KR102161338B1 - Recovering Method of Essential Oil of Plant, Essential Oil Obtained therefrom, and Cosmetic Composition Comprising The Same - Google Patents

Abstract

The present invention comprises the steps of steaming the subject; Freezing the steamed subject; Performing an extraction process by placing the frozen object in a vacuum chamber maintained at 20° C. or less and -500 mmHg or less; And condensing the extract obtained through the extraction process to obtain a liquid essential oil. It relates to a method for recovering vegetable essential oils using vacuum extraction at a low temperature comprising the step of removing and purifying moisture using a non-polar trap.

Description

Recovery Method of Essential Oil of Plant, Essential Oil Obtained therefrom, and Cosmetic Composition Comprising The Same}

The present invention relates to a method for recovering vegetable essential oil, and more specifically, without using an organic solvent and water, using an essential oil recovery trap from vaporized gas during freeze-vacuum drying to efficiently remove moisture and purify and recover vegetable essential oil It is a technology that is very human-friendly because it does not apply organic solvents or heat, and can suppress decomposition or denaturation by heat. Bio-based solvent non-polar vegetable oils used in oil recovery traps are very economical and environmentally friendly. The vegetable essential oil thus obtained can be usefully used as a component constituting a composition such as food, cosmetics, and beverages.In the present invention, the method of efficiently removing moisture and purifying and recovering vegetable essential oils It is intended to provide a vegetable essential oil and a cosmetic composition comprising the same.

Korean ginseng (高麗人蔘), including wild ginseng, is a medicinal plant that has been widely used traditionally. It prevents dementia, anti-aging, improves sexual function, relieves symptoms of menopausal women, improves anti-cancer, immune function, anti-diabetes, and anti-fatigue. It is widely known for having a variety of functionalities, so even though it is expensive, it is characterized by a very thick consumer base that recognizes it as a premium well-being food.

Recently, ginseng essential oils are known to have an aroma therapy effect, and are processed into premium essential oils, soaps, and cosmetics as well as folk remedies.

Kitagawa et al. (1983) and Kim et al. (1984) found that the main fragrance components of ginseng are monoterpene and sesquiterpene, and this sesquiterpene is composed of azulene and menthene. Han et al. (2008) confirmed that the main compounds of ginseng essential oil extracted with hexane are hydrocarbon, aldehyde, sesquiterpene, sesquiterpene alcohol, acid, and ester. In addition, Han et al. (2008) reported that essential ginseng oil has excellent effects on acne bacteria ( Propionibacterium acne ), dandruff bacteria ( Pityrosporum ovale ), and fungi ( Candida albican ), but ginseng essential oil is a microorganism that causes various skin vitalization as above. As it has antibacterial and antifungal effects, it is highly likely to be developed as an expensive treatment for skin diseases.

The most common method of obtaining essential oil from ginseng on an industrial scale is to extract it under high temperature conditions using an organic solvent. However, such an extraction method may cause denaturation or decomposition of ginseng essential oil due to high temperature, and an additional process for completely removing the organic solvent is required for use in food or cosmetics. In addition, in the process of extracting ginseng essential oil, there is a problem in that functional components such as various saponins are lost, or major components of wild ginseng such as protein, starch, glucose, dietary fiber, and arabinose are discarded as processed by-products, so use an organic solvent. Obtaining essential oils from expensive ginseng is very uneconomical.

On the other hand, in a low-temperature vacuum condition, the temperature at which water or volatile essential oil vaporizes or sublimates is low, so denaturation or decomposition by heat does not occur, there is no need to directly add a solvent, and water and essential oil can be easily recovered from a low-temperature condenser. . In addition, in a vacuum condition at a low temperature, an organic solvent is not directly added to the edible part of ginseng, so no processing by-products are generated.

However, the obtained essential oil contains a high content of moisture. Since water can decompose essential oil components or cause problems of concentration, it must be separated from essential oil components, and therefore additional technology development for separating and purifying water is required.

It is an object of the present invention to provide a method for efficiently removing moisture and recovering vegetable essential oil from a gas vaporized (or sublimated) under a low-temperature vacuum condition without using an organic solvent and water using a refinery recovery trap.

Another object of the present invention is to provide a vegetable essential oil obtained by the above method.

Another object of the present invention is to provide a cosmetic composition containing as an active ingredient the vegetable essential oil obtained as described above.

The technical object of the present invention as described above is achieved by the following means.

(1) steaming the subject; Freezing the steamed subject; Performing a vaporization process by putting the frozen object in a vacuum chamber; And separating water from the gas obtained through the vaporization process using a refinery recovery trap and purifying and recovering the essential oil.

(2) In the above (1),

A method of recovering vegetable essential oil using an essential oil recovery trap, characterized in that the frozen object is placed in a vacuum chamber maintained at 20° C. or less and -500 mmHg or less to perform a vaporization process.

(3) In the above (1),

Removal of water from the vaporized gas and purification and recovery of essential oil is performed for 1 to 10 hours at 20 ℃ or less recovery method of vegetable essential oil using an essential oil recovery trap.

(4) In the above (1),

A method for recovering vegetable essential oil, wherein the temperature of the essential oil recovery trap is 20°C or less.

(5) In the above (1),

A method for recovering vegetable essential oil, characterized in that the material used in the essential oil recovery trap is a non-polar vegetable oil, a non-polar animal oil, a polar vegetable oil, or an oil obtained by mixing at least two or more of them.

(6) In (1) above,

The object is ginseng, wild ginseng, sesame leaves, angelica leaves, gosam, iris, or licorice recovery method of vegetable essential oil, characterized in that.

(7) Vegetable essential oil obtained by the method of any one of the above (1) to (6).

(8) A cosmetic composition comprising the vegetable essential oil of (7) as an active ingredient.

According to the present invention, since the vegetable essential oil is purified and recovered at low temperature without using an organic solvent and water, it is very human-friendly and can suppress decomposition or denaturation by heat, and the vegetable essential oil obtained thereby can be used in food, cosmetics, It provides an effect that can be usefully used as an ingredient constituting a composition such as a beverage. In addition, it is possible to efficiently separate moisture from the gas obtained through the gasification (or sublimation) process using an oil recovery trap, and to purify and recover vegetable essential oils.

1A is a process diagram of purification and recovery of vegetable essential oil from which moisture has been removed from vaporized gas generated in a low-temperature vacuum condition according to the present invention.
Figure 1b is an explanatory diagram of oil recovery using the oil recovery trap according to the present invention.
Figure 2 is a particle size and size distribution analysis results of the vegetable essential oil purified and recovered by the essential oil recovery trap according to the present invention.
3 is an analysis result of the change in particle size and size of vegetable essential oils purified and recovered by the essential oil recovery trap according to the present invention.
4 is a result of analysis of major volatile components of vegetable essential oils analyzed using gas chromatography mass spectrophotometry.

Hereinafter, the present invention will be described in detail.

The method for recovering vegetable essential oil according to the present invention comprises the steps of steaming a subject; Freezing the steamed subject; Performing a vaporization process by putting the frozen object in a vacuum chamber; And separating water from the gas obtained through the vaporization process using an oil recovery trap, and purifying and recovering the essential oil.

In the present invention, the "object" may be a part or the whole of any plant containing useful components, for example, leaves, stems, flowers or roots of the plant may all be extracted "objects". For example, ginseng or wild ginseng leaves, stems, and roots, as well as sesame leaves, angelica leaves, gosam, irises, licorice, garlic, ginger, cinnamon, jojoba, juniper berry, nutmeg, ylang-ylang, lemon, basil, aziwain Or, in addition to peppermint, various herbal medicines may be included here. Preferably, the object is wild ginseng.

In the present invention, in order to recover the vegetable essential oil, the subject is preferably steamed. Preferably, steaming is performed with steam at 100° C. for 5-20 minutes.

The steamed wild ginseng is subjected to freezing treatment, and freezing is preferably performed at -50°C or lower for 2 to 10 hours, more preferably 4 to 6 hours. Through this process, moisture contained inside the object is rapidly frozen.

The frozen object undergoes a vaporization process in a vacuum chamber as shown in FIG. 1A. In this process, preferably, a chamber in which the temperature is in a low temperature state of 20° C. or less and the pressure is maintained in a vacuum state of -500 mmHg or less is used. The object is put in this chamber and vaporization is performed for 24 to 96 hours, preferably for 48 hours. In the process of evaporation, the frozen moisture is evaporated and released from the inside of the object together with various aromatic components, and these vapors are introduced into the refinery recovery trap in order to separate the water and purify and recover vegetable essential oils at the rear end.

The essential oil recovery trap is preferably maintained at 20° C. or less, preferably -10 to 20° C., and the purified and recovered vegetable essential oil can be recovered after removing the essential oil recovery trap. The materials used in the oil recovery trap are non-polar vegetable oils (corn, soybeans, canola, olives, sunflowers, palms, walnuts, peanuts, flax, safflower, grape seeds, avocados, hemp seeds, cottonseed oil, etc.), non-polar animal oils ( It may be lard, tallow, milk fat, etc.), polar vegetable oils (macadamia, coconut, sunflower seeds, castor, almond oil, etc.), or an oil obtained by mixing these oils in an appropriate ratio. Preferably, the lipid used at this time contains antioxidants (eg, vitamin E, selenium, etc.).

The essential oil recovery trap used in the present invention is, as shown in the example of FIG. 1B, when a mixture of water and essential oil flows into the non-polar trap containing oil, the essential oil component dissolves in the oil and diffuses to the top of the oil layer. do. At this time, when the moisture diffused by the vacuum pump at the rear stage moves to the moisture recovery trap, the moisture is frozen and recovered. In the present invention, in the case of using an oil component generally used in cosmetics as the oil contained in the trap as described above, the oil component in the trap can be recovered as it is and used as a component of a cosmetic without the need to additionally separate essential oil components. In addition, when it is desired to separate only pure essential oil components, it is of course possible to separate essential oil components from trap oil components by conventional standard (or published) separation methods.

Preferably, in the present invention, the essential oil recovered as described above is separated and purified from the oil contained in the trap and the vegetable essential oil to be obtained using a fractional distillation method. At this time, the temperature of the fractionation still is preferably in the range of 40 to 60°C, and the vaporized vegetable essential oil can be recovered by passing through a condenser. The temperature of the condenser at this time is preferably in the range of 0-10°C. Finally, the separated and purified vegetable essential oil is preferably stored in a brown bottle at low temperature.

Although not shown, the oil recovery trap according to the present invention can be configured in series in multiple stages. That is, the water diffused in FIG. 1B is introduced into the oil refining trap at the rear stage, so that the remaining amount of essential oil that may be contained in the water can be recovered. Preferably, the oil recovery trap at the front is a non-polar trap (containing non-polar oil), and the oil recovery trap connected in series at the rear is configured as a polar trap (containing polar oil) to maximize separation efficiency.

The essential oil according to the present invention obtained as described above can be used as an active ingredient in a cosmetic composition.

The cosmetic composition containing the essential oil obtained in the present invention as an active ingredient is a skin external preparation formulation among cosmetics that can be applied to the skin.Paste, cream, gel, foundation, spray, essence, pack, soap, patch, spray, ointment, warning It may be prepared and used as a composition in the form of an external preparation for skin such as an agent, a lotion agent, a liniment agent, a pasta agent, or a cataplasma agent, but is not limited thereto.

When the formulation of the present invention is a paste, cream or gel, animal fiber, plant fiber, wax, paraffin, starch, tracant, cellulose derivatives, polyethylene glycol, silicone, bentonite, silica, talc, or zinc oxide may be used as carrier components. I can.

When the formulation of the present invention is a foundation or a spray, lactose, talc, silica, aluminum hydroxide, calcium silicate or polyamide powder may be used as a carrier component. In particular, in the case of a spray, additionally 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, a solvating agent or an emulsifying agent is used as a carrier component, such as water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, propylene glycol, 1 ,3-butylglycol oil, glycerol aliphatic ester, polyethylene glycol or fatty acid ester of sorbitan.

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

When the formulation of the present invention is a surfactant containing cleansing, as a carrier component, aliphatic alcohol sulfate, aliphatic alcohol ether sulfate, sulfosuccinic acid monoester, isethionate, imidazolinium derivative, methyltaurate, sarcosinate, fatty acid amide Ether sulfates, alkylamidobetaines, fatty alcohols, fatty acid glycerides, fatty acid diethanolamides, vegetable oils, linoline derivatives, or ethoxylated glycerol fatty acid esters may be used.

In addition, when the cosmetic composition according to the present invention is to be prepared as a cosmetic, the cosmetic may include a composition selected from the group consisting of water-soluble vitamins, fat-soluble vitamins, polymer peptides, polymer polysaccharides, sphingo lipids, and seaweed extract.

The cosmetic composition according to the present invention may further contain the above ingredients and other ingredients, which are usually blended in cosmetics, if necessary. Examples of the additives that can be added include stabilizers, fats and oils, moisturizers, emollients, surfactants, organic and inorganic pigments, organic powders, ultraviolet absorbers, preservatives, disinfectants, antioxidants, pH adjusters, alcohols, pigments, fragrances, and blood circulation accelerators. , Cooling agents, restrictive agents, and purified water.

In addition, the blending components that may be added are not limited thereto, and any of the above components can be blended within a range that does not impair the object and effect of the present invention, but preferably 0.01 to 5% by weight based on the total weight, further Preferably it may be blended in 0.01 to 3% by weight.

In the cosmetic composition according to the present invention, the blending amount of the essential oil according to the present invention is preferably 0.0001 to 20% by weight, more preferably 0.001 to 10% by weight based on the total weight of the composition, which is effective in less than 0.001% by weight. This is because there is a risk of a decrease, and if it exceeds 20% by weight, it is difficult to expect an increase in the effect even if blended.

Hereinafter, the contents of the present invention will be described in more detail with reference to preferred embodiments, but these embodiments are provided for explaining the contents of the present invention, and the scope of the present invention is not limited to these embodiments. .

[Example 1] Sanyangsam essential oil purification and recovery

In order to purify and recover the essential oil of wild ginseng, wild ginseng (including leaves and stems) was subjected to steaming for 20 minutes after removing foreign substances using distilled water. The steamed wild ginseng was frozen at -50°C for 5 hours. The frozen wild ginseng was vaporized in a vacuum chamber for 48 hours. At this time, the pressure and temperature of the chamber were maintained at -500 mmHg and 20°C, respectively, and the temperature of the oil recovery trap (containing corn oil) was 20°C. Corn oil containing sanyangsam essential oil was recovered after removing the essential oil recovery trap.

The recovered essential oil was separated and purified from corn oil and wild ginseng essential oil using a fractional distillation method. The temperature of the fractionation still proceeded in the range of 40 to 60°C, and the vaporized sanyangsam essential oil was recovered by passing through a condenser. The temperature of the condenser at this time was in the range of 0-10°C. Finally, the separated and purified sanyangsam essential oil was put in a brown bottle and stored at low temperature for use in the experiment.

In order to confirm the industrial applicability of wild ginseng essential oil, dispersion stability and particle size were analyzed. Sanyangsam essential oil was mixed with 2% of distilled water to prepare a homogeneous emulsion using a high pressure homogenizer.

[Example 2]

Essential oils were recovered in the same manner as in Example 1, except that the subject was made of sesame leaves.

[Example 3]

Essential oils were recovered by the same method as in Example 1, except that the subject was made of angelica leaves.

[Example 4]

Essential oil was recovered by the same method as in Example 1, except that the subject was used as Gosam.

[Example 5]

Essential oil was recovered by the same method as in Example 1, except that the subject was used as iris.

[Example 6]

Essential oil was recovered by the same method as in Example 1, except that the subject was licorice.

[Example 7]

Essential oil was recovered by the same method as in Example 1, except that the subject was made of garlic.

[Example 8]

Essential oils were recovered by the same method as in Example 1, except that the subject was made of ginger.

[Example 9]

Essential oil was recovered by the same method as in Example 1, except that the subject was cinnamon.

[Example 10]

Essential oil was recovered by the same method as in Example 1, except that the subject was used as jojoba.

[Example 11]

Essential oils were recovered in the same manner as in Example 1, except that the subject was juniper berry.

[Example 12]

Essential oil was recovered by the same method as in Example 1, except that the subject was used as nutmeg.

[Example 13]

Essential oils were recovered by the same method as in Example 1, except that the subject was used as ylang-ylang.

[Example 14]

Essential oils were recovered by the same method as in Example 1, except that the subject was lemon.

[Example 15]

Essential oil was recovered by the same method as in Example 1, except that the subject was made of basil.

[Example 16]

Essential oil was recovered by the same method as in Example 1, except that the subject was made Azwain.

[Example 17]

Essential oil was recovered in the same manner as in Example 1, except that the subject was made with peppermint.

[Experimental Example 1] Physicochemical Characteristics and Stability Analysis of Sanyangsam Essential Oil

The particle size size, which is a physicochemical characteristic of the sanyangsam essential oil obtained in Example 1, was measured using a particle size analyzer (Nano ZS, Malvern Co. Ltd., UK). Storage stability analysis of the essential oil of wild ginseng was confirmed by measuring the change in particle size at low temperature (10°C) for 10 weeks.

As a result of the experiment, the recovery rate of the sanyangsam essential oil recovered and purified by the essential oil recovery trap of Example 1 was 65%, and the volume mean particle size was 465 nm.

Extraction efficiency and particle size analysis result of sanyangsam essential oil extracted by low temperature vacuum extraction method Recovery efficiency (g/100g fresh ginseng) Volume average particle size (nm) 65±81 465.57±11.04

2 is a particle size distribution result of the essential oil of wild ginseng obtained in Example 1, and it can be seen that the particle size is uniformly distributed. In addition, Figure 3 shows the result of analyzing the particle size and size change of the essential oil of sanyangsam for 10 weeks. According to this, it was confirmed that the particle size increased from 465 nm to 602 nm, and the volume average particle size was 498 nm, which was very stable.

[Experimental Example 2] Analysis of Volatile Components of Sanyangsam Essential Oil Using Gas-Chromatography

In order to analyze the volatile content of the sanyangsam essential oil, hexane and sanyangsam essential oil were mixed at a ratio of 1:5, heated in a 50°C constant temperature water bath for 10 minutes, and then left at a low temperature for 24 hours to completely generate phase separation. After separating the supernatant (hexane layer) for volatile component analysis, the analysis was performed in the following manner.

Gas chromatography-mass spectrophotometry (7890A GC system, Agilent Technologies Inc., Palo Alto, CA, USA) was used to analyze the volatile content of the essential oil of wild ginseng. The detector and column were mass selective detector (5975C inert MSD) and DB-5 MS capillary column (30 m×250 um i.d., 0.25 um thickness, Agilent Technologies Inc., Palo Alto, CA, USA), respectively. Helium used as the mobile phase was flowed in split mode (split ratio = 5:1). The inlet temperature was 50°C and the oven temperature was 15°C/min. The interface temperature was 250°C and analyzed in scan mode (scan parameter 30-600 m/z).

4 shows chromatography, which is a result of analysis of volatile components in sanyangsam essential oil. The sanyangsam essential oil recovered and purified by an essential oil recovery trap after vaporization using a freeze-vacuum dryer under low temperature conditions contained β- panasinsene, cyclopropeazulene, spathulenol, alloaromadendrene, β- selinene, isopropyllidene, isospathulenol, etc. Such volatile components are mainly found in distilled extracts and are known to be the main components that exhibit ginseng flavor.

[Example 18] Preparation of Essence Containing Sanyangsam Essential Oil

Essence was prepared under the conditions shown in Table 2. Collagen was dissolved in purified water, heated and stirred at room temperature for 2 hours. Collagen, ethanol, glycerin, and purified water were mixed with the sanyangsam essential oil obtained in Example 1`, and a homogeneous essence was prepared using a high-speed homogenizer.

Conditions for Essence Composition Containing Sanyangsam Essential Oil Composition weight% Example 18 Comparative example Sanyangsam essential oil
Propylene glycol
glycerin
Sodium hyaluronate aqueous solution (1%)
ethanol
Polyoxyethylene hardened castor oil
Paraoxybenzoic acid methyl
Carbomer
Triethanolamine
incense
Purified water 10.0
10.0
10.0
5.0
5.0
1.0
0.1
0.3
0.4
0.1
Balance -
10.0
10.0
15.0
5.0
1.0
0.1
0.3
0.4
0.1
Balance

[Experimental Example 3] Viscosity Measurement of Essence Containing Sanyangsam Essential Oil

The physicochemical characteristics of the essence were confirmed by analyzing the viscosity and phase separation. The viscosity was analyzed at room temperature (25°C) using a viscosity meter (LVDV III Ultra, Brook filed Co. Ltd., USA).

Table 3 shows the results of comparing the effect on the physical properties and pH of the essence containing and without the sanyangsam essential oil of Example 18 (Comparative Example). When sanyangsam essential oil was added, viscosity and pH change were not affected.

Measurement results of physical properties and acidity of essence containing wild ginseng essential oil Viscosity (cP) pH Example 18 200.54±12.41 6.47±0.54 Comparative example 198.20±2.24 6.95±0.11

Conclusion: can be purified and recovered sanyangsam essential oil efficiently as essential oil recovery trap after vaporization sanyangsam essential oil from vacuum conditions of low temperature according to the invention as described above, the essential oil has a β main component showing a ginseng flavor of the key volatile -panasinsene, cyclopropeazulene, spathulenol, alloaromadendrene, β -selinene, isopropyllidene, isospathulenol, etc. were found to be contained. Sanyangsam essential oil was very stably dispersed at about 498 nm in aqueous solution, and as a result of measuring the storage stability for 10 weeks (70 days), no aggregation, precipitation, or floating phenomenon between the dispersed essential oil particles was confirmed. From these results, it is judged that sanyangsam essential oil exhibits a physicochemically stable dispersion characteristic and thus has a very high industrial value.

In addition, sanyangsam essential oil could be used as an essence for skin disease improvement, and sanyangsam essential oil did not affect the viscosity and pH changes of the essence.

As described above, the present invention has been described with reference to preferred embodiments of the present invention, but those skilled in the art can variously modify and modify the present invention within the scope not departing from the spirit and scope of the present invention described in the following claims. You will understand that you can change it.

Claims (8)

Steaming for 5 to 20 minutes with steam at 100°C for part or all of the plant; Freezing the steamed subject at -50°C or lower for 2 to 10 hours; Putting the frozen object in a vacuum chamber maintained in a vacuum state of 20° C. or less and -500 mmHg or less and performing a vaporization process for 24 to 96 hours; And separating moisture from the gas obtained through the vaporization process using a refinery recovery trap maintained at -10 to 20°C, and purifying and recovering the essential oil,
The oil recovery trap is a method of recovering vegetable essential oil using an essential oil recovery trap, characterized in that a non-polar trap containing a non-polar oil and a polar trap containing a polar oil are connected in series to purify and recover essential oil components. delete delete delete delete The method of claim 1,
Recovery method of vegetable essential oil, characterized in that the subject is ginseng, wild ginseng, sesame leaves, angelica leaves, gosam, irises, or licorice Vegetable essential oil obtained by the method of claim 1. A cosmetic composition comprising the vegetable essential oil of claim 7 as an active ingredient.

Images