KR102300897B1 - Manufacturing method of solid phase schizandra concentration - Google Patents

Abstract

The present invention relates to a method for producing a solid Schisandra concentrate, and more particularly, to a method for preparing a solid Schisandra concentrate by extracting active ingredients from Schisandra by simulating the biomineralization process and preparing a solid concentrate. is about To this end, the solid Schisandra concentrate manufacturing method comprises: a first step of crushing Schisandra, mixing with ethanol, and extracting the active ingredient in Schisandra by ultrasonic waves; After cooling at room temperature, a second step of filtering the active ingredient; a third step of concentrating the filtrate to prepare a Schisandra extract; A fourth step of mixing after adding a solution containing calcium ions and a solution containing carbonate ions to the Schisandra extract; After centrifugation, a fifth step of washing with ethanol; and a sixth step of drying to prepare a solid Schisandra concentrate.

Description

Method for producing a solid Schisandra concentrate {MANUFACTURING METHOD OF SOLID PHASE SCHIZANDRA CONCENTRATION}

The present invention relates to a method for producing a solid Schisandra concentrate, and more particularly, to a method for preparing a solid Schisandra concentrate by extracting active ingredients from Schisandra by simulating the biomineralization process and preparing a solid concentrate. is about

The main physiologically active substances (medicinal ingredients) of omija are lignans, a type of polyphenol, and include schizandrin, gomisin A, and gomisin N. According to the Herbal Medicine Research Division, the content standard that the sum of schizandrin, gomisin A, and gomisin N is more than 0.7% when Schisandra fruit is extracted from the herbal medicine quality standardization data book. These physiologically active substances of Schisandra show a high difference in yield depending on the extraction method. In particular, when extracted with water, it is known that the content is 0.02 to 42% lower than when extracted with ethanol or methanol. Therefore, there is a need for a method to improve the extraction process or increase the concentration of the concentrate.

Biomineralization refers to the process by which living organisms make minerals, which often increases the hardness or strength of existing tissues. Such tissues are called mineralized tissues. Biomineralization is a very widespread phenomenon, with silicates in algae and diatoms, carbonates in invertebrates, and calcium phosphates and carbonates in vertebrates. Structural features, such as shells and bones of mammals and birds, are often created from these minerals. In terms of taxonomic distribution, the most common biomineral is calcium carbonate, which, together with organic polymers such as collagen and chitin, is used to structurally support bones and shells. The structures made of these biocomposites are highly controlled from the nanometer to the microscopic level, resulting in complex structures with diverse functions. The reason for considerable interest in understanding and elucidating biomineralization mechanisms regulated by organisms is the need to control mineral production in this way in applied materials engineering.

In particular, the biomimetic biomineralization process refers to mimicking nature's way of producing materials such as apatites. The phase of the mineral is not pure, but a complex material with organic parts is produced, which is controlled and participates in biomineralization. Therefore, various composite materials can be designed by combining organic materials and biomineralization processes, and these are designed together with organic materials, resulting in precipitation. Focusing on these processes, a method for preparing a Schisandra concentrate in a solid form was conceived by separating, purifying, and concentrating the Schisandra extract, which is an organic complex material.

Republic of Korea Patent Publication No. 10-2013-0050536

The present invention is to solve the above problems, and an object of the present invention is to overcome the disadvantages of the conventional manufacturing method showing a high difference in yield depending on the extraction method by focusing on the biomineralization process, and to overcome the disadvantages of the Schisandra concentrate in solid form An object of the present invention is to provide a method for preparing a solid Schisandra concentrate that can produce

These and other objects and advantages of the present invention will become apparent from the following description of preferred embodiments.

The object is, after crushing Schisandra, a first step of mixing with ethanol, and extracting the active ingredients in Schisandra by ultrasonic waves; After cooling at room temperature, a second step of filtering the active ingredient; a third step of concentrating the filtrate to prepare a Schisandra extract; A fourth step of mixing after adding a solution containing calcium ions and a solution containing carbonate ions to the Schisandra extract; After centrifugation, a fifth step of washing with ethanol; and a sixth step of drying to prepare a solid Schisandra concentrate.

At this time, in the first step, omiza and ethanol may be mixed in a weight ratio of 1: 5-15, and ultrasonic extraction may be performed at a temperature of 50-70° C. for 60-120 minutes.

In addition, in the third step, the Schisandra extract may be prepared by being concentrated at a temperature of 40-50° C. and a pressure of 60-80 mbar.

In addition, in the fourth step, the solution containing calcium ions is calcium chloride (CaCl ₂ ) aqueous solution, and the solution containing carbonate ions is ammonium carbonate ((NH ₄ ) ₂ CO ₃ ) aqueous solution. Preferably, calcium chloride (CaCl ₂ ) aqueous solution can be prepared by mixing 0.1 to 5.0 parts by weight of calcium chloride with respect to 100 parts by weight of distilled water, and ammonium carbonate ((NH ₄ ) ₂ CO ₃ ) aqueous solution is ammonium carbonate with respect to 100 parts by weight of distilled water. It can be prepared by mixing 0.1 to 5.0 parts by weight.

In addition, the drying of the sixth step may be performed at a temperature of 50 ~ 70 ℃.

In addition, between the third and fourth steps, mixing the Schisandra extract with beta-cyclodextrin (β-cyclodextrin) may further include; beta-cyclodextrin (β-cyclodextrin) is 100 parts by weight of distilled water It can be prepared by mixing 0.1 to 10.0 parts by weight of beta-cyclodextrin.

According to the present invention, it has the effect of effectively extracting a physiologically active substance (active ingredient) from Schisandra.

Specifically, by focusing on the biomineralization process and developing it, it is simpler than the conventional method, the yield is high, and has the effect of being able to prepare the Schisandra concentrate in a solid form.

Furthermore, the solid Schisandra concentrate prepared by the present invention can be applied to various fields such as food materials and cosmetic materials, and has the effect of contributing to the growth of the food industry and cosmetic industry.

However, the effects of the present invention are not limited to the above-mentioned effects, and other effects not mentioned will be clearly understood by those skilled in the art from the following description.

1 is a view schematically showing a method for preparing a solid Schisandra concentrate according to an embodiment of the present invention.
2 is an SEM photograph of the embodiment.
3 is an SEM photograph of a comparative example.
4 is a graph showing the BET surface area of the Example.
5 is an Isotherm linear plot graph of the embodiment.
6 is a graph analyzing the BJH adsorption characteristics of Examples.
7 is a graph analyzing the BJH desorption characteristics of Examples.
8 is a graph showing the PSA results of Examples.
9 is a graph showing the XRD analysis of Examples.
10 is a graph showing the TGA analysis of Examples.

Hereinafter, the present invention will be described in detail with reference to embodiments and drawings of the present invention. It will be apparent to those of ordinary skill in the art that these examples are only presented by way of example to explain the present invention in more detail, and that the scope of the present invention is not limited by these examples. .

Further, unless otherwise defined, 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, and in case of conflict, this specification, including definitions description will take precedence.

In order to clearly explain the invention proposed in the drawings, parts irrelevant to the description are omitted, and similar reference numerals are attached to similar parts throughout the specification. And, when a part "includes" a certain component, this means that other components may be further included, rather than excluding other components, unless otherwise stated. In addition, "unit" described in the specification means one unit or block that performs a specific function.

In each step, the identification number (first, second, etc.) is used for convenience of description, and the identification number does not describe the order of each step, and each step does not clearly describe a specific order in context. It may be performed differently from the order specified above. That is, each step may be performed in the same order as specified, may be performed substantially simultaneously, or may be performed in the reverse order.

1 is a view schematically showing a method for producing a solid Schisandra concentrate according to an embodiment of the present invention. Referring to FIG. 1 , a method for producing a solid Schisandra concentrate according to an embodiment of the present invention comprises: a first step of crushing Schisandra, mixed with ethanol, and extracting the active ingredients in Schisandra by ultrasonic waves; After cooling at room temperature, a second step of filtering the active ingredient; a third step of concentrating the filtrate to prepare a Schisandra extract; A fourth step of mixing after adding a solution containing calcium ions and a solution containing carbonate ions to the Schisandra extract; After centrifugation, a fifth step of washing with ethanol; and a sixth step of drying to prepare a solid Schisandra concentrate. The present invention focuses on the biomineralization process, which is simpler and has a higher yield than the conventional method, and has the effect of effectively extracting a physiologically active substance (active ingredient) from Schisandra Schisandra to produce a solid form of Schisandra concentrate. have

The first step is to extract the physiologically active substances in Schisandra, using ethanol as a solvent and ultrasonic extraction method. When ethanol is used as a solvent, a higher content of active ingredients can be extracted than when extraction is performed using water. Specifically, after crushing omija and mixing it with ethanol having a concentration of about 70% in a weight ratio of 1 : 5 to 15, the active ingredient can be extracted using ultrasound at a temperature of 50 to 70 ° C for 60 to 120 minutes. .

The second step is a step of cooling and filtering the liquid component containing the active ingredient extracted using ultrasonic waves at room temperature (meaning 20-30°C). At this time, a filtration membrane may be used for filtration, and various known filtration membranes may be used, and it is preferable to use a filtration membrane having pores of about 3.0 μm.

The third step is to prepare a Schisandra extract by first concentrating the filtrate containing the filtered active ingredient. In this case, the first concentration process may be performed at a temperature of 40-50° C. and a pressure of 60-80 mbar, and through this, a concentrated Schisandra extract can be prepared in a state in which the active ingredients are entangled with each other.

The process after the third step is to prepare a solid form of Schisandra concentrate by first separating and purifying the concentrated Schisandra extract, and further concentrating it.

The fourth step is a step of mixing after adding a solution containing calcium ions and a solution containing carbonate ions to the Schisandra extract prepared in the third step. Calcium ions and carbonate ions combine to form calcium carbonate, and the formed calcium carbonate surrounds the Schisandra extract. Accordingly, the Schisandra extract is separated from other components and precipitated. At this time, the solution containing calcium ions _{may use an aqueous solution of calcium chloride (CaCl 2} ), and the solution containing carbonate ions may use an aqueous solution of ammonium carbonate ((NH ₄ ) ₂ CO ₃ ), each in 100 parts by weight of distilled water. It is preferable to prepare by mixing 0.1 to 5.0 parts by weight of calcium chloride and 0.1 to 5.0 parts by weight of ammonium carbonate.

Preferably, between the third step and the fourth step, the step of mixing the Schisandra extract with beta-cyclodextrin (β-cyclodextrin) may be further included. By mixing Schisandra extract and beta-cyclodextrin (β-cyclodextrin), it can have the effect of further binding the hydrophobic active ingredient. Therefore, if the active ingredient extracted from Schisandra can be effectively combined, it is possible to use other solutions. It is preferable to use beta-cyclodextrin (β-cyclodextrin) prepared by mixing 0.1 to 10.0 parts by weight of beta-cyclodextrin with respect to 100 parts by weight of distilled water to effectively bind the hydrophobic component.

Step 5 is a step of centrifuging the Schisandra extract surrounded by calcium carbonate, followed by washing with ethanol. Centrifugation may use a known method under various conditions, and after centrifugation, it is preferable to wash at least twice with ethanol.

The sixth step is to prepare a solid Schisandra concentrate by drying the material washed with ethanol. Drying may use a dry oven, but is not limited thereto, and various drying methods may be used. The drying step is preferably performed at a temperature of 50 to 70° C., and by going through the drying step, a solid Schisandra concentrate can be obtained.

Hereinafter, the configuration of the present invention and its effects will be described in more detail through specific examples and comparative examples. However, these examples are for explaining the present invention in more detail, and the scope of the present invention is not limited to these examples.

[Material preparation]

Calcium chloride (CaCl ₂ ) and ammonium carbonate ((NH ₄ ) ₂ CO ₃ ) as necessary reagents were purchased from Sigma, beta-cyclodextrin (β-cyclodextrin, β-CD), and ethanol were purchased from Daejeong.

[Example]

A solid Schisandra concentrate was prepared in the following order.

1. After mixing 100 g of crushed omija with 1,000 g of 70% ethanol, the active ingredient was extracted using ultrasonic waves at 60° C. for 90 minutes.

2. After cooling the extracted active ingredient at 30° C., it was filtered using a 3.0 μm pore filtration membrane.

3. The filtrate was first concentrated at a temperature of 45° C. and a pressure of 70 mbar to prepare a Schisandra extract.

4. β-CD (1.2 g/100 mL DW) was put in a bottle and dissolved, mixed with 15 mL of a solution containing Schisandra extract, and stirred for 2 hours and 30 minutes.

5. Calcium chloride (CaCl ₂ , 1.1 g/100 mL DW) solution was added and stirred for 30 minutes.

6. Then, ammonium carbonate ((NH ₄ ) ₂ CO ₃ , 0.96 g/100 mL DW) solution was added and stirred for 10 minutes.

7. After centrifugation, it was washed twice with ethanol, and samples were collected.

8. The sample was put in a dryer (60° C.) and dried to prepare a solid Schisandra concentrate, and then stored at room temperature.

[Comparative example]

After performing only steps 1 to 3 of the above example, Schisandra extract was prepared.

[Experimental example]

SEM image analysis

SEM photographs of Examples and Comparative Examples were compared (see FIGS. 2 and 3).

While the Example showed the particle form, the Comparative Example showed the gel form.

BET surface area, BJH adsorption and desorption analysis

4 to 7 are diagrams analyzing the BET surface area, Isotherm linear plot, BJH adsorption, and BJH desorption characteristics of Examples, respectively, showing mesoporous characteristics with a ^{surface area of 5.559 m 2} /g and a pore volume of 0.015 cm ^{3 /g} confirmed that it has

Particle size analyzer (PSA) analysis

8 is a diagram showing the PSA results of Examples and shows the distribution of particle sizes. It could be confirmed that the average diameter was 17.59ㅁ19.46㎛, and it was a very irregularly shaped micro-sized particle.

XRD analysis

9 is a view showing the XRD analysis of the example, through which it can be confirmed that the example is an amorphous particle.

TGA analysis

10 is a view showing the TGA analysis of the example, and through this, it was confirmed that the organic matter derived from the primarily concentrated Schisandra extract (Comparative Example) was 73.44 wt%.

Analysis of concentration of bioactive substances

Tables 1 and 2 below are the results of analyzing the concentrations of Examples and Comparative Examples by HPLC, respectively. In the case of the comparative example, it was confirmed that the concentration was about 3.3 times to 8,680 ppm, whereas the concentration was 2,638 ppm.

[Table 1]

[Table 2]

In this specification, only a few examples among the various embodiments performed by the present inventors are described, but the technical spirit of the present invention is not limited or limited thereto, and it is of course that it may be modified and variously implemented by those skilled in the art.

Claims (10)

A first step of crushing Schisandra, mixing the crushed Schisandra with 70% concentration of ethanol, and extracting the active ingredient in Schisandra by ultrasonic wave at a temperature range of 50° C. to 70° C. for 60 minutes to 120 minutes;
After cooling at room temperature, a second step of filtering the active ingredient using a filtration membrane having a pore size of 3.0 μm;
a third step of concentrating the filtrate to prepare a Schisandra extract;
a fourth step of mixing the Schisandra extract with a beta-cyclodextrin solution prepared by mixing 0.1 to 10 parts by weight of beta-cyclodextrin with respect to 100 parts by weight of distilled water;
a fifth step of adding an aqueous solution of calcium chloride and an aqueous solution of ammonium carbonate to the omija extract mixed with the beta-cyclodextrin solution and then mixing;
After centrifugation, a sixth step of washing twice or more with ethanol; and
a seventh step of preparing a solid Schisandra concentrate by drying at a temperature of 50° C. to 70° C. using a dry oven;
A method for producing a solid omija concentrate, comprising: According to claim 1,
In the first step, omija and ethanol are mixed in a weight ratio of 1: 5-15, a method for producing a solid Schisandra concentrate. delete According to claim 1,
In the third step, the Schisandra extract is concentrated at a temperature of 40-50° C. and a pressure of 60-80 mbar. delete According to claim 1,
Calcium chloride (CaCl ₂ ) aqueous solution is prepared by mixing 0.1 to 5.0 parts by weight of calcium chloride with respect to 100 parts by weight of distilled water. According to claim 1,
Ammonium carbonate ((NH ₄ ) ₂ CO ₃ ) aqueous solution is prepared by mixing 0.1 to 5.0 parts by weight of ammonium carbonate with respect to 100 parts by weight of distilled water. delete delete delete

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