KR20070021587A - Preparation method and their materials of soluble nano-sized beta Glucan from medicinal mushroom - Google Patents

Abstract

The present invention provides a water-soluble nano-sized particle size from the fruiting bodies and mycelium of medicinal mushrooms represented by Phellinus linteus, Sparassis crispa, Ganodederma lucidum, Agaricus blazei, and the like. It relates to a method for efficiently preparing beta glucan having. Specifically, medicinal mushroom fruiting bodies and mycelium are extracted with hot water while in-line rotating at high speed with a specially designed device in a circulating liquid phase, and after extraction, polymer pigments other than beta glucan are aggregated with a flocculant in a container and removed by centrifugation. It is a method for economically producing a high concentration of water-soluble nano-sized beta glucan to recover.

Medicinal mushrooms, mushrooms, mushrooms, agaricus, fruiting bodies, mycelium, water-soluble, nano-sized, inline high speed grinding, flocculant.

Description

Preparation method and extract of water-soluble nano-size beta glucan derived from medicinal mushrooms {Preparation method and their materials of soluble nano-sized beta Glucan from medicinal mushroom}

The present invention relates to a method for efficiently preparing a water-soluble nano-sized beta glucan from fruiting bodies and mycelium of medicinal mushrooms. Medicinal mushrooms include, but not necessarily, mushrooms, blossom mushrooms, ganoderma lucidum mushrooms and agaricus mushrooms.

Medicinal mushrooms contain abundant beta-glucans that form the cell wall in addition to general nutrients such as edible mushrooms, and have a large amount of dark or light pigments. It is also used as a diet food, and beta glucan has been found to have an antioxidant effect. In particular, it is recently used as a raw material for wrinkle improvement and whitening functional cosmetics.

In particular, beta glucan in mushrooms is water-soluble and non-water soluble. Water-soluble beta glucan is well extracted by general hot water extraction. However, water-insoluble beta glucan, which has a high molecular weight or is associated with chitin, has a separate treatment method, that is, hydrogen peroxide, high concentration sulfuric acid, It is known that some of the solubilization is required, although ultrasonic, and chemical, mechanical and enzymatic methods such as beta glucanase should be applied.

Hydrogen peroxide or high concentration of sulfuric acid and sonication is a method of randomly degrading beta1-3 or beta1-6 bonds of betaglucan to lower the molecular weight and solubilizing the polymer. Hydrolysis of -3, or beta 1-6 bonds.

However, the method using hydrogen peroxide and high concentration sulfuric acid is a material that is difficult to use as a food additive, or there is a risk of productivity degradation due to excessive decomposition. Ultrasonic extraction is a high-cost method that requires more than 48 hours even in a small volume of ultrasonic irradiation time. The method using glucanase is not economical because it uses expensive enzymes but the processing speed is very low.

In addition, when extracting mushrooms, a large amount of water-soluble pigments are also extracted. The method of removing the pigments by column method using an ionic resin in a laboratory is known, but it is expensive to remove a large amount of pigments by column method. It is not economical because the column must be large.

The method for producing beta glucan at nano size is introduced to obtain nano-sized fruiting body or mycelium by colliding dry fruiting body and dry mycelium at high temperature in cryogenic state, but this is the cost of maintaining cryogenic temperature and high speed collision energy. Because of its high consumption, it is uneconomical to process large quantities of fruiting bodies or mycelium. In addition, in order to extract beta glucan from nano-sized fruiting bodies or mycelium, nano-sized fruiting bodies or mycelium dry particles become swelled and condensed by viscous cell material during the extraction process, and it is necessary to disassemble the condensate again. In addition, since other materials other than beta glucan are also extracted and separated from the beta glucan, it is not efficient as a method for preparing pure beta glucan.

In the case of woody mushrooms, Ganoderma lucidum, and chaga, the total extraction rate including beta glucan is known to be less than 1% in hot water extraction, but the extraction yield is improved to about 20% by the same method as the above ultrasonic grinding method. There is an example. On the other hand, soft mushrooms, that is, mushrooms, agaricus, leaf mushrooms, such as the case of the usual extraction method is known to extract about 10% or about 10% if a separate method is added.

Medicinal mushrooms are usually expensive, so improving the extraction yield economically is an essential issue for efficient utilization of expensive resources.

The present invention improves the total extraction calculated by the amount of solids dissolved in the extraction solvent represented by water in the extraction process from the expensive medicinal mushrooms, while at the same time lowering the molecular weight of some polymer beta glucan in the liquid phase, polymer materials such as pigments and proteins Agglomerated and removed in the same vessel to produce a high value of water-soluble nano-sized beta glucan at a high concentration.

The present invention, while grinding the fruiting body or mycelium of medicinal mushrooms with an ordinary grinder to extract in the extractor while installing in-line high-speed rotary grinder between the separate circulation pipe to extract the swelling fruiting body or mycelium particles to the size of 300-600 mesh Increase the concentration of betaglucan.

When the extraction is completed, alum or cationic or anionic flocculant is added to an appropriate concentration to aggregate and precipitate a large amount of pigment and beta glucan of the water-insoluble polymer. The extract of the upper layer having a small amount of aggregate is centrifuged to take the supernatant, and the solid portion of the lower layer having a large amount of aggregate is filtered to collect the filtrate.

The supernatant and the filtrate are combined and concentrated to an appropriate concentration, and in a concentrated state where the volume is small, aggregates such as proteins are further precipitated, so it is centrifuged again to take the supernatant to obtain a liquid substance. This liquid substance contains some pigments other than beta glucan and low molecular weight substances, so that beta glucan is precipitated by high concentration alcohol and centrifuged to obtain purified beta glucan in the form of precipitate. It is dried by the phosphorus drying method to prepare a powder product.

The beta glucan thus prepared is 50-300 nm in the most frequent particles in a water-soluble and dissolved state again.

The production method of the present invention can be used to extract beta glucan from all mushrooms, such as shiitake mushrooms, matsutake mushrooms, ganoderma lucidum mushrooms, agaricus mushrooms, as well as shiitake mushrooms, leaf mushrooms and chaga mushrooms.

 The present invention will be described in more detail with reference to the following examples. However, in the examples, the mushroom weight, the amount of purified water, the extraction temperature, the concentration of the flocculant represented by alum and the like are for illustrating the present invention, but are not limited thereto.

Example 1 Extraction of Grinding Mushroom Powder after Grinding to 20-50 Mesh

 Situation of mushroom powder 20kg into a 1.5 ton extractor, 1000 liters of purified water, and then circulating the extract while maintaining the temperature at 100 ℃. 6 hours at 5000 rpm to obtain the maximum total extraction yield while changing the in-line ultra high speed grinder installed in the circulation pipe at a rotational speed of 1000 rpm to 8000 rpm for 0, 1, 2, 3 and 6 hours. Set to. The total extraction yield was measured by centrifuging the collected sample and inverting the solid content from the water content of the supernatant. Table 1

Example 2 Removal of Pigment in Situation Mushroom Extract

Centrifugation was carried out to 100 ml of extract extracted under the proper conditions so that the concentration of alum, which is a kind of flocculant, was 0-10%, and quantitative analysis of beta glucan in the supernatant by megazyme method. Set. Table 2

Experimental Example 1. Grain size analysis in aqueous mushroom solution

Zobetaglucan obtained under final titration was purified by alcohol to make 0.001-1% aqueous solution, and then the particle size analysis in the aqueous solution was performed. Table 3

Table 1. Change of Total Extraction Rate by Time by Rotational Speed

Rotation speed and time 0 hours (%) 1 hours(%) 2 hours(%) 3 hours(%) 6 hours (%) 1000 rpm 0 5 15 20 36 3000 rpm 0 12 24 34 45 5000 rpm 0 26 41 66 88 8000 rpm 0 31 48 79 90

      Table 2. The amount of beta glucan by the concentration of alum (mg / 100ml extract)

Amount of alum (%) (mg / 100ml) 0 0.1 One 5 10  Beta Glucan Extract (mg / 100ml) 0 65 148 107 82

      Table 3. Most frequent particle size analysis by beta glucan concentration

Beta-glucan concentration (%) 0.001 0.01 0.1 One Most frequent particle size (nm) 120 150 350 570

    Example 3. Extracting after crushing the mushroom mushroom powder to 20-50 mesh

    10 kg of the mushroom powder was added to a 1.5 ton extractor, 1200 liters of purified water was added, and the extract was circulated while maintaining the temperature at 80 ° C. 6 hours at 5000 rpm to obtain the maximum total extraction yield while changing the in-line ultra high speed grinder installed in the circulation pipe at a rotational speed of 1000 rpm-8000 rpm for 0, 2, 4, 6 and 8 hours. Set to. The total extraction yield was measured by centrifuging the collected sample and inverting the solid content from the water content of the supernatant. Table 4

    Example 4 Removing Pigment in Blossom Mushroom Extract

    Centrifugation was carried out to 100 ml of extract extracted under the proper conditions so that the concentration of alum, which is a kind of flocculant, was 0-5%, and quantitative analysis of beta glucan in the supernatant by megazyme method. Set. Table 5

    Experimental Example 2 Analysis of Particle Size in Aqueous Mushrooms

    Zobetaglucan obtained under the final titration conditions was purified by alcohol to make 0.001-1% aqueous solution, and the particle size analysis in the aqueous solution was performed. Table 6

Table 4. Change of Total Extraction Rate by Time by Rotational Speed

Rotation speed and time 0 hours (%) 1 hours(%) 2 hours(%) 3 hours(%) 6 hours (%) 1000 rpm 0 8 23 25 42 3000 rpm 0 20 31 38 51 5000 rpm 0 34 67 85 87 8000 rpm 0 40 80 87 88

      Table 5. The amount of beta glucan by the concentration of alum (mg / 100ml extract)

Amount of alum (%) (mg / 100ml) 0 0.1 One 5 10  Beta Glucan Extract (mg / 100ml) 0 21 40 36 20

      Table 6. Most frequent particle size analysis by beta glucan concentration

Beta-glucan concentration (%) 0.001 0.01 0.1 One Most frequent particle size (nm) 130 170 390 460

     [Experiment result]

    When extracting the situation mushrooms, the optimum rotational speed of the high-speed rotary grinder was 5000 rpm and the rotation time was 6 hours. This is about 176 times for the extraction rate of about 0.5% by the conventional hot water extraction method, and about 4,4 times improvement compared to about 20% for the improvement method such as ultrasonic waves. In the case of flowering mushrooms, the total extraction yield was 85% at 5000 rpm and 6 hours of rotation time. This yielded an extraction yield of 85 times higher than the yield of 1% of the general hot water extraction method and about 8 times higher than the improved ultrasonic extraction method.

    The concentrations of alum for the removal of pigments were 1% and 0.5% in case of situation mushroom and flower mushroom, respectively, and the concentration of beta glucan was 148 mg and 40 mg in 100 ml of extract, respectively. This is 1480 g of beta glucan recovered in 20 kg of the fruiting body fruit of the situation, about 41% of the water-soluble nano-sized beta glucan was recovered from 3.6 kg, which is an estimated 18% of the total beta glucan in the fruiting body. In the case of the flower mushroom, 4Kg of beta glucan was recovered from 10Kg of dried fruiting body, and 40% of the whole fruiting body was recovered as beta glucan.

    The particle size of the beta glucan was measured differently according to the concentration in the aqueous solution, and analyzed at a lean concentration of about 120-150 nm. This was confirmed as a result that satisfies the conditions that can be absorbed by the stomach should be a particle size less than 1um (micrometer).

The beta glucan purification method using the hot water extraction method using the inline high-speed rotary grinder according to the present invention and the flocculant such as alum are much more advanced and innovative and economical methods than the conventional hot water extraction method or the improved extraction method, and the total extraction rate and high purity water-soluble nano As a method for producing a large amount of beta glucan, edible and medicinal mushrooms such as matsutake mushrooms, situation mushrooms, ganoderma lucidum mushrooms, agaricus, leaf mushrooms and shiitake mushrooms can be economically utilized in cosmetics, foods and medicines. .

In addition, if the precipitated pigment aggregates after alum treatment to recover the co-precipitated water-soluble beta glucan can be obtained higher beta glucan yield.

Furthermore, the supernatant obtained by concentrating the supernatant treated with the flocculant, and distilling beta glucan from the alcohol and centrifuging it, has a number of useful water-soluble low molecular materials of mushrooms, which can be utilized as a new functional by-product.

Claims (4)

A method of extracting medicinal mushroom fruiting bodies and mycelium powders using an inline high speed mill.      Method of removing the pigment in the medicinal mushroom fruiting body and mycelium extract using a flocculant.      The nano-size water-soluble beta glucan according to claim 1 or 2, wherein medicinal or general mushrooms, such as ganoderma lucidum mushroom, agaricus mushroom, chaga mushroom, shiitake mushroom, etc., are used as raw materials in addition to the situation mushrooms and matsutake mushrooms. Manufacturing Method      Nano-size water-soluble beta of medicinal mushrooms and edible mushrooms, such as matsutake mushrooms, situation mushrooms, agaricus, ganoderma lucidum, chaga, shiitake and leaf mushrooms, respectively, extracted by claims 1, 2 and 3 Glucan