series of separation and purification methods are subsequently adopted, and finally the glucomannan with the medium molecular weight (the weight average molecular weight of 15300-17600) and the glucomannan with the low molecular weight (the weight average molecular weight of 6800-8500) are separated and obtained, so that the application possibility of the glucomannan is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
I. Medium molecular weight glucomannan
The invention provides medium molecular weight glucomannan, which is prepared by the following method: adding 10 parts of konjac refined powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 300-65U cellulase under the stirring state, carrying out enzymolysis for 48-60h under the conditions of the stirring rotation speed of 200-300r/min and the temperature of 60-65 ℃, carrying out enzyme deactivation in a boiling water bath for 15-20min, adding 10-15 parts of a gel-releasing agent, stirring for 3-5h, carrying out centrifugal separation, separating the obtained centrifugal liquid through a molecular sieve separation device, adding 30-50 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 3-5h, repeating 3-5 times of repeated precipitation-centrifugation-stirring as above, taking the precipitate obtained by the last centrifugation, and drying in a dryer to obtain the medium molecular weight glucomannan;
wherein, the height ratio of the separation column diameter of the molecular sieve equipment is 1 (30-50), the linear flow velocity is 8-10L/min, the particle diameter of the molecular sieve is 0.3-0.7mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1.2: 1;
wherein, the slow release solution is prepared from a citric acid solution and a sodium citrate solution with the concentration of 0.1 mol/L.
Examples
Example 1
A medium molecular weight glucomannan is prepared by the following steps: adding 10 parts of konjac refined powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 300U of cellulase under the stirring state, carrying out enzymolysis for 60 hours under the conditions of stirring rotation speed of 300r/min and temperature of 60-65 ℃, inactivating the enzyme in a boiling water bath for 15 minutes, adding 10 parts of a gel-releasing agent, stirring for 5 hours, carrying out centrifugal separation, separating the obtained centrifugal liquid through a molecular sieve separation device, adding 50 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 3 hours, repeating the steps of precipitating, centrifuging and stirring for 3 times as above, taking the precipitate obtained by the last centrifugation, and drying in a dryer to obtain the medium molecular weight glucomannan;
wherein the height ratio of the separation column diameter of the molecular sieve equipment is 1:30, the linear flow velocity is 10L/min, the particle diameter of the molecular sieve is 0.3-0.7mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1.2: 1;
wherein, the slow release solution is prepared from a citric acid solution and a sodium citrate solution with the concentration of 0.1 mol/L.
Tests show that the medium molecular weight glucomannan provided in this example has a weight average molecular weight of 15300-17600 and a purity of > 96.
Example 2
A medium molecular weight glucomannan is prepared by the following steps: adding 10 parts of konjac fine powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 500U of cellulase under the stirring state, carrying out enzymolysis for 50 hours under the conditions of stirring rotation speed of 200r/min and temperature of 60-65 ℃, inactivating the enzyme in a boiling water bath for 20 minutes, adding 13 parts of a gel-releasing agent, stirring for 4 hours, carrying out centrifugal separation, separating the obtained centrifugal liquid through a molecular sieve separation device, adding 40 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 5 hours, repeating precipitation-centrifugation-stirring for 5 times as above, taking the precipitate obtained by the last centrifugation, and drying in a dryer to obtain the medium molecular weight glucomannan;
wherein the height ratio of the separation column diameter of the molecular sieve equipment is 1:50, the linear flow velocity is 8L/min, the particle diameter of the molecular sieve is 0.3-0.7mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1.2: 1;
wherein, the slow release solution is prepared from a citric acid solution and a sodium citrate solution with the concentration of 0.1 mol/L.
Tests show that the medium molecular weight glucomannan provided in this example has a weight average molecular weight of 15300-17600 and a purity of > 96.
Example 3
A medium molecular weight glucomannan is prepared by the following steps: adding 10 parts of konjac refined powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 400U of cellulase under the stirring state, carrying out enzymolysis for 48 hours under the conditions of stirring speed of 270r/min and temperature of 60-65 ℃, inactivating the enzyme in a boiling water bath for 15 minutes, adding 10 parts of a gel-releasing agent, stirring for 3-5 hours, carrying out centrifugal separation, separating the obtained centrifugal liquid through a molecular sieve separation device, adding 30-50 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 4 hours, repeating the steps of precipitating-centrifuging-stirring for 4 times as above, taking the precipitate obtained by the last centrifugation, and drying in a dryer to obtain the glucomannan with the molecular weight of the medium;
wherein the height ratio of the separation column diameter of the molecular sieve equipment is 1:40, the linear flow velocity is 9L/min, the particle diameter of the molecular sieve is 0.3-0.7mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1.2: 1;
wherein, the slow release solution is prepared from a citric acid solution and a sodium citrate solution with the concentration of 0.1 mol/L.
Tests show that the medium molecular weight glucomannan provided in this example has a weight average molecular weight of 15300-17600 and a purity of > 96.
Low molecular weight glucomannan
The invention provides a low molecular weight glucomannan, which is prepared by the following method: adding 10 parts of konjac refined powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 300-65U cellulase under the stirring state, carrying out enzymolysis for 72-75h under the conditions of the stirring rotation speed of 200-300r/min and the temperature of 60-65 ℃, carrying out deactivation of enzyme in a boiling water bath for 15-20min, adding 7-10 parts of a gel-releasing agent, stirring for 3-5h, carrying out centrifugal separation, separating the obtained centrifugal liquid through a molecular sieve separation device, adding 30-50 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 3-5h, repeating 3-5 times of repeated precipitation-centrifugation-stirring as above, taking the precipitate obtained by the last centrifugation, and drying in a dryer to obtain the low-molecular-weight glucomannan;
wherein, the height ratio of the separation column diameter of the molecular sieve equipment is 1 (30-40), the linear flow velocity is 8-10L/min, the particle diameter of the molecular sieve is 0.3-0.5mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1: 1.
The preparation method is also characterized in that the slow release solution is prepared from a citric acid solution and a sodium citrate solution with the concentration of 0.1 mol/L.
Examples
Example 1
A low molecular weight glucomannan is prepared by the following steps: adding 10 parts of konjac fine powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 300U of cellulase under the stirring state, carrying out enzymolysis for 72 hours under the conditions of stirring speed of 300r/min and temperature of 60-65 ℃, inactivating enzyme in a boiling water bath for 15 minutes, adding 7 parts of a gel-releasing agent, stirring for 5 hours, carrying out centrifugal separation, separating the obtained centrifugal liquid through a molecular sieve separation device, adding 50 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 3 hours, repeating the steps of precipitating, centrifuging and stirring for 5 times as above, taking the precipitate obtained by the last centrifugation, and drying in a dryer to obtain the low-molecular-weight glucomannan;
wherein the height ratio of the separation column diameter of the molecular sieve equipment is 1:34, the linear flow velocity is 10L/min, the particle diameter of the molecular sieve is 0.3-0.5mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1: 1.
The preparation method is also characterized in that the slow release solution is prepared from a citric acid solution and a sodium citrate solution with the concentration of 0.1 mol/L.
Tests show that the low molecular weight glucomannan provided by the embodiment has the weight average molecular weight of 6800-8500 and the purity of more than 96.
Example 2
A low molecular weight glucomannan is prepared by the following steps: adding 10 parts of konjac refined powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 500U of cellulase under the stirring state, carrying out enzymolysis for 75 hours at the stirring rotation speed of 200r/min at the temperature of 60-65 ℃, adding 10 parts of a gel-releasing agent after carrying out enzyme deactivation in a boiling water bath for 17 minutes, stirring for 4 hours, carrying out centrifugal separation, separating the obtained centrifugal liquid through molecular sieve separation equipment, adding 30 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 4 hours, repeating the steps of precipitating, centrifuging and stirring for 3 times as above, taking the precipitate obtained by the last centrifugation, and drying in a dryer to obtain the low-molecular-weight glucomannan;
wherein the height ratio of the separation column diameter of the molecular sieve equipment is 1:40, the linear flow velocity is 9L/min, the particle diameter of the molecular sieve is 0.3-0.5mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1: 1.
The preparation method is also characterized in that the slow release solution is prepared from a citric acid solution and a sodium citrate solution with the concentration of 0.1 mol/L.
Tests show that the low molecular weight glucomannan provided by the embodiment has the weight average molecular weight of 6800-8500 and the purity of more than 96.
Example 3
A low molecular weight glucomannan is prepared by the following steps: adding 10 parts of konjac fine powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 400U of cellulase under the stirring state, carrying out enzymolysis for 73 hours under the conditions of stirring speed of 270r/min and temperature of 60-65 ℃, inactivating the enzyme in a boiling water bath for 20 minutes, adding 8 parts of a gel-releasing agent, stirring for 5 hours, carrying out centrifugal separation, separating the obtained centrifugal liquid through a molecular sieve separation device, adding 40 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 5 hours, repeating the precipitation-centrifugation-stirring for 4 times as above, drying the precipitate obtained by the last centrifugation in a dryer, and obtaining the low-molecular-weight glucomannan;
wherein the height ratio of the separation column diameter of the molecular sieve equipment is 1:30, the linear flow velocity is 8L/min, the particle diameter of the molecular sieve is 0.3-0.5mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1: 1.
The preparation method is also characterized in that the slow release solution is prepared from a citric acid solution and a sodium citrate solution with the concentration of 0.1 mol/L.
Tests show that the low molecular weight glucomannan provided by the embodiment has the weight average molecular weight of 6800-8500 and the purity of more than 96.
Efficacy compositions
The invention provides an efficacy composition which is prepared from the following raw materials in parts by weight: 1 part of low molecular weight glucomannan, 1 part of medium molecular weight glucomannan and 2 parts of rose hydrosol.
According to the invention, the effective compound which is easy to absorb and has the characteristics of water replenishing, moisture retaining and anti-aging is formed by compounding the low-molecular-weight glucomannan, which is easy to absorb transdermally, and the medium-molecular-weight glucomannan, which is easy to form a film and retain water, with the assistance of the nano-scale micromolecules which are both hydrophilic and oleophilic, namely the rose hydrosol.
Test for moisture retention
Weighing an efficacy composition, taking pure rose hydrosol, distilled water, 15 wt% glycerol aqueous solution, a reference sample 1 and a reference sample 2 as blank reference samples respectively, placing the solutions in weighing dishes respectively, placing the solutions in a constant-temperature moisture preservation box with the temperature of 25 ℃ and the relative humidity of 30% in an open manner, and calculating the moisture preservation rate, wherein the moisture preservation rate is m/m0 × 100%, m in the formula is the total mass of the weighing dishes before placing, and m0 is the total mass of the weighing dishes after placing;
wherein, the comparative sample 1 is prepared from the medium molecular weight glucomannan and the rose hydrosol provided by the invention according to the weight ratio of 1:1, and a comparison sample 1 is prepared by mixing the low molecular weight glucomannan provided by the invention and the rose hydrosol according to the weight ratio of 1:1 is formed by compounding.
The efficacy compositions of the present invention, the blank control, and the control, were tested for their moisturizing properties as shown in the following table:
as can be seen from the above table, the functional composition formed by compounding the high molecular weight glucomannan, the low molecular weight glucomannan and the rose hydrosol provided by the invention still has a good moisturizing effect after 24 hours.
IV radical scavenging test
In the invention, a system is determined after hydroxyl radical is generated by Fenton reactionAbsorbance value D at wavelength 536nmf(ii) a Replacing hydrogen peroxide in the reaction with equal volume of distilled water, repeating the test, and determining the absorbance value D of the system at the wavelength of 536nm0(ii) a Replacing hydrogen peroxide in the reaction with the functional composition with different volumes and concentrations, repeating the test, and determining the absorbance value D of the system at the wavelength of 536nmx(ii) a Replacing hydrogen peroxide in the reaction with the equivalent-volume effect composition, repeating the test, and determining the absorbance value D of the system at the wavelength of 536nmsAnd calculating to obtain the free radical clearance (%), wherein the calculation formula of the free radical clearance is shown as follows:
clearance rate ═ 1- (D)s-Dx)/(D0-Df)]*100％
The radical scavenging rate of the efficacy composition provided in the present invention calculated from the above formula is shown in the following table:
| clearance rate/%) | |
| Efficacy composition | 87.33 |
| Vc | 45 |
From the above table, the scavenging ability of the functional composition provided by the present invention to hydroxyl radicals is stronger than that of vitamin C (i.e. Vc in the above table), which is mainly because the molecular weight glucomannan molecular chain of the present invention introduces the biofunctional polysaccharide, so the functional composition provided by the present invention can effectively scavenge free radicals in the human body, so as to effectively slow down the aging of the human body.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A method for preparing medium molecular weight glucomannan, which is characterized by comprising the following steps: adding 10 parts of konjac refined powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 300-65U cellulase under the stirring state, carrying out enzymolysis for 48-60h under the conditions of the stirring rotation speed of 200-300r/min and the temperature of 60-65 ℃, carrying out enzyme deactivation in a boiling water bath for 15-20min, adding 10-15 parts of a gel-releasing agent, stirring for 3-5h, carrying out centrifugal separation, separating the obtained centrifugal liquid through a molecular sieve separation device, adding 30-50 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 3-5h, repeating 3-5 times of repeated precipitation-centrifugation-stirring as above, taking the precipitate obtained by the last centrifugation, and drying in a dryer to obtain the medium molecular weight glucomannan;
wherein, the height ratio of the separation column diameter of the molecular sieve equipment is 1 (30-50), the linear flow velocity is 8-10L/min, the particle diameter of the molecular sieve is 0.3-0.7mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1.2: 1.
2. The preparation method according to claim 1, wherein the sustained-release solution is prepared from a citric acid solution and a sodium citrate solution, both of which have a concentration of 0.1 mol/L.
3. An intermediate molecular weight glucomannan produced by the method of claim 1 or 2.
4. A method for preparing low molecular weight glucomannan, comprising the steps of: adding 10 parts of konjac refined powder into an enzymolysis liquid formed by preparing 30 parts of a slow release liquid with the pH value of 5.7 and 300-65U cellulase under the stirring state, carrying out enzymolysis for 72-75h under the conditions of the stirring rotation speed of 200-300r/min and the temperature of 60-65 ℃, carrying out deactivation of enzyme in a boiling water bath for 15-20min, adding 7-10 parts of a gel-releasing agent, stirring for 3-5h, carrying out centrifugal separation, separating the obtained centrifugal liquid through a molecular sieve separation device, adding 30-50 parts of absolute ethyl alcohol into the separated separation liquid, carrying out strong stirring for 3-5h, repeating 3-5 times of repeated precipitation-centrifugation-stirring as above, taking the precipitate obtained by the last centrifugation, and drying in a dryer to obtain the low-molecular-weight glucomannan;
wherein, the height ratio of the separation column diameter of the molecular sieve equipment is 1 (30-40), the linear flow velocity is 8-10L/min, the particle diameter of the molecular sieve is 0.3-0.5mm, and the molecular sieve material is resin before separation and transformation;
wherein the gel remover is formed by mixing sodium citrate and sodium salicylate according to the mass ratio of 1: 1.
5. The preparation method according to claim 4, wherein the sustained-release solution is prepared from a citric acid solution and a sodium citrate solution, both of which have a concentration of 0.1 mol/L.
6. A low molecular weight glucomannan produced by the method of claim 5 or 6.
7. The efficacy composition is characterized by comprising the following raw materials in parts by weight: 1 part of low molecular weight glucomannan, 1 part of medium molecular weight glucomannan and 2 parts of rose hydrosol.
8. The efficacious composition of claim 7 wherein said rose hydrosol is prepared by distillation from fresh rose damascena.
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