KR102728256B1 - Extraction method of natural products using hot water extraction using distilled extract as an extraction solvent - Google Patents

Abstract

The present invention relates to a method for extracting a natural product, which comprises using a distillation extract of a first natural product as an extraction solvent to hot-water extract a second natural product, and to a hot-water extract extracted by the method. The method maximizes the extraction efficacy of useful components or active components of the second natural product, and the hot-water extract of the second natural product provides excellent skin efficacy.

Description

Extraction method of natural products using hot water extraction using distilled extract as an extraction solvent

This relates to a method for extracting natural products by hot water extraction using a distillation extract as an extraction solvent.

Most of the useful substances derived from natural products have physiological activities such as antiviral, antibacterial, and antioxidant abilities, and are attracting attention as ideal resources that can be developed into new effective substances. Because they are derived from natural products, they also have the advantage of being both effective and friendly to the human body.

Methods used to extract natural products include hot water extraction, which boils natural products directly using water to extract active ingredients contained in the natural products; distillation extraction, which extracts by spraying the steam produced by boiling water onto natural products; solvent extraction, which uses a solvent such as alcohol to dissolve and separate active ingredients from solid or liquid samples; supercritical extraction, which extracts using supercritical fluids; compression extraction, and ultrasonic extraction.

Meanwhile, the inventors of the present invention have tried to maximize the extraction efficiency of useful components derived from natural products and also to maximize the skin efficacy of the extracted extract. As a result, they used a distilled extract of natural products as a solvent instead of a general solvent, and confirmed the skin efficacy thereof, thereby completing the present invention.

One aspect is (1) a step of obtaining a distillation extract of the first natural product by distillation extraction of the first natural product; and

(2) A method for extracting a natural product is provided, comprising the step of using the distillation extract of the first natural product as an extraction solvent to extract the second natural product with hot water to obtain a hot water extract of the second natural product.

Another aspect provides a hot water extract of a second natural product using a distillation extract of a first natural product prepared by the above method as an extraction solvent.

Another aspect provides a cosmetic composition comprising a hot water extract of a second natural product using a distilled extract of a first natural product as an extraction solvent as an effective ingredient.

Other objects and advantages of the present application will become more apparent from the following detailed description, taken in conjunction with the appended claims and drawings. Anything not described in this specification will be omitted, as it is readily apparent to those skilled in the art or a similar art field of the present application.

Each description and embodiment disclosed in this application can also be applied to each other description and embodiment. That is, all combinations of various elements disclosed in this application fall within the scope of this application. In addition, the scope of this application cannot be considered limited by the specific description described below.

One aspect is (1) a step of obtaining a distillation extract of the first natural product by distillation extraction of the first natural product; and

(2) A method for extracting a natural product is provided, comprising the step of using the distillation extract of the first natural product as an extraction solvent to extract the second natural product with hot water to obtain a hot water extract of the second natural product.

The above method is characterized by using a distillation extract of a first natural product as an extraction solvent to hot-extract a second natural product, thereby maximizing the extraction efficacy of useful or active components of the second natural product.

The term “extract” as used herein includes a substance extracted from a natural product, regardless of the extraction method, extraction solvent, extracted component, or form of the extract, and includes a fraction obtained by fractionating the extracted substance with a specific solvent.

The above extract may be extracted from one or more selected from the group consisting of the whole plant, root, stem, branch, leaf, seed, and fruit of natural products, but is not limited to a specific part. The above natural product may be used as is without damaging its original form, or may be used after performing a pretreatment process in consideration of the process speed and process (manufacturing) efficiency intended by a person skilled in the art. The above pretreatment process may include, for example, conventional selection, washing, cutting, powdering, drying, etc.

In one specific embodiment, the first natural product may be Hamamelis virginiana , Hippophae rhamnoides , Pyrus malus , Oryza Sativa bran, Aloe vera leaf, Panax ginseng , or a combination thereof. In one specific embodiment, the first natural product may be Hamamelis virginiana leaves, stems, or whole plants, Oryza Sativa bran leaves, stems, or whole plants, Apple fruit, Rice bran, Aloe vera leaves, or Ginseng roots.

In one specific example, the first natural product and the second natural product may be the same or different. Accordingly, the second natural product may be at least one selected from the group consisting of Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf, ginseng, purslane, mugwort, green tea, and cypress.

The above natural product can be extracted through various methods such as distillation extraction, hot water extraction, cold extraction, reflux extraction, and ultrasonic extraction. Specifically, it can be extracted through a method of distillation extraction or hot water extraction. The above extract may mean a distillation extract or hot water extract of the natural product.

The above extract can be extracted with one or more solvents selected from the group consisting of purified water, C ₁ -C ₆ organic solvents, and subcritical or supercritical fluids. The C ₁ -C ₆ organic solvent may be one or more selected from the group consisting of C ₁ -C ₆ alcohol, acetone, ether, benzene, chloroform, ethyl acetate, methylene chloride, hexane, cyclohexane, and petroleum ether, but is not limited thereto.

In one specific example, the solvent for distillation extraction in step (1) may be purified water.

According to one experimental example, a method of hot-water extracting a second natural product using a distillation extract of a first natural product as an extraction solvent maximized the extraction efficiency of the active ingredients of the first natural product and/or the second natural product.

In the above step (1), the distillation extraction can be performed at 60°C to 90°C. For example, it can be performed at 60°C to 90°C, 60°C to 85°C, 60°C to 80°C, 60°C to 75°C, 60°C to 70°C, 60°C to 65°C, 70°C to 90°C, 70°C to 85°C, 70°C to 80°C, 70°C to 75°C, 80°C to 90°C, 80°C to 85°C, or 85°C to 90°C. If the temperature is too high, exceeding the above range, the active ingredient may be deteriorated, and if it is too low, below the above range, the active ingredient contained in the natural product may not be sufficiently dissolved in the extraction solvent.

In the above step (1), the distillation extraction can be performed by cooling the water vapor passing through the first natural product to 2°C to 10°C to obtain a distillation extract.

In the above step (2), the hot water extraction can be performed at 50°C to 90°C. For example, it can be performed at 50°C to 90°C, 50°C to 85°C, 50°C to 80°C, 50°C to 75°C, 50°C to 70°C, 50°C to 65°C, 50°C to 60°C, 60°C to 90°C, 60°C to 85°C, 60°C to 80°C, 60°C to 75°C, 60°C to 70°C, 60°C to 65°C, 70°C to 90°C, 70°C to 85°C, 70°C to 80°C, 70°C to 75°C, 80°C to 90°C, 80°C to 85°C, or 85°C to 90°C. If the temperature is too high, exceeding the above range, the active ingredient may deteriorate, and if it is too low, below the above range, the active ingredient contained in the natural product may not be sufficiently dissolved in the extraction solvent.

The distillation extraction of step (1) or the hot water extraction of step (2) may be performed for 1 to 5 hours, 1 to 4 hours, 1 to 3 hours, 1 to 2 hours, 2 to 5 hours, 2 to 4 hours, 2 to 3 hours, 3 to 5 hours, 3 to 4 hours, or 4 to 5 hours. If the extraction time is too long, exceeding the above range, the extraction efficiency may decrease and unnecessary components may be extracted, and if it is too short, less than the above range, a problem may occur in which the active ingredient cannot be sufficiently extracted.

The distillation extraction of the above step (1) or the hot water extraction of the step (2) can be performed by adding an extraction solvent of 10 to 100 times the total weight of the natural product. For example, it can be performed by adding 10 to 80 times, 10 to 50 times, 10 to 30 times, 30 to 100 times, 30 to 80 times, 30 to 50 times, 50 to 100 times, or 50 to 80 times. If the content is too much exceeding the above range, a problem may occur in which the content of the active ingredient may become relatively low, and if it is too little below the above range, a problem in which sufficient extraction is impossible may occur.

The above extract can then be filtered, concentrated, or dried to remove the solvent, and filtration, concentration, and drying can all be performed. For example, filtration can be performed using filter paper or a vacuum filter, concentration can be performed using a vacuum concentrator, and drying can be performed using a freeze-drying method, but is not limited thereto.

The above extract may then be further fractionated using a solvent selected from the group consisting of hexane, methylene chloride, acetone, ethyl acetate, ethyl ether, chloroform, water, and mixtures thereof. The temperature during the fractionation may be, but is not limited to, 4°C to 120°C.

Another aspect provides a hot water extract of a second natural product prepared by the above method using a distillation extract of a first natural product as an extraction solvent.

Another aspect provides a cosmetic composition comprising a hot water extract of a second natural product using a distilled extract of a first natural product as an extraction solvent as an effective ingredient.

Among the terms or elements mentioned in the description of the method for extracting the above natural product, those that are identical to those already mentioned are as described above.

In one specific example, the hot water extract of the second natural product using the distillation extract of the first natural product as an extraction solvent may have an increased content of active ingredients of the second natural product compared to the hot water extract using distilled water as an extraction solvent.

In one specific example, the first natural product is Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf, ginseng or a combination thereof;

The second natural product may be at least one selected from the group consisting of purslane, mugwort, green tea, and cypress.

According to one experimental example, the useful components of distilled extracts of Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf or ginseng all increased the contents of madecassoside, quercetin, catechin or polyphenol, although they were different from the useful components of centella asiatica, mugwort, green tea or cypress.

The above cosmetic composition may be used for improving skin health, improving skin beauty, or improving skin condition.

In one specific example, the cosmetic composition may include a hot water extract of a second natural product using a distilled extract of a first natural product as an extraction solvent as an active ingredient, so that the content of the active ingredient of the second natural product increases compared to a hot water extract using distilled water as an extraction solvent, thereby increasing skin efficacy.

The term "included as an effective ingredient" means that the ingredient is added to an extent that it can exhibit the effects mentioned in this specification, and includes formulation in various forms by adding various ingredients as auxiliary ingredients to increase skin efficacy and stabilize the formulation.

The hot water extract is present in an amount of 0.0001 wt% to 99.9999 wt% based on the total weight of the cosmetic composition, for example, 0.001 wt% to 80 wt%, 0.01 wt% to 60 wt%, 0.01 wt% to 40 wt%, 0.01 wt% to 30 wt%, 0.01 wt% to 20 wt%, 0.01 wt% to 10 wt%, 0.01 wt% to 5 wt%, 0.05 wt% to 60 wt%, 0.05 wt% to 40 wt%, 0.05 wt% to 30 wt%, 0.05 wt% to 20 wt%, 0.05 wt% to 10 wt%, 0.05 wt% to 5 wt%, 0.1 wt% to 60 wt%, 0.1 wt% to 40 wt%, It may be included in an amount of 0.1 wt% to 30 wt%, 0.1 wt% to 20 wt%, 0.1 wt% to 10 wt%, or 0.1 wt% to 5 wt%, but is not particularly limited thereto. The content of the effective ingredient may be selected as an appropriate content that can be formulated within a content range that can exhibit the effects mentioned herein by a person skilled in the art.

The above cosmetic composition can be prepared in a formulation including a toner (skin lotion), skin softener, skin toner, astringent, lotion, milk lotion, moisture lotion, nutrition lotion, massage cream, nutrition cream, moisture cream, eye cream, hand cream, foundation, essence, nutrition essence, eye essence, pack, soap, cleansing foam, cleansing lotion, cleansing cream, body lotion, body cream, body cleanser, suspension, gel, powder, paste, mask pack, or sheet or aerosol composition. A composition of such a formulation can be prepared according to a conventional method in the art.

The ingredients included in the above cosmetic composition may include ingredients commonly used in cosmetic compositions in addition to the composition as an effective ingredient, and may include, for example, conventional auxiliary agents and carriers such as stabilizers, solubilizers, vitamins, pigments, and fragrances.

A method of extracting a natural product of one aspect can maximize the extraction efficacy of useful or active ingredients of the second natural product by using a distillation extract of the first natural product as an extraction solvent and hot water extracting the second natural product.

The hot water extract of the second natural product extracted by the one-way method provides excellent skin efficacy.

Figure 1 is a schematic diagram of a method for extracting a natural product by using a distillation extract of a first natural product as an extraction solvent and hot-water extracting a second natural product.

Hereinafter, preferred examples are presented to help understand the present invention. However, the following examples are provided only to help understand the present invention more easily, and the content of the present invention is not limited by the following examples.

Experimental Example 1. Preparation of distilled extracts of Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf, or ginseng

In this experimental example, distillation extracts of Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf, or ginseng were prepared for use as extraction solvents for natural products.

First, (i) the leaves, stems, and whole plants of Hamamelis Virginiana, (ii) the leaves, stems, and whole plants of Zelkova serrata, (iii) the fruits of apples, (iv) rice bran, (v) aloe vera leaves, or (vi) the roots of ginseng were crushed to an average diameter of 5 cm or less. The crushed material was placed in an extraction vessel, and purified water was heated to a temperature of 60°C to 90°C so that steam was introduced into the extraction vessel. When the steam passing through the extraction vessel escaped from the extraction vessel, the steam was cooled and condensed to a temperature of 2°C to 10°C to obtain an extract. The above process was performed for 1 to 5 hours to obtain a distillation extract of Hamamelis Virginiana, Zelkova serrata, apples, rice bran, aloe vera leaves, or ginseng.

Experimental example 2. Obtaining extracts of natural products using distilled extracts as extraction solvents

Centella asiatica, mugwort, green tea, or thuja were extracted using distilled extracts of Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf, or ginseng as extraction solvents.

Specifically, the distillation extract of the above Experimental Example 1 was used as an extraction solvent to extract purslane, mugwort, green tea, or cypress at a temperature of 50°C to 90°C for 1 to 5 hours to obtain the final extract, which is an effective ingredient of a cosmetic composition.

Experimental Example 3. Confirmation of useful component content in the final extract

The content of useful components was confirmed in the final extract extracted with hot water using the distilled extract as an extraction solvent.

The contents of useful components in the final extracts extracted by hot water using distilled extracts of Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf, or ginseng as extraction solvents are shown in Tables 1 to 6, respectively. As a comparative group, an extract extracted by hot water using purified water as an extraction solvent was used, and the contents of useful components thereof are shown in Table 7.

Hot water extract using Virginia Clematis
Useful ingredients
(natural product) Example 1
(bottle grass) Example 2
(Eoseongcho) Example 3
(green tea) Example 4
(Cypress) Madecassoside of bottlebrush
(mg/100g) 364 Quercetin from Eoseongcho (mg/100g) 219 Green tea catechin (mg/100g) 6537 Cypress polyphenol (mg/100g) 3215

Hot water extract using vitamin tree water
Useful ingredients
(natural product) Example 5
(bottle grass) Example 6
(Eoseongcho) Example 7
(green tea) Example 8
(Cypress) Madecassoside of bottlebrush
(mg/100g) 389 Quercetin from Eoseongcho (mg/100g) 159 Green tea catechin (mg/100g) 5921 Cypress polyphenol (mg/100g) 2612

Using apple cider vinegar
Hot water extract
Useful ingredients
(natural product) Example 9
(bottle grass) Example 10
(Eoseongcho) Example 11
(green tea) Example 12
(Cypress) Madecassoside of the plant
(mg/100g) 317 Quercetin from Eoseongcho (mg/100g) 142 Green tea catechin (mg/100g) 6420 Cypress polyphenol (mg/100g) 2834

Using rice bran
Hot water extract
Useful ingredients
(natural product) Example 13
(bottle grass) Example 14
(Eoseongcho) Example 15
(green tea) Example 16
(Cypress) Madecassoside of bottlebrush
(mg/100g) 332 Quercetin from Eoseongcho (mg/100g) 172 Green tea catechin (mg/100g) 6103 Cypress polyphenol (mg/100g) 3092

Using aloe vera leaf water
Hot water extract
Useful ingredients
(natural product) Example 17
(bottle grass) Example 18
(Eoseongcho) Example 19
(green tea) Example 20
(Cypress) Madecassoside of bottlebrush
(mg/100g) 348 Quercetin from Eoseongcho (mg/100g) 192 Green tea catechin (mg/100g) 5892 Cypress polyphenol (mg/100g) 3123

Using ginseng water
Hot water extract
Useful ingredients
(natural product) Example 21
(bottle grass) Example 22
(Eoseongcho) Example 23
(green tea) Example 24
(Cypress) Madecassoside of the plant
(mg/100g) 324 Quercetin from Eoseongcho (mg/100g) 204 Green tea catechin (mg/100g) 6231 Cypress polyphenol (mg/100g) 2702

Hot water extract using purified water
Useful ingredients
(natural product) Comparative Example 1
(bottle grass) Comparative Example 2
(Eoseongcho) Comparative Example 3
(green tea) Comparative Example 4
(Cypress) Madecassoside of the plant
(mg/100g) 282 Quercetin from Eoseongcho (mg/100g) 125 Green tea catechin (mg/100g) 5720 Cypress polyphenol (mg/100g) 2432

According to Tables 1 to 7 above, the content of useful components was significantly increased in the final extract in which natural products were extracted using distilled extracts as a solvent compared to the extract in which natural products were extracted using purified water as a solvent. Specifically, in the case of Centella asiatica, the content of madecassoside increased in Examples 1, 5, 9, 13, 17, and 21 compared to Comparative Example 1, in the case of Houttuynia cordata, the content of quercetin increased in Examples 2, 6, 10, 18, and 22 compared to Comparative Example 2, in the case of green tea, the content of catechin increased in Examples 3, 7, 11, 19, and 23 compared to Comparative Example 3, and in the case of thuja, the content of total polyphenol increased in Examples 4, 8, 12, 20, and 24 compared to Comparative Example 4.

Experimental Example 4. Analysis of the content of indicator substances in distilled extracts

In this experimental example, the extraction efficiency of useful components by using distilled extracts as extraction solvents and hot water extraction was evaluated. Specifically, the distilled extracts of Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf, or ginseng were used as extraction solvents, and the index substance contents of extracts of Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf, or ginseng were again extracted with hot water.

Specifically, a distillation extract was prepared by the method of Experimental Example 1, and a hot water extract using the distillation extract was finally obtained by the method of Experimental Example 2. In this Experimental Example, a distillation extract using purified water or a hot water extract using purified water was used as a comparative group.

The results of evaluating the useful component content of the above hot water extract are shown in Tables 8 to 13 below.

Virginia Clematis
indicator substance Comparative Example 5
(distillation extraction) Comparative Example 6
(hot water extraction) Example 25
(Hot water extraction using distilled extract) Tannin (ppm) 10365 18315 32401

Vitamin tree
indicator substance Comparative Example 7
(distillation extraction) Comparative Example 8
(hot water extraction) Example 26
(Hot water extraction using distilled extract) Ascorbic acid
(mg/100g) 422 4782 5832

apologize
indicator substance Comparative Example 9
(distillation extraction) Comparative Example 10
(hot water extraction) Example 27
(Hot water extraction using distilled extract) Malsan
(mg/100g) 207 299 320

Rice bran
indicator substance Comparative Example 11
(distillation extraction) Comparative Example 12
(hot water extraction) Example 28
(Hot water extraction using distilled extract) Ferulic acid
(mg/100g) 1.3 1.5 2.1

Aloe vera leaves
indicator substance Comparative Example 13
(distillation extraction) Comparative Example 14
(hot water extraction) Example 29
(Hot water extraction using distilled extract) Total polyphenols
(mg/100g) 25.1 28.4 33.6

ginseng
indicator substance Comparative Example 15
(distillation extraction) Comparative Example 16
(hot water extraction) Example 30
(Hot water extraction using distilled extract) Ginsenoside Rg1
(mg/100g) 572 595 669

According to Tables 8 to 13 above, the index substances of extracts obtained by using distilled extracts of Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf, or ginseng as extraction solvents and then extracting Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf, or ginseng with hot water were found to increase significantly compared to extracts extracted by distillation or hot water with purified water.

Specifically, the contents of tannin in Virginia creeper, ascorbic acid in vitamin tree, malic acid in apple, ferulic acid in rice bran, total polyphenol in aloe vera leaf, and ginseng ginseng Rg1 increased compared to extracts distilled or hot water extracted with purified water.

In summary of the results of the above Experimental Examples 3 and 4, the method of using the distillation extract of the first natural product as an extraction solvent to extract the second natural product with hot water maximized the extraction efficiency of the useful components of the first natural product and/or the second natural product.

In addition, it was found that the useful components of distilled extracts of Virginia creeper, vitamin tree, apple, rice bran, aloe vera leaf or ginseng increased the contents of madecassoside, quercetin, catechin or polyphenol, although they were all different from the useful components of centella asiatica, mugwort, green tea or cypress.

The above description of the present invention is for illustrative purposes only, and those skilled in the art will understand that the present invention can be easily modified into other specific forms without changing the technical idea or essential characteristics of the present invention. Therefore, it should be understood that the embodiments described above are exemplary in all respects and not restrictive.

Claims (11)

(1) a step of obtaining a distillation extract of the first natural product by distillation extraction of the first natural product; and
(2) A method for extracting a natural product, comprising: a step of using the distillation extract of the first natural product as an extraction solvent to extract the second natural product with hot water to obtain a hot water extract of the second natural product;
The first natural product is Hamamelis virginiana , Hippophae rhamnoides , Pyrus malus , Oryza Sativa bran, Aloe vera leaf, Panax ginseng , or a combination thereof;
A method, wherein the second natural product is at least one selected from the group consisting of purslane, mugwort, green tea, and cypress.
delete A method for extracting a natural product according to claim 1, wherein in step (1), the solvent for distillation extraction is purified water.
A method for extracting a natural product according to claim 1, wherein in the step (1), the distillation extraction is performed at 60°C to 90°C.
A method for extracting a natural product according to claim 1, wherein in the step (2), the hot water extraction is performed at 50°C to 90°C.
delete delete A hot water extract of a second natural product using a distillation extract of a first natural product as an extraction solvent, prepared by the method of any one of claims 1, 3, 4 and 5.
A cosmetic composition comprising a hot water extract of a second natural product using a distilled extract of the first natural product of claim 8 as an extraction solvent as an effective ingredient.
A cosmetic composition according to claim 9, wherein the hot water extract of the second natural product using the distilled extract of the first natural product as an extraction solvent has an increased content of active ingredients of the second natural product compared to the hot water extract using distilled water as an extraction solvent.
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