KR102098598B1 - Method for obtaining anthocyanin-containing water-soluble polysaccharide composite powder from purple corn bracts and sapphires using hydrolysis and antisolvent recrystallization - Google Patents

Abstract

The present invention relates to a method for obtaining an anthocyanin-containing water-soluble polysaccharide complex powder from purple cornella and genus using subcritical water hydrolysis and semi-solvent recrystallization. More specifically, when producing an anthocyanin-containing water-soluble polysaccharide complex, subcritical water hydrolysis that can improve the rate of acid hydrolysis of fibrin under a catalyst and semi-solvent recrystallization that can promote supersaturation of the hydrolyzate, is used Micropowdered water-soluble polysaccharide complexes containing high concentrations of anthocyanins can be recovered from corn bracts and coles, and the anthocyanin-containing water-soluble polysaccharide complex powders exhibit bioactive effects such as antioxidant, anti-inflammatory, and skin protection by UV exposure. Since it undergoes a micro-powdering process using semi-solvent recrystallization, the solubility in water is very high, so it does not require the use of ethanol to increase the solubility of the solubilizer and solubilizer used in the preparation of the cosmetic composition, and the unique odor of the raw material crop is obtained. Subcritical water hydrolysis and anti-solvent recrystallization that can be reduced From purple corn bracts and in using as it relates to the anthocyanin-containing water-soluble polysaccharide obtained composite powder method.
To this end, the present invention is a raw material preparation step of preparing a solvent containing powdered raw materials and purified water by preparing powdered bracts and cobs of purple corn; A mixing step of mixing the raw material and the solvent prepared in the raw material preparation step; A subcritical water hydrolysis step in which the mixed mixed pressure in the mixing step is introduced into the reactor and the conditions are pressurized and heated to a subcritical water environment to perform subcritical water hydrolysis; A filtration step of removing residues remaining in the subcritical water hydrolyzate after performing the subcritical water hydrolysis step; A semi-solvent recrystallization step of injecting the filtrate that has undergone the filtration step through an injection nozzle onto an anti-solvent inside a leach tank set to a specific temperature and specific concentration to induce rapid recrystallization; And an anthocyanin-containing water-soluble polysaccharide complex powder from sub-critical water hydrolysis and semi-solvent recrystallization using an anti-solvent recrystallization step to obtain a recrystallized product collected at the bottom of a needle line. Provides a method of obtaining.

Description

Method for obtaining anthocyanin-containing water-soluble polysaccharide composite powder from purple corn bracts and sapphires using hydrolysis and antisolvent recrystallization }

The present invention relates to a method for obtaining an anthocyanin-containing water-soluble polysaccharide complex powder from purple cornella and genus using subcritical water hydrolysis and anti-solvent recrystallization. More specifically, when producing an anthocyanin-containing water-soluble polysaccharide complex, subcritical water hydrolysis that can improve the rate of acid hydrolysis of fibrin under a catalyst and semi-solvent recrystallization that can promote supersaturation of the hydrolyzate, is used Micropowdered water-soluble polysaccharide complexes containing high concentrations of anthocyanins can be recovered from corn bracts and coles, and the anthocyanin-containing water-soluble polysaccharide complex powders exhibit bioactive effects such as antioxidant, anti-inflammatory, and skin protection by UV exposure. Since it undergoes a micro-powdering process using semi-solvent recrystallization, the solubility in water is very high, so it does not require the use of ethanol to increase the solubility of the solubilizer and solubilizer used in the preparation of the cosmetic composition, and the unique odor of the raw material crop is obtained. Subcritical water hydrolysis and anti-solvent recrystallization that can be reduced From purple corn bracts and in using as it relates to the anthocyanin-containing water-soluble polysaccharide obtained composite powder method.

Anthocyanin is a water-soluble light reddish-purple natural pigment that is known to have antioxidant properties, lower cholesterol, anti-cancer effects and anti-inflammatory properties, protect blood vessels, prevent arteriosclerosis and heart disease, suppress diabetes, and protect against UV rays. Also, recently, anthocyanin pigments delphinidin-3-glucoside (D3G), cyanidin-3-glucoside (C3G) and petunidin-3-glucoside (Pt3G) have the ability to inhibit lipid peroxidation by UV and inhibit tyrosinase activity that is involved in melanin production. Has been reported.

In general, anthocyanins are reported to be contained in large amounts in black beans, purple corn bracts, and genera, and are mainly extracted with methanol or ethanol. In addition, hydrochloric acid or organic acid is added to adjust the acidity to enhance the extraction effect. However, the extraction efficiency of anthocyanin pigments depends not only on the solvent, but also on the pH of the solvent, so to increase the extraction efficiency, the effect of the type and concentration of the extraction solvent and the acid added must be considered.

The existing anthocyanin extraction process is applied by using acid / base cross extraction using the anthocyanin solubility characteristics. In this process, acid / base compounds and inorganic salts remain in the production of the final product, and the solubility of anthocyanins and inorganic salts is similar, resulting in unstable yields during purification and poor product purity due to low purification yields.

Prior Art Document: KR Publication Patent Publication No. 2014-0089000 (2014.7.14. Publication)

The present invention has been devised to solve the above problems, and in particular, the use of organic solvents or stepwise solvent fractionation by recovering anthocyanin-containing water-soluble polysaccharide complexes from purple corn vesicles and genera using subcritical water hydrolysis and anti-solvent recrystallization. It can exhibit physiologically active effects such as antioxidant, anti-inflammatory, and skin protection by UV exposure without performing the process, and it undergoes a micropowdering process using anti-solvent recrystallization, so the solubility in water is very high. It is not required to use ethanol to increase the solubilizer and solubilizer solubility used in, and the anthocyanin-containing water-soluble polysaccharide complex from purple corn vesicles and genus using subcritical water hydrolysis and semi-solvent recrystallization that can reduce the peculiar odor of medicinal crops Purpose to provide a method for obtaining a powder There is this.

The method for obtaining anthocyanin-containing water-soluble polysaccharide composite powder from purple maize bracts and genera using subcritical water hydrolysis and semi-solvent recrystallization according to the present invention devised to achieve the above object is prepared by powdering the bracts and genera of purple corn And, a raw material preparation step of preparing a solvent containing the powdered raw material and purified water; A mixing step of mixing the raw material and the solvent prepared in the raw material preparation step; A subcritical water hydrolysis step in which the mixed mixed pressure in the mixing step is introduced into the reactor and the conditions are pressurized and heated to a subcritical water environment to perform subcritical water hydrolysis; A filtration step of removing residues remaining in the subcritical water hydrolyzate after performing the subcritical water hydrolysis step; A semi-solvent recrystallization step of injecting the filtrate that has undergone the filtration step through an injection nozzle onto an anti-solvent inside a leach tank set to a specific temperature and specific concentration to induce rapid recrystallization; It may include a powder recovery step of performing a semi-solvent recrystallization step to obtain a recrystallized product collected at the bottom of the needle bar.

In addition, the semi-solvent recrystallization step is performed to transfer the anti-solvent and the anti-solvent soluble cargo that have passed through the leaching tank to the separator to be separated into vapor and liquid at a temperature above the anti-solvent boiling point in the separator, and the vaporized anti-solvent is condenser. It may further include a semi-solvent recycling step to be condensed through and recycled to the leaching tank.

In addition, the subcritical water hydrolysis step may further include performing an reaction at a saturated water vapor pressure according to a temperature increase of 100 ° C. or more and 300 ° C. or less, so that acid hydrolysis is performed under a non-catalyst by ion-decomposing an organic material.

According to the present invention, when producing an anthocyanin-containing water-soluble polysaccharide complex, sub-critical water hydrolysis that can improve the rate of acid hydrolysis of fibrin under a catalyst and semi-solvent recrystallization that can promote supersaturation of the hydrolyzate, purple corn It is effective in recovering a micropowdered water-soluble polysaccharide complex containing a high concentration of anthocyanin from the bract and genus.

In addition, according to the present invention, the anthocyanin-containing water-soluble polysaccharide composite powder exhibits physiologically active effects such as antioxidant, anti-inflammatory, and skin protection by exposure to UV light, and undergoes a micropowdering process using anti-solvent recrystallization, solubility in water. It is very high and does not require the use of solubilizer and solubilizer used to increase the solubility of the solubilizer used in the preparation of the cosmetic composition, and has an effect in reducing the peculiar odor of the raw material crop.

In addition, according to the present invention, the acid / base compound and inorganic salts do not remain due to the use of subcritical water hydrolysis technology without using a toxic organic solvent and an acid or base catalyst and without undergoing a stepwise solvent fractionation process. There is no need to go through a separate removal process.

In addition, according to the present invention, as an eco-friendly process that can replace the conventional acid / base cross-extraction technology, it has an effect of excellent extraction and purification yield and ease of human safety.

In addition, according to the present invention, since the fine powdering technology using semi-solvent recrystallization can reduce raw material backlash and fine powder, additional deodorization and powdering processes are not added to the process, thereby reducing process operation cost and energy consumption. It has the effect of reducing.

1 is a process diagram of a method for obtaining an anthocyanin-containing water-soluble polysaccharide complex powder from purple cornella and genus using subcritical water hydrolysis and semi-solvent recrystallization according to a preferred embodiment of the present invention,
Figure 2 is a diagram showing the change in the dielectric constant and ionization constant of water according to the temperature change,
3 is a diagram showing a phase transformation path and a phase equilibrium diagram of water,
Figure 4 is the powder size of the anthocyanin-containing water-soluble polysaccharide composite powder prepared by a method for obtaining an anthocyanin-containing water-soluble polysaccharide composite powder from purple cornella and the genus using subcritical water hydrolysis and semi-solvent recrystallization according to a preferred embodiment of the present invention Photographs taken with analytical equipment (Field emission scanning electron microscopy.FE-SEM),
Figure 5 is a particle size distribution analysis of anthocyanin-containing water-soluble polysaccharide composite powder prepared by a method for obtaining anthocyanin-containing water-soluble polysaccharide composite powder from purple maize bladder and genera using subcritical water hydrolysis and semi-solvent recrystallization according to a preferred embodiment of the present invention Drawings showing graphs and tables,
Figure 6 is a view showing a comparison of the odor component analysis (VOCs) of the conventional extract and anthocyanin-containing water-soluble polysaccharide complex powder of the present invention,
Figure 7 is a photograph comparing the anti-inflammatory activity of the anthocyanin-containing water-soluble polysaccharide complex powder of the present invention and a positive control, and
Figure 8 is a diagram showing the cytotoxicity of the extract prepared by the present invention comparing the antioxidant activity and anti-inflammatory activity of the conventional extract and anthocyanin-containing water-soluble polysaccharide complex powder of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. First, it should be noted that in adding reference numerals to the components of each drawing, the same components have the same reference numerals as possible, even if they are displayed on different drawings. In addition, in describing the present invention, when it is determined that detailed descriptions of related well-known configurations or functions may obscure the subject matter of the present invention, detailed descriptions thereof will be omitted. In addition, a preferred embodiment of the present invention will be described below, but the technical spirit of the present invention is not limited to or limited thereto, and can be variously implemented by a person skilled in the art.

The present invention relates to a method for obtaining an anthocyanin-containing water-soluble polysaccharide complex powder (S100) from purple cornella and genus using subcritical water hydrolysis and anti-solvent recrystallization. More specifically, when producing an anthocyanin-containing water-soluble polysaccharide complex, subcritical water hydrolysis that can improve the rate of acid hydrolysis of fibrin under a catalyst and semi-solvent recrystallization that can promote supersaturation of the hydrolyzate, is used Micropowdered water-soluble polysaccharide complexes containing high concentrations of anthocyanins can be recovered from corn bracts and coles, and the anthocyanin-containing water-soluble polysaccharide complex powders exhibit bioactive effects such as antioxidant, anti-inflammatory, and skin protection by UV exposure. Since it undergoes a micro-powdering process using semi-solvent recrystallization, the solubility in water is very high, so it does not require the use of ethanol to increase the solubility of the solubilizer and solubilizer used in the preparation of the cosmetic composition, and the unique odor of the raw material crop is obtained. Subcritical water hydrolysis and anti-solvent recrystallization that can be reduced From purple corn bracts and in using as it relates to the anthocyanin-containing water-soluble polysaccharide obtained composite powder method (S100).

1 is a process diagram of a method for obtaining an anthocyanin-containing water-soluble polysaccharide complex powder (S100) from amethyst hydrolysis and semi-solvent recrystallization using a subcritical water hydrolysis and semi-solvent recrystallization, and FIG. 2 shows a change in temperature. A diagram showing the change in dielectric constant and ionization constant of water, FIG. 3 is a diagram showing a phase conversion path and phase equilibrium of water, and FIG. 4 is using subcritical water hydrolysis and anti-solvent recrystallization according to a preferred embodiment of the present invention This is a photograph of the powder size of the anthocyanin-containing water-soluble polysaccharide composite powder produced by the method for obtaining anthocyanin-containing water-soluble polysaccharide composite powder from purple cornella and the genus (Field emission scanning electron microscopy.FE-SEM), 5 is a subcritical water hydrolysis and semi-solvent recrystallization according to a preferred embodiment of the present invention. A graph showing a particle size distribution analysis graph and a table of anthocyanin-containing water-soluble polysaccharide composite powder prepared by a method (S100) for obtaining anthocyanin-containing water-soluble polysaccharide complex powder from salivary glands and genus, and FIG. 6 is a conventional extract and anthocyanin of the present invention FIG. 7 shows a comparison of odor component analysis (VOCs) of the water-soluble polysaccharide complex powder containing, and FIG. 7 is a photograph comparing the anti-inflammatory activity of the anthocyanin-containing water-soluble polysaccharide complex powder of the present invention and the positive control. It is a diagram showing the cytotoxicity of the extract prepared by the present invention comparing the antioxidant activity and anti-inflammatory activity of the extract and the anthocyanin-containing water-soluble polysaccharide complex powder of the present invention.

The method for obtaining an anthocyanin-containing water-soluble polysaccharide composite powder (S100) from purple maize bladder and genera using subcritical water hydrolysis and semi-solvent recrystallization according to a preferred embodiment of the present invention, referring to FIG. 1, is a raw material preparation step (S10) ), Mixing step (S20), subcritical water hydrolysis step (S30), filtration step (S40), semi-solvent recrystallization step (S50), semi-solvent recirculation step (S60), and powder recovery step (S70) Is done.

Hereinafter, the raw material preparation step (S10) will be described in detail.

The raw material preparation step (S10) is prepared by powdering the bracts and coles of purple corn containing anthocyanins, and weighing and preparing a solvent containing the powdered raw materials and purified water (water) at a weight ratio of 1: 5 or more and 30 or less. It is a step.

More specifically, in the raw material preparation step (S10), the ratio of the raw material and the solvent content is preferably prepared at least 5 times or more and 30 times or less as compared to the raw material, and when it is 5 times or less, the water content of the raw material to the solvent is This is because most of the solvent is absorbed by the raw material and smooth stirring is not performed. In the case of 30 times or more, when the amount of the solvent for the raw material is high, the extraction yield is high, but the solvent amount of 30 times or more has a significant effect on the extraction yield. This is because it does not exceed the economic ratio by causing an increase in the process operation cost.

The mixing step (S20) is a step of mixing the raw material and the solvent prepared in the raw material preparation step (S10) in a temperature range of 40 ° C or higher and 100 ° C or lower.

In more detail, when the mixing temperature of the mixing step (S20) is less than 40 ° C, the diffusion rate of the solvent into the raw material is slow, so that the execution time of the preliminary mixing step (S20) increases, and the mixing temperature exceeds 100 ° C. This is because it is impossible to reach a temperature of 100 ° C or higher based on atmospheric pressure.

The subcritical water hydrolysis step (S30) is a step of performing subcritical water hydrolysis by introducing the mixed pressure mixture in the mixing step (S20) into the reactor, and pressurizing and heating the conditions to the subcritical water environment.

In addition, the subcritical water hydrolysis step (S30) includes performing a reaction at a saturated water vapor pressure according to a temperature increase of 100 ° C. or more and 300 ° C. or less to ion-decompose an organic material to perform acid hydrolysis under a non-catalyst.

More specifically, subcritical water, called an ideal low-cost "green" solvent, has a wide range of temperatures and pressures, and the properties of water vary widely under these conditions.

For example, properties such as polarity, viscosity, and surface tension of water can be rapidly changed. By using these various properties, there is a great advantage that it can bring about the effect of extracting and removing specific substances without using an existing chemical solvent.

In addition, in the field related to the present invention, a supercritical fluid is a material at a temperature at a critical state in which two states of liquid and gas cannot be distinguished from each other, and a vapor pressure at this time, that is, a temperature and pressure higher than its critical point. When, that is, it means a fluid that is above the supercritical point. In addition, in the present invention, a sub-supercritical fluid means a fluid having a characteristic almost similar to that of a supercritical fluid.

Referring to FIG. 3, in general, the boiling point of water at 1 atmospheric pressure is 100 ° C. However, at high pressure, it remains liquid even at elevated temperatures. Water in this state is called subcritical water. When the temperature is raised to 374 ° C or higher, it becomes a supercritical water state. The subcritical fluid may be water, carbon dioxide (CO2), ethylene, ethane, propane, acetylene or ammonia, preferably more economical, free of harmful components, and can be safely disposed of, which is not only environmentally friendly but also extracted by the present invention It may be water that confirms conditions that can maximize efficiency, and more preferably, subcritical water. The subcritical water means water under subcritical condition.

The subcritical water used in the present invention is water at a temperature of 100 to 300 ° C and vapor pressure.

In addition, since the dielectric constant (ε) according to the temperature of the subcritical water is within the range of 15 to 50, it is similar to organic solvents such as methanol (ε = 32) and ethanol (ε = 24), so it has similar solubility characteristics to organic solvents. The dielectric constant of water at normal temperature and normal pressure is about ε = 79, and a material that is not soluble in water at normal temperature and normal pressure can also be dissolved and extracted in a subcritical state.

In particular, referring to FIG. 2, the ionization constant of water is an equilibrium constant that changes depending on temperature and pressure, and the ionization constant of water is at room temperature (25 at a pressure condition of 1 atm below 100 ° C and vapor pressure at 100 ° C or above. ℃) is 1.02 ^-14 (mol / L) ^2, but it rises rapidly with temperature rise, 4.90 ^-12 (mol / L) ² at 200 ℃ temperature, 478 times higher than room temperature, and 6.31 ^-12 (mol at 250 ℃ temperature) / L) ² , 616 times higher than normal temperature, 4.57 ^-12 (mol / L) ² at 300 ℃ temperature, 446 times higher than normal temperature, reaching the maximum at temperatures above 250 ℃ and below 300 ℃ and rapidly exceeding 350 ℃ The decrease can be confirmed through FIG. 2.

As a result, when the temperature is heated to a proper temperature (about 180 ° C or more and 250 ° C or less) by applying a pressure equal to or higher than the vapor pressure of water, the ionization constant of the ion concentration of water of the organic material becomes 3.0 × 10 ^-12 (mol / L) ² or more, The silver ion is decomposed to rapidly decompose the acid under the absence of a catalyst, and this process is a subcritical water hydrolysis step (S30).

Therefore, the effect of subcritical water hydrolysis cannot be expected at a temperature below 100 ° C, and at a temperature above 300 ° C, the effect of acid hydrolysis cannot be expected by decreasing the acidic ion content and increasing the concentration of hydroxyl ion content.

In addition, the subcritical water hydrolysis step (S30) performs subcritical water hydrolysis by pressing and heating the conditions in the reactor to a subcritical water environment. Here, the reactor input means is not limited.

The filtration step (S40) is a step of removing unreacted residue remaining in the subcritical water hydrolyzate after performing the subcritical water hydrolysis step (S30).

In the anti-solvent recrystallization step (S50), the filtrate subjected to the filtration step (S40) is passed through a spray nozzle and sprayed onto an anti-solvent inside a leaching tank set at a specific temperature and specific concentration to rapidly recrystallize. It is a step to induce.

The anti-solvent is a substance that precipitates a dissolved solute, and is introduced into an existing solution to interfere with the solubility between the solute and the solvent to promote supersaturation of the solute with respect to the existing solvent to exclude the solute from the solution. It acts as a second solvent.

The key operating conditions are the temperature and concentration of the antisolvent in the three-component system.

The preferred temperature is 40 ° C or more and 60 ° C or less, and if the temperature is less than 40 ° C, the rate of diffusion into the hydrolyzate is low compared to the rate of recrystallization of the solute by an anti-solvent, and the absorption rate of the solvent in the hydrolyzate is lowered, resulting in determination. There is a problem in that the content of the solvent mixed at the interface is high, and when it exceeds 60 ° C, the solubility of the solvent in the hydrolyzate to the antisolvent is high, and there is a problem in that the content of the antisolvent required for the supersaturation concentration increases.

In addition, the preferred anti-solvent concentration is a concentration of 20% or more and 80% or less compared to the reactants, and if it is less than 20%, the recrystallization reaction is not performed because the concentration of the supersaturation of the solvent in the hydrolyzate for the anti-solvent is not satisfied, 80 If it is more than%, the rate of recrystallization increases, but the particle size increases, which may result in difficulty in obtaining fine powder.

In addition, in the present invention, it is preferable to use an anti-solvent concentration compared to a reactant concentration of 30 brix or more.

The semi-solvent recirculation step (S60) is performed by performing the anti-solvent recrystallization step (S50) to transfer the semi-solvent and the anti-solvent soluble cargo that have passed through the leaching tank to the separator, and is separated into vapor and liquid at a temperature above the semi-solvent boiling point in the separator. , The vaporized anti-solvent is condensed through a condenser to be recycled to the leaching tank.

The anti-solvent is recovered separately at a temperature above the boiling point, the highest purity (approximately 90%) at the time of the first recovery, and the purity decreases as the cycle is repeated.

The powder recovery step (S70) is a step of performing a semi-solvent recrystallization step (S50) to obtain a recrystallized product collected at the bottom of the needle bar.

4, the powder size obtained by the powder recovery step (S70) of the present invention can be confirmed that the fine powder is obtained at 100nm (nanometer).

5, the particle size distribution analysis graph of the powder obtained by the powder recovery step (S70) of the present invention, the average particle size is 250.15nm, the most distributed particle size was 266.42nm.

In addition, referring to Figure 6, the odor component analysis (VOCs: volatile organic compounds) graph of the powder obtained by the powder recovery step (S70) of the present invention, the odor of the present invention, compared to the conventional extract, the lower the value of odor Can be seen.

Therefore, referring to FIGS. 4 to 6, since the micropowdering technology using the anti-solvent recrystallization of the present invention can reduce raw material backlash and fine powder, additional deodorization and powdering processes are not added to the process. There is an advantage that it can be a great help in reducing the process operation cost and reducing energy consumption.

< Example >

1> Raw material preparation step (S10): The raw material powder and purified water are weighed and put into a pre-mixer.

-Raw material and purified water content ratio (raw material (100 g): solvent (900 g) = 1: 9)

2> Mixing step (S20): a raw material and a solvent are mixed with a mixer. (75 ± 5 ℃ / 60rpm / 10 min.)

3> Subcritical water hydrolysis step (S30): The premixed raw material solution is introduced into a subcritical water reactor, and the conditions in the reactor are pressurized and heated to a subcritical water environment to perform subcritical water hydrolysis. (50 bar, 250 ℃ / 60 min.)

4> Filtration step (S40): After the subcritical water hydrolysis reaction is finished, the raw material in the reactor is discharged through an outlet and the filtrate through which the unreacted residue is removed through filtering is passed through. (3 to 5 micron filter)

5> Anti-solvent recrystallization step (S50): Rapid recrystallization is induced by spraying the subcritical water hydrolysis filtrate through a 5 micron fine spray nozzle into a semi-solvent phase inside a leaching tank set at 40 ° C. The concentration of anti-solvent inside the leaching tank is continuously supplied to maintain more than 50%.

6> Anti-solvent recirculation step (S60): after the anti-solvent recrystallization, the anti-solvent and the anti-solvent soluble cargo that have passed through the leaching tank are transferred to a separator, separated into vapor and liquid at a temperature above the non-solvent boiling point in the separator and vaporized The anti-solvent is condensed through a condenser and then recycled to the leaching tank.

7> Powder recovery step (S70): The anti-solvent recrystallized material is collected in a filtration filter at the bottom of the leaching tank, and is obtained by decomposing the lower portion of the leaching tank for recovery.

< Experimental group >

Referring to FIG. 7, a total of 6 experimental rats were used in this experiment, and were classified into six groups. Indomethacin (: steroid-based anti-inflammatory agent) (30 mg / ml) was applied to only one group, and the other 5 groups were hydrolyzate derived from purple corn bracts and genera, that is, water-soluble polysaccharides containing anthocyanins (1, 25, 50, 75, 100 mg). / Ml) was applied to the rat's ear.

[Positive control group]

One group was coated with Indomethacin (30 mg / ml), a well-known nonsteroidal anti-inflammatory agent.

[Voice control group]

In the remaining 5 groups, anti-inflammatory activity was measured immediately after application of the hydrolyzate to the experimental mice (0 hours) and 10 hours later.

In addition, referring to Figure 8, the powder of the present invention has been confirmed that the antioxidant activity (DPPH), anti-inflammatory activity (NO assay) is higher than the value of the conventional extract, the antioxidant activity and anti-inflammatory activity is superior to the conventional, cytotoxicity (MTT assy).

The above description is merely illustrative of the technical idea of the present invention, and those of ordinary skill in the art to which the present invention pertains may make various modifications, changes, and substitutions without departing from the essential characteristics of the present invention. will be. Therefore, the embodiments and the accompanying drawings disclosed in the present invention are not intended to limit the technical spirit of the present invention, but to explain the scope of the technical spirit of the present invention. . The scope of protection of the present invention should be interpreted by the claims below, and all technical spirits within the scope equivalent thereto should be interpreted as being included in the scope of the present invention.

S10-Raw material preparation stage
S20-mixing stage
S30-subcritical water hydrolysis step
S40-Filtration step
S50-anti-solvent recrystallization step
S60-anti-solvent recycling step
S70-powder recovery step
S100-Purple corn bract using subcritical water hydrolysis and anti-solvent recrystallization and
Method for obtaining water-soluble polysaccharide complex powder containing anthocyanin from the genus

Claims (3)

A raw material preparation step of preparing the bracts and cobs of purple corn by powdering, and preparing a solvent containing powdered raw materials and purified water in a weight ratio of 1: 5 to 30;
A mixing step of mixing the raw material and the solvent prepared in the raw material preparation step at a temperature of 40 ° C or higher and 100 ° C or lower;
A subcritical water hydrolysis step in which the mixed mixed pressure in the mixing step is introduced into the reactor and the conditions are pressurized and heated to a subcritical water environment to perform subcritical water hydrolysis;
A filtration step of removing residues remaining in the subcritical water hydrolyzate after performing the subcritical water hydrolysis step;
A semi-solvent recrystallization step of injecting the filtrate that has undergone the filtration step through an injection nozzle onto an anti-solvent inside a leach tank set to a specific temperature and specific concentration to induce rapid recrystallization;
The semi-solvent recrystallization step is performed to transfer the semi-solvent and the anti-solvent soluble cargo that have passed through the leaching tank to the separator to separate into vapor and liquid at a temperature above the anti-solvent boiling point in the separator, and the vaporized anti-solvent condenses through a condenser. A semi-solvent recycling step to be recycled to the leaching tank; And
Powder recovery step of performing a semi-solvent recrystallization step to obtain recrystallization trapped at the bottom of the needle bar
Including,
The subcritical water hydrolysis step
The reaction is carried out at saturated water vapor pressure according to a temperature increase of 100 ° C or more and 300 ° C or less, so that the organic material is ion-decomposed to undergo acid hydrolysis under a non-catalyst.
It includes,
The anti-solvent concentration in the anti-solvent recrystallization step is 20% or more and 80% or less compared to the reactants that are filtrates that have undergone the filtration step.
Including,
The anti-solvent temperature is between 40 ℃ and 60 ℃
Method for obtaining an anthocyanin-containing water-soluble polysaccharide complex powder from purple cornella and genus using subcritical water hydrolysis and semi-solvent recrystallization. delete delete

Images