KR102276882B1 - manufacturing method for soap nut with supercritical extraction and composition having soap nut extracts - Google Patents

Abstract

The present invention relates to a soap nut supercritical extraction method and a soap nut extract composition. A method for manufacturing a soap nut supercritical extract comprises a step of supercritical-extracting dried soap nuts under a temperature of 30 to 60℃ and a pressure of 200 to 400 bar. By using the method for manufacturing a soap nut supercritical extract, an extract comprising a high content of crude saponin can be simply manufactured. A soap nut extract composition according to the present invention can be stored for a long time without addition of a chemical preservative.

Description

Soap nut supercritical extraction method and soap nut extract composition {manufacturing method for soap nut with supercritical extraction and composition having soap nut extracts}

The present invention relates to a method for supercritical extraction of soapnut and a composition for extracting soapnut.

Soapnut fruit is a natural fruit called soap nut or soapberry, a compound word of soap and nut. It contains saponin, has anti-inflammatory and antibacterial effects, and is widely used as a detergent.

Saponins are a group of compounds present in various plants, and their name is amphipathic glycoside, derived from the Latin word 'Sapo', meaning 'soap'.

Saponin is a glycoside of steroid, steroid alkaloid, or triterpene. It is a generic term for a substance that dissolves in water and exhibits a soapy foaming action. It exists in various plants and is a ginsenoside, a kind of saponin contained in ginseng. (ginsenoside) and eleutheroside are famous.

Korean Patent Application Laid-Open No. 2019-0118691 relates to an eco-friendly fabric softening functional detergent composition comprising a soapnut shell as an active ingredient, comprising the steps of: (a) drying and stabilizing the soapnut fruit; (b) removing the seeds of the dried soapnut fruit; and (c) pulverizing the softwood skins; disclosed a method for producing an eco-friendly fabric softening functional detergent comprising a softwood skins.

However, since the cleaning effect can be enhanced when the saponin contained in the soap nut is extracted and used separately, methods for extracting saponin from the soap nut with high efficiency have been studied.

Korean Patent No. 10-1087734 discloses a method for purifying saponin from a patient-free tree, a dichloromethane fraction of a patient-free tree, and a hair cosmetic composition comprising the same. Although it was possible to increase the content of saponin by additionally performing a dichloromethane fractionation process from the crude saponin extract, there is a problem in that the additionally performed fractionation step is cumbersome.

Korean Patent Application Laid-Open No. 10-2016-0052066 discloses a method for extracting saponin from the fruit of a patient-free tree and a cleaning composition comprising the same. This improved the yield of saponin extraction by adding inorganic powder when extracting the patient-free tree, but since the extract contains inorganic powder, it may act as an unwanted additive when used as a detergent, detergent, cosmetic, etc.

In addition, the liquid soap nut extracted as described above has a problem in that microbial contamination is often generated during storage.

Therefore, it is necessary to develop a method for extracting saponin, known as a cleaning component, from the soap nut in a high yield and storing it for a long time without microbial contamination.

Accordingly, as a result of the present inventors' efforts to solve the above problems, in the case of supercritical extraction of soapnut, an extract having a higher content of saponin than solvent extraction or hot water extraction can be obtained, In the case of using natural preservatives such as grass, primrose, honeysuckle, firefly, and dandelion extract, it was confirmed that long-term preservation is possible without the addition of chemical preservatives, and the present invention was completed.

An object of the present invention is to provide a method capable of extracting a high content of saponin from soapnut.

Another object of the present invention is to provide a soap nut extract composition capable of preventing microbial contamination even during long-term storage.

In order to achieve the above object, the present invention provides a method for preparing a supercritical softwood extract comprising the step of supercritically extracting dried soapnut at a temperature of 30 to 60°C and a pressure of 200 to 400bar.

In the present invention, the supercritical extraction is characterized in that the extraction is performed using supercritical carbon dioxide and water as solvents.

In the present invention, after centrifugation of the supercritical extract, it characterized in that it further comprises the step of filtering.

The present invention also includes a soap nut extract and a preservative, wherein the preservative is selected from the group consisting of nadosuyeong extract, satin grass extract, snow primrose extract, seaweed extract, firefly extract and dandelion extract, characterized in that it is selected from the group consisting of extracts. A composition is provided.

In the present invention, the soap nut extract is characterized in that it is selected from the group consisting of a solvent extract, a supercritical extract, and a hot water extract.

In the present invention, the preservative is characterized in that it contains 0.01 to 2 parts by weight based on 100 parts by weight of the soap nut extract.

In the present invention, the soap nut extract is characterized in that it contains 7 ~ 15g / 100g of saponin.

The present invention also provides an eco-friendly detergent composition comprising the soap nut extract composition.

The present invention also provides a cosmetic composition comprising the soap nut extract composition.

By using the method for preparing a soapnut supercritical extract according to the present invention, an extract containing a high content of saponin can be easily prepared, and the soapnut extract composition according to the present invention can be stored for a long time without the addition of chemical preservatives. .

1 is a component analysis result of a soapnut supercritical extract extracted according to an embodiment of the present invention.
2 is a component analysis result of the hot water extract of soapnut.
3 is a component analysis result of a soap nut solvent extract.
4 and 5 are photographs measuring the preservation effect of the soap nut extract composition prepared according to the present invention.

In the present invention, when the soap nut is supercritically extracted, an extract having a higher content of saponin than solvent extraction or hot water extraction can be obtained, and in the soap nut extract, nadosuyeong, satin grass, snow primrose, sea buckthorn, champignon, dandelion extract can be obtained. In case of using natural preservatives, such as, it was tried to confirm that long-term preservation is possible without adding chemical preservatives.

First, in the present invention, hot water extraction, solvent extraction, and supercritical extraction were performed using a soapnut. As a result, it was confirmed that the content of saponin was the highest during supercritical extraction.

Accordingly, the present invention relates to a method for preparing a supercritical soapnut extract comprising the step of supercritically extracting dried soapnut at a temperature of 30 to 60° C. and a pressure of 200 to 400 bar.

In the supercritical extraction step, when supercritical extraction is performed under a temperature or pressure condition outside the above range, there is a problem in that the saponin is not extracted from the soapnut or the yield is lowered even if it is extracted.

In the present invention, the supercritical fluid is not particularly limited, but carbon dioxide is more preferable. Carbon dioxide is a solvent mainly used in supercritical fluid extraction. After extraction, it is vaporized under atmospheric pressure and released into the atmosphere, so there is no residual solvent, so it is non-toxic and non-hazardous. It can be used to make products without contamination in food and pharmaceutical manufacturing industries. have.

In the present invention, supercritical extraction is characterized in that the extraction is performed using supercritical carbon dioxide and water as solvents in order to increase the extraction yield of the active ingredient. That is, the extraction yield can be increased by using water as an auxiliary solvent while performing extraction with the supercritical fluid.

The method for preparing the soapnut supercritical extract of the present invention may further include the step of filtering the supercritical extract after centrifugation. If filtration is not performed, impurities may be included and deteriorated easily during storage.

On the other hand, in the present invention, as preservatives, Nadosuyeong extract, satin grass extract, snow primrose extract, seaweed extract, firefly extract, and dandelion extract were added to the soapnut supercritical extract as preservatives, and it was confirmed that contamination of microorganisms does not occur even during long-term storage. did.

Therefore, the present invention includes a soap nut extract and a preservative, wherein the preservative is selected from the group consisting of Nadosuyeong extract, Satin grass extract, Snow primrose extract, S. to the composition.

In the present invention, the soap nut extract can be used without any particular limitation as long as saponin, an useful component, is extracted from the soap nut. For example, solvent extracts, supercritical extracts, hot water extracts, etc. can be used, and in consideration of the functional effect of saponins, it is preferable to use those containing 7-15 g/100 g of saponin. When the content of the saponin is less than 7 g per 100 g of the extract, there is a slight problem in the efficacy of the saponin.

In the present invention, the preservative is for improving the storability of the soap nut extract composition, and inhibits the generation of bacteria or fungi to increase the distribution and storage period and inhibit the invasion or propagation of harmful microorganisms from the outside ( Oxyria digyna ) extract, Sida spinosa extract, Primula modesta var.fauriae extract, seaweed ( Themeda triandra var.japonica ) extract, firefly ( Sanicula chinensis ) extract and Abelia mosanensis extract using it is preferable

The solvent of the extract may be water, alcohol, or a mixture thereof. C1 to C2 lower alcohol may be used as the alcohol, and 30% ethanol, 50% ethanol, 70% ethanol or methanol may be used as the lower alcohol. The extraction method may be reduced pressure high temperature extraction, hot water extraction, reflux extraction, hot water extraction, cold extraction, room temperature extraction, ultrasonic extraction or steam extraction, but is not limited thereto. The extraction may be performed by adding the extraction solvent 1 to 10 times based on the weight of the plant. The extraction temperature may be 30 to 100 ℃, but is not limited thereto. In addition, the extraction time may be 2 to 48 hours, but is not limited thereto.

The preservative may be included in an amount of 0.01 to 2 parts by weight based on 100 parts by weight of the soap nut extract. When the content of the natural preservative is less than 0.01 parts by weight, the preservative effect is insignificant, and when it exceeds 2 parts by weight, the natural flavor and color of the natural preservative may affect the application of the final product.

On the other hand, the soap nut extract composition of the present invention can be used as an eco-friendly detergent because it contains saponin, which is known to have a cleaning effect, and a natural preservative for its preservation.

Accordingly, the present invention relates to an eco-friendly detergent composition comprising a soap nut extract composition from another viewpoint.

As used herein, the term "environmentally friendly" means that it does not pollute or destroy the natural environment and goes well with the natural environment. Specifically, the detergent composition of the present invention uses a natural detergent component, so environmental pollution caused after washing can reduce the concerns of

The eco-friendly detergent means a detergent that does not contain any artificially synthesized material or contains an amount of 20 wt% or less. Also, "detergent" means capable of removing a contaminant. The detergent may be applied to a detergent selected from among kitchen cleaners, glass cleaners, bathroom cleaners, vehicle cleaners, household cleaners, stainless steel cleaners, food cleaners, clothes cleaners, and baby cleaners, but is not limited thereto. . Specifically, the detergent may be a detergent for clothes.

The eco-friendly detergent composition may include one or more additives selected from surfactants, moisturizers, thickeners, pigments and fragrance ingredients commonly used in detergents, provided that the cleaning power and fabric softening function are not reduced, and the added substances are Those that can be obtained from natural materials can be mainly used. Specifically, but not limited thereto, the composition may further include any one component selected from the group consisting of sancho, peppermint, rosemary, mint or coconut powder, and combinations thereof.

In the present invention, the soap nut extract composition of the present invention can be used as a cosmetic because it contains saponin, which is known to have anti-inflammatory and whitening effects, and a natural preservative for its preservation.

In another aspect, the present invention relates to a cosmetic composition comprising a soap nut extract composition.

The cosmetic composition of the present invention is an external skin ointment, cream, softening lotion, nourishing lotion, pack, essence, hair tonic, shampoo, conditioner, hair conditioner, hair treatment, gel, skin lotion, skin softener, skin toner, astringent, lotion , Milk Lotion, Moisture Lotion, Nourishing Lotion, Massage Cream, Nourishing Cream, Eye Cream, Moisture Cream, Hand Cream, Foundation, Nourishing Essence, Sunscreen, Soap, Cleansing Foam, Cleansing Lotion, Cleansing Cream, Body Lotion and Body Cleanser It may have a formulation selected from the group consisting of, but is not limited thereto. The composition of each of these formulations may contain various bases and additives necessary and appropriate for the formulation of the formulation, and the types and amounts of these components can be easily selected by those skilled in the art.

When the formulation of the present invention is a paste, cream or gel, animal fiber, vegetable fiber, wax, paraffin, starch, tracanth, cellulose derivative, polyethylene glycol, silicone, bentonite, silica, talc or zinc acid may be used as a carrier component. can

When the formulation of the present invention is a powder or a spray, lactose, talc, silica, aluminum hydroxide, calcium silicate or polyamide powder may be used as a carrier component, and in particular, in the case of a spray, additional chlorofluorohydrocarbon, propane /may contain propellants such as butane or dimethyl ether.

When the formulation of the present invention is a solution or emulsion, a solvent, solvating agent or emulsifying agent is used as a carrier component, for example, water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, propylene glycol, 1 ,3-butylglycol oil, glycerol aliphatic esters, fatty acid esters of polyethylene glycol or sorbitan, and the like.

When the formulation of the present invention is a suspension, as a carrier component, water, a liquid diluent such as ethanol or propylene glycol, a suspending agent such as ethoxylated isostearyl alcohol, polyoxyethylene sorbitol esters and polyoxyethylene sorbitan esters, microcrystalline Cellulose, aluminum metahydroxide, bentonite, agar or tracanth may be used.

When the formulation of the present invention is a surfactant-containing cleansing agent, aliphatic alcohol sulfate, aliphatic alcohol ether sulfate, sulfosuccinic acid monoester, isethionate, imidazolinium derivative, methyl taurate, sarcosinate, fatty acid amide as carrier components Ether sulfate, alkylamidobetaine, aliphatic alcohol, fatty acid glyceride, fatty acid diethanolamide, vegetable oil, linolin derivative or ethoxylated glycerol fatty acid ester and the like can be used.

[Example]

Hereinafter, the present invention will be described in more detail through examples. These examples are only for illustrating the present invention, and it will be apparent to those of ordinary skill in the art that the scope of the present invention is not to be construed as being limited by these examples.

Example 1: Preparation of Soapnut Supercritical Extract

4 kg of dried soap nut (origin: Nepal) and 40 L of water were placed in a supercritical extractor, and supercritical extraction was performed using carbon dioxide at 40° C., 300 (bar) for 6 hours. The extract was placed in a centrifuge and centrifuged at 5,000 rpm for 10 minutes, and then the skin and suspension of the softwood fruit were filtered to obtain 40L of the final supercritical extract.

Comparative Example 1: Preparation of Soapnut Hot Water Extract

100 g of dried soap nut (origin: Nepal) and 2 L of water were placed in a low-temperature vacuum extraction pot, and heated at 2 kg/cm 2 and 110° C. for 7 hours to obtain 1 L of hot water extract of soap nut.

Comparative Example 2: Preparation of Soapnut Solvent Extract

100 g of dried soap nut (origin: Nepal) is put in 0.5 L of ethanol and 0.5 L of purified water, and the first extraction is performed for 24 hours at room temperature, and then put again in 0.5 L of ethanol and 0.5 L of purified water in the soap nut, and the second is 24 hours at room temperature. extracted. 2L of the primary and secondary extracts were filtered, the filtered soapnut extract was put in a concentrator, and concentrated at 40°C at 70rpm at 70rpm until the soapnut liquid became thick, to finally obtain 1L of the soapnut extract.

The extracts prepared in Example 1, Comparative Examples 1 and 2 were requested to the Oriental Medicine Life Resource Research Center of Daegu Haany University, and the saponin content was analyzed, and the results are shown in Table 1 and FIGS. 1 to 3 below.

Ingredient name supercritical extract hot water extract solvent extract saponin 14.15g/100g 7.63g/100g 8.65g/100g

From Table 1, it was confirmed that the supercritical extract contains more saponin than the hot water extract and the solvent extract.

That is, it was found that, when using supercritical extraction, it was possible to obtain an extract containing a high content of saponin in an environmentally friendly and rapid manner.

Example 2: Preparation of natural preservatives

100 g of Nadosuyeong outpost, satin grass, snow primrose outpost, sea buckthorn outpost, firefly leaf, and dandelion stems, each of which was confirmed to have antibacterial effect through preliminary experiments, was crushed, placed in 1L of water, and extracted by heating at 70°C for 90 minutes, The first extract was obtained by filtration. After cooling the obtained primary extract to room temperature, the precipitated material was filtered through a filter paper to obtain a purified natural preservative extract.

Experimental Example 1: Storage evaluation

0.1ml and 1ml of the preservative extract prepared in Example 2 were respectively added to 100ml of the soapnut supercritical extract prepared in Example 1 to prepare a soapnut extract composition to which a preservative was added.

10ml of the soapnut extract composition added with a preservative is put in a Petri dish, exposed to air for 30 minutes, and then it is checked whether contamination of microorganisms occurs at room temperature for 2 months, and the results are shown in Table 2, FIGS. 4-5 shown in

division Preservative 0.1ml treatment 1ml preservative treatment 1 week 2 weeks 4 weeks 1 week 2 weeks 4 weeks Soapnut extract + Nadosuyeong extract × × × × × × Soapnut Extract + Satin Grass Extract × × △ × × × Soapnut Extract + Snow Primrose Extract × × × × × × Soapnut Extract+Seaweed Extract × × △ × × × Soapnut Extract + Charm Firefly Extract × × × × × × Soapnut Extract + Dandelion Extract × × × × × × Soapnut Extract △ ○ ○ △ ○ ○

○: Severe microbial contamination △: Weak microbial contamination ×: No microbial contamination

From Table 2 and Figures 4 to 5, when no preservative was added, the mold started to turn cloudy from the 7th to the 8th, and the black mold was clearly confirmed with the naked eye from 2 weeks. There was no microbial contamination in the extracts and dandelion extracts when 0.1 ml or 1 ml were contained, and when 0.1 ml of the extracts of Satin grass and seaweed extract were included, microbial contamination was weakly observed on the 4th week, but there was no microbial contamination when 1 ml was contained. could check

Therefore, it was confirmed that the soap nut extract composition of the present invention can be used as a detergent composition or a cosmetic composition because it has excellent storage stability while containing a high content of soap nut.

As the specific parts of the present invention have been described in detail above, for those of ordinary skill in the art, it is clear that these specific descriptions are only preferred embodiments, and the scope of the present invention is not limited thereby. will be. Accordingly, it is intended that the substantial scope of the present invention be defined by the appended claims and their equivalents.

Claims (9)

(a) supercritical extraction of the dried soap nut using carbon dioxide and water as solvents under a temperature of 30 to 60° C. and a pressure of 200 to 400 bar; and
(B) after centrifugation of the supercritical extract, a method for producing a saponin-containing soapnut supercritical extract comprising the step of filtering.
delete delete It includes a soap nut extract and a preservative, wherein the preservative is selected from the group consisting of nadosuyeong extract, satin grass extract, snow primrose extract, seaweed extract, firefly extract, and dandelion extract.
5. The composition of claim 4, wherein the soapnut extract is selected from the group consisting of a solvent extract, a supercritical extract, and a hot water extract.
[Claim 5] The soap nut extract composition according to claim 4, wherein the preservative is included in an amount of 0.01 to 2 parts by weight based on 100 parts by weight of the soap nut extract.
[Claim 5] The composition of claim 4, wherein the soap nut extract contains 7-15 g/100 g of saponin.
An eco-friendly detergent composition comprising the soap nut extract composition of claim 4.
A cosmetic composition comprising the soap nut extract composition of claim 4.

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