KR20110018166A - Natural antiseptic compositions containing propolis, lavender essetial oil and lemon essential oil - Google Patents

Abstract

PURPOSE: A natural antiseptic composition is provided to remove the smell of propolis which is difficult to use in cosmetic products and to apply in cosmetics or detergents. CONSTITUTION: A natural antiseptic composition contains 0.3-2% of propolis, 0.045-0.3% of lavender essential oil, and 0.045-0.3% of lemon essential oil. The composition also contains 5% of ethanol as a solvent, 0.5% of polysorbate 20 as a solubilizer, 0.5% of polysorbate 80, and PEG(60) hydrogen-added castor oil. The composition further contains sodium coco PG-dimonium chloride phosphate or 1,3-butylene glycol as a moisturizer, and linoleamido propyl PG-dimonium chloride phosphate as a softener.

Description

NATURAL ANTISEPTIC COMPOSITIONS CONTAINING PROPOLIS, LAVENDER ESSETIAL OIL AND LEMON ESSENTIAL OIL}

The present invention relates to natural preservative compositions containing propolis, lavender essential oil and lemon essential oil, which can be applied to household goods, in particular cosmetics or detergents.

Cosmetics and detergents have continued to develop with human history. They aim to clean the body, to express themselves beautifully and attractively by make-up, etc. as human instinct desires, to enrich the mind, to prevent aging to protect the skin and hair from ultraviolet rays and dryness, and to clean the surrounding objects. In order to protect the body from harmful bacteria, etc., it is an essential household product that is indispensable in real life.

Cosmetics and detergents consist mainly of oil and water, and cosmetics in particular contain amino acid derivatives and proteins as nitrogen sources such as glycerin and sorbitol, which are carbon sources of microorganisms. Therefore, microorganisms, such as mold and bacteria, are likely to penetrate similarly to foods with similar ingredients. Compared to food, cosmetics have a long life span, so the risk of microbial change is not comparable to food. Therefore, cosmetics are easily contaminated from fingers, etc., and need to be protected for a long time from the decay and odor caused by microorganisms, and thus have to use preservatives.

Preservatives are formulated into cosmetics to inhibit the growth of microorganisms that contaminate cosmetics from the outside and kill the microorganisms over time to prevent product changes. However, the US FDA, Japan's Ministry of Health and Welfare and the Korea Food and Drug Administration are controversial on the safety level to regulate the limit of preservatives, and there are so many problems that the harmful effects of preservatives are reported on the news media. This is weighted.

In spite of these problems, when preservatives are not used, more and more problems occur, such as deterioration of products, contamination of microorganisms, and germs that are harmful to humans.

Therefore, an object of the present invention is to provide a natural preservative applicable to household goods such as cosmetics, which can overcome the above problems.

In order to solve the above problems, the present invention provides a natural preservative composition containing both propolis, lavender essential oil, lemon essential oil.

In addition, the present invention is a natural preservative further comprising a solubilizer, such as polysorbate 20, polysorbate 80, and PEG (60) hydrogenated castor oil for the solubilization of the propolis and herbal essential oil, and a solvent To provide a composition.

Hereinafter, the present invention will be described in detail.

Propolis is a fat-soluble complex obtained from honeycomb. It is a resinous, sticky, rubbery form made by bees gathering honeybees that secrete to protect the growth of various buds and trees and mix them with their own salivary gland secretions. It has been used as a substance to fill the entrance or gap of the honeycomb with the material to reinforce the inside of the honeycomb, to make the honeycomb aseptic due to its strong sterilizing power, and to prevent the invasion of harmful microorganisms. Since the millennium, it has been used in medicine because it has been found in various fields such as antibacterial, anti-tumor, anti-inflammatory, and free radical removal.

Propolis contains about 50 ~ 55% of viscous resin, about 30% of wax, about 8 ~ 10% of essential oils, about 5 ~ 10% of pollen esters, about 20 amino acids, and perpenoids Species flavonoids are included.

There is no restriction on the type of propolis that can be used in the present invention, but preferably Propolis EEP100 of Seoul Propolis Co., Ltd. Propolis EEP100 is obtained by removing the yellow wax phase from the honeycomb and leaching and filtering in alcohol. It is a mixture of many kinds and has a characteristic of mixing well in ethanol but not mixing well with water and oil.

Currently, propolis is mainly used for health foods, and is also used as an antibacterial material for soaps and cosmetics. However, Bacillus subtilis subtilis ), Proteus vulgaris ) and Bacillus alvei showed strong antimicrobial activity, and Salmonella gallinarum ) and S. dublin have been reported to be effective, but it was difficult to use it alone to use the antiseptic effect. There was a disadvantage of being reluctant to use.

Despite its excellent antiseptic properties, herbal essential oils are used to eliminate the fragrance of propolis, which is not suitable for cosmetics or detergents.

Herb is a generic term for green plants that benefit from food, beauty, medicinal, fragrances, insect repellents, preservatives and deodorants. You can take oil from these helpful plants and take advantage of their unique properties. This oil is called essential oil. There are many essential oils that have various effects listed above, among which lavender and lemon are used in various ways.

Lavender is a very important kind of herb. Its fragrance and softness make it the nickname of herb queen. Lavender essential oil is generally used as a fragrance ingredient in soaps, cosmetics, perfumes, and many other foods such as ice cream, candy, bread, and gum. In addition, it is known to have antimicrobial, antifungal and bactericidal effects.

Lemon is a citrus-based fruit that is used a lot in real life. It is very sour and tastes fresh. Essential oils squeezed out of the shell are used as fragrances in cosmetics and detergents. It also has antimicrobial activity against E. coli, which also acts as an antibacterial agent.

Lavender essential oil is a pure oily mixture extracted by wet distillation, and lemon essential oil is a pure oily mixture extracted by cold pressing. The two essential oils also do not mix with water, and the oil may mix well depending on the type, or may float or sink depending on the specific gravity difference.

The propolis, lavender essential oil, lemon essential oil are the main ingredients in exhibiting the antiseptic effect of the present natural preservative composition.

The present natural preservative composition may preferably contain about 0.3 to 2% of propolis, about 0.045 to 0.3% of lavender essential oil, and about 0.045 to 0.3% of lemon essential oil.

The natural preservative composition may include a solubilizer to help dissolve the propolis, lavender essential oil and lemon essential oil.

The type of solubilizer suitable for the present invention is not particularly limited, but preferably polysorbate 20, polysorbate 80, PEG-60 hydrogenated castor oil, and more preferably polysorbate 20 of Southeast Synthetic. And Polysorbate 80, PEG (60) hydrogenated castor oil from Nihon Emulsion.

PEG-60 hydrogenated castor oil, a solubilizer, is a material that has a great effect on the formulation in the form of a paste. Generally, the solubility is improved as the amount is increased, but the feeling applied to the skin is stiff. Therefore, since the content of PEG-60 hydrogenated castor oil included in the natural preservative of the present invention has a great effect on the feeling of use, formulation form, and quality of the product, it is necessary to use the content recommended in the present invention.

The present natural preservative composition may include about 0.5% of polysorbate 20 and about 0.5% of polysorbate 80 as a solubilizer, and PEG (60) hydrogenated castor oil in the above composition ratio contains 0.45% or more. Should be.

In addition, the solvent for the present natural preservative composition may contain about 5% of ethanol.

On the other hand, the present invention relates to a product comprising a natural preservative composition, including all products that can exert an antiseptic effect, including natural preservatives, that is, cosmetics, detergents, food, pharmaceuticals, household goods, etc. Use is preferred.

Suitable formulations and additives can be used in accordance with methods well known to those skilled in the art to produce products comprising the present natural preservative compositions.

Cosmetics containing the present natural preservative composition further comprises a moisturizer, a softener, a surfactant, and the like, specifically, in the present invention, sodium coco PG-dimonium chloride phosphate or 1,3-butylene glycol as a moisturizing agent, and linol as a softener. Reamidopropyl PG-dimonium chloride phosphate may be used.

As an embodiment of the cosmetic of the present invention, facial cleansing, facial cleansing, cleansing cream, cleansing lotion, massage cream, latex, lotion, cream, hair treatment, hair cream and the like.

Natural preservative composition of the present invention by containing propolis, lavender essential oil and lemon essential oil has the advantage of excellent antiseptic effect and harmless to the human body while solving the unique scent of propolis difficult to use in cosmetics, cosmetics or detergents It can be applied to household goods.

Preferred examples are provided to aid the understanding of the present invention but are not intended to limit the invention to the following examples.

In the present invention, a natural preservative composition was prepared by solubilizing propolis, lavender essential oil, and lemon essential oil, and E. coli ( E) which is generally used in a preservative effect test in cosmetics and foods for the antiseptic test of the natural preservative composition. . coli) and a brush as Bacillus stearate Russ (Bacillus stearothermophilus ) was used.

Example 1 Preparation of Natural Preservative Composition

(1) experimental materials

To give moisturizing effect to natural preservatives, Sodium Coco PG-Dimmonium Chloride Phosphate sold by Uniiqema as a raw material for cosmetics and detergents was used. Linoleamidopropyl PC-Dimonium from Unichema Chloride phosphate was used. In addition, 1.3-butylene glycol, which is one of the moisturizers widely used in cosmetics, also uses a product of Unichema.

To solubilize propolis, lavender essential oil and lemon essential oil, Polysorbate 20 and Polysorbate 80 from Southeast Synthetic were used. Lavender essential oil and lemon essential oil were used by Italian perfume company ACEF. Inc. was used. Propolis used the Propolis EEP100 model of Seoul Propolis. PEG (60) hydrogenated castor oil, a solubilizer from Nihon Emulsion, was used, and LB culture medium from Sigma was used for cultivation of E. coli among microorganisms, and Bacillus stearium Bacillus stearothermophilus ) was used as a product of Sigma.

Ethanol was used as 95% product of Korea Alcohol, and water was used as purified water through a purified water production apparatus. E. coli used strains stored in the Department of Biotechnology, Ajou University, and Bacillus stearothermophilus also used strains stored in the Department of Biotechnology, Ajou University. Raw materials and reagents used in this experiment are as described in Table 1.

matter water Usage manufacturer Sodium coco PG-dimonium chloride phosphate 99% Moisturizer Ubiquima Linoleamidopropyl PG-dimonium chloride phosphate 99% Softener Ubiquima 1,3-butylene glycol 99% Moisturizer Ubiquima Polysorbate 20 100% Soluble Southeast Polysorbate 80 100% Soluble Southeast Lavender essential oil 100% Active substance A.C.E.F. Lemon essential oil 100% Active substance A.C.E.F. Propolis EEP 100 100% Active substance Seoul Propolis PEG (60) hydrogenated castor oil 99% Soluble Nihon Emulsion LB culture 100% Microbial culture Sigma B. Steamo Thermophilus Culture 100% Microbial culture Sigma ethanol 95% menstruum Korean alcohol

(2) experimental devices

In this experiment, a stirrer for solubilization was used basically, and the turbidity of the formulation by solubilization was measured using a Lamotte Turbidimeter 2020. Shimadzu's UV / VIS spectrophotometer, UV-2550 model was used to measure the optical density of the strain. The DF-94BU shaking incubator model of Duriscience was used to cultivate E. coli and Bacillus stearus, and the incubator of J-100S model of Jisico Co., Ltd. was used to test the disc diffusion method. Was used. A deep press of Sanyo's MDF-236 model was used to store the strains to be tested, and an autoclave of J-NAS4 model of Indic Kosa was used to sterilize the experimental instruments. As a workbench, a clean bench of J-CBW2 model was used.

The apparatus used for the experiment is shown in Table 2.

Experimental apparatus Product number Usage manufacturer UV / VIS Spectrophotometer UV-2550 analysis Shimazu Turbidity Meter 2020 analysis Ramote Shaking incubator DF-94BU Microbial culture Douri Science Incubator J-100S Microbial culture Instruction Deep freezer MDF-236 Microbial storage Sanyo Autoclave J-NAS4 Sterile Instruction Clean bench J-CBW2 Microbial workbench Instruction mixer PI-ss41D mix Wind forest

(3) Preparation of natural preservative composition

83.1 g of purified water was added to a 200 ml beaker at room temperature, and the stirrer was operated slowly. 1 g of sodium coco PG-dimonium chloride phosphate as an aqueous phase material and 0.3 g of linoreamidopropyl PG-dimonium chloride phosphate were added, followed by stirring until the phase became clear. 1 g of 1,3-butylene glycol, 0.5 g of polysorbate 20 and 0.5 g of polysorbate 80 were added, followed by stirring until the phase became clear. In a 50 ml beaker, 5 g of 95% ethanol, 0.3 g of lavender essential oil, and 0.3 g of lemon essential oil were added to the alcohol phase at room temperature, followed by stirring until it became a uniform phase.

The PEG (60) hydrogenated castor oil was melted at 40 ° C. in a separate thermostat, and then added in accordance with the compositional ratios of 10 types in Tables 3 and 4, and operated at a stirring speed of about 50 rpm for 5 minutes until a uniform phase was obtained. I was. After checking the homogeneous phase, 2 g of propolis EEP100 was added and stirred until it became a homogeneous phase. The content of the 50 ml beaker which is an alcohol phase was added little by little to the 200 ml beaker stirring the water phase material, and the solubilization which was added little by little again checking the uniform phase was performed. After the addition was completed, the stirring was continued for about 5 minutes while maintaining the stirring speed of 50rpm. After the solubilization was completed, the stirring was stopped and the preparation was completed. The production process of this natural preservative is shown in FIG.

number
matter
Formula (Wt.%) One 2 3 4 5 One Purified water 89.10 89.05 89.00 88.95 88.90 2 Sodium coco PG-dimonium chloride phosphate 1.00 1.00 1.00 1.00 1.00 3 Linoleamidopropyl PG-dimonium chloride phosphate 0.30 0.30 0.30 0.30 0.30 4 1,3-butylene glycol 1.00 1.00 1.00 1.00 1.00 5 Polysorbate 20 0.50 0.50 0.50 0.50 0.50 6 Polysorbate 80 0.50 0.50 0.50 0.50 0.50 7 ethanol 5.00 5.00 5.00 5.00 5.00 8 Lavender essential oil 0.30 0.30 0.30 0.30 0.30 9 Lemon essential oil 0.30 0.30 0.30 0.30 0.30 10 PEG (60) hydrogenated castor oil - 0.05 0.10 0.15 0.20 11 Propolis EEP 100 2.00 2.00 2.00 2.00 2.00 all 100.00 100.00 100.00 100.00 100.00

number
matter
Formula (Wt.%) 6 7 8 9 10 One Purified water 88.855 88.80 88.75 88.70 88.65 2 Sodium coco PG-dimonium chloride phosphate 1.00 1.00 1.00 1.00 1.00 3 Linoleamidopropyl PG-dimonium chloride phosphate 0.30 0.30 0.30 0.30 0.30 4 1,3-butylene glycol 1.00 1.00 1.00 1.00 1.00 5 Polysorbate 20 0.50 0.50 0.50 0.50 0.50 6 Polysorbate 80 0.50 0.50 0.50 0.50 0.50 7 ethanol 5.00 5.00 5.00 5.00 5.00 8 Lavender essential oil 0.30 0.30 0.30 0.30 0.30 9 Lemon essential oil 0.30 0.30 0.30 0.30 0.30 10 PEG (60) hydrogenated castor oil 0.25 0.30 0.35 0.40 0.45 11 Propolis EEP 100 2.00 2.00 2.00 2.00 2.00 all 100.00 100.00 100.00 100.00 100.00

(4) solubilization results of propolis and essential oils

According to the composition ratios shown in Tables 3 and 4, the amount of PEG (60) hydrogenated castor oil was changed to examine the natural preservative composition. Propolis 2%, lavender essential oil 0.3%, lemon essential oil 0.3%, polysorbate When the 20 0.5%, polysorbate 80 0.5%, ethanol 5%, the content of PEG (60) hydrogenated castor oil is constant from 0.45% or more can be seen in Figure 2. Figure 2 graphically shows the change in turbidity with the amount of PEG (60) hydrogenated castor oil.

Example 2 Antiseptic Test

The antiseptic test was applied to the agar culture medium evenly, and then used a disk diffusion method (disco diffusion method) to inoculate the sample to be tested and a method of measuring the optical density with a UV / VIS spectrum photometer by culturing in a liquid.

(1) Disk diffusion method for E. coli

The E. coli culture in the logarithmic phase was dropped in the LB agar plate and then spread evenly with a spreader. The sterile paper discs were then placed in place. Each test sample was dropped by an appropriate amount onto the placed paper disk for absorption. After incubation for about 12 hours in a 37 ℃ incubator was determined whether the inhibitory ring and the size of the inhibitory ring.

As a comparative group for the antiseptic test of the present invention, a mixture of 5% ethanol and 95% purified water, such as the amount of alcohol mixed in a natural preservative composition, was selected, and compared with methylparaben, a commonly used preservative, To this end, a mixture of 0.2% methylparaben and 99.8% purified water was used, and 100% purified water was also used as a comparative group.

 The disk diffusion method confirms that the agar becomes transparent as the microorganisms die around the paper disk, and the ring generally becomes larger and larger. Referring to FIG. 3 showing the results of the disk diffusion test, it was found that after 24 hours, the natural preservative composition (a) of the present invention had a larger ring size than that of the comparative groups (b) to (d). It can be seen that.

(2) Optical density measurement for E. coli

Test samples were diluted 5, 10 and 15% in LB liquid medium, respectively. The culture of the logarithmic phase was inoculated 1%. Incubation in a 37 ° C. shaking incubator measured the optical density of 620 nm at every 4 hours using UV / VIS spectrophotometer to investigate the growth of E. coli at each concentration.

Optical density measurement method uses the principle of absorbing the 620nm wavelength portion of the cell wall of the microorganism, the more the microorganisms, the higher the optical density.

In FIG. 4, a change in phase according to the growth of microorganisms is shown in a photograph. FIGS. 5, 6, and 7 are photographs obtained by measuring the optical density by diluting the natural preservative composition in distilled water at 5%, 10%, and 15%, respectively.

5 and 6, when compared with the comparative group, the use of the natural preservative composition of the present invention has an E. coli inhibitory effect, it can be seen that E. coli breeds eventually.

On the other hand, as shown in Figure 7, methyl paraben 0.2% (■), ethanol 5% (▲), the comparison group (purified water) (*) was found to be almost constant after 4 hours after the optical density sharply increased over time Can be. After 20% of the natural preservative diluent, the same result as the 15% of the natural preservative diluent is obtained. For this reason, the preservative effect is good from 15% to 100%. Inverting the amount of propolis, lavender essential oil, and lemon essential oil from natural preservatives contained in 15% diluent shows that preservative effect is observed in 0.3% of propolis, 0.045% of lavender essential oil, and 0.045% of lemon essential oil. Can be.

Propolis alone is not good for inhibiting the growth of E. coli, but synergistic effects of Lavender Essential Oil and Lemon Essential Oil indicate that E. Coli's growth has been increased.

(3) Disk Diffusion Method for Bacillus Stearothermophilus

A brush as Bacillus stearate Russ (Bacillus stearothermophilus ) culture medium was dropped into the Bacillus stearo Morphilus culture medium in the logarithmic growth phase and then spread evenly rubbed with a spreader. Sterile paper discs were placed in each place. Each test sample was dropped by the same amount on the paper disk to be absorbed. After incubation for about 12 hours in a 37 ℃ incubator was determined whether the inhibitory ring and the size of the inhibitory ring.

The comparison groups used are the same as those used in the disk diffusion method for E. coli.

8 is a test result of the antiseptic force of Bacillus stearin Morphilus by the disk diffusion method. As shown in Figure 8, 24 hours after the inoculation of the bacterium natural preservatives (a) than the comparison group (b) to (d) it can be confirmed that has a better antiseptic effect on Bacillus stearin mophilus have.

(4) Optical Density Determination for Bacillus Stearothermophilus

 Test samples were diluted to 5, 10 and 15% in Morphilus culture medium with Bacillus stear. And 1% inoculation of the Morphilus culture with Bacillus stea of the logarithmic growth stage. Thereafter, the optical density was measured with a UV / VIS spectrophotometer every 4 hours while incubating in a 37 ° C shaking incubator to compare the growth inhibition of microorganisms at each concentration.

9, 10, and 11 are graphs of optical densities measured after diluting the natural preservative composition to 5%, 10%, and 15%, respectively, and were similar to the graph of FIG. 11 from 15% to 100% of the natural preservative diluent. . Referring to the optical density of FIG. 11, the other comparative group can see that Bacillus stearromophilus grows very actively with time, but it can be seen that there is almost no change in optical density in the natural preservative composition of the present invention. It means that the natural preservative composition of the present invention is more excellent antiseptic effect.

In addition, since the graphs of FIGS. 9 and 10 do not show a large change with the graph of 15%, it can be seen that the preservative effect is also obtained in the 5% of the natural preservative diluent.

1 is a schematic diagram showing a manufacturing process of a natural preservative composition.

2 is a graph showing the change in turbidity according to the amount of PEG (60) hydrogenated castor oil.

Figure 3 is a photograph showing the results of the antiseptic test by the disk diffusion method for E. coli.

Figure 4 is a photograph showing the change in phase with the growth of microorganisms over time.

5, 6 and 7 are graphs of optical density measured by diluting the natural preservative composition in distilled water at 5%, 10% and 15%, respectively.

8 is a photograph showing the results of the antiseptic test by the disk diffusion method for Bacillus stearothermophilus.

9, 10 and 11 is a graph measuring the optical density after diluting the natural preservative composition to 5%, 10%, 15%, respectively.

Claims (5)

Natural preservative composition containing 0.3 to 2% of propolis, 0.045 to 0.3% of lavender essential oil, and 0.045 to 0.3% of lemon essential oil. The natural preservative composition according to claim 1, wherein 5% ethanol as a solvent, 0.5% polysorbate 20, 0.5% polysorbate 80, and 0.45% PEG (60) hydrogenated castor oil in the natural preservative composition. Natural preservative composition comprising a. A cosmetic comprising the natural preservative composition of claim 1. 4. A cosmetic according to claim 3 comprising sodium coco PG-dimonium chloride phosphate or 1,3-butylene glycol as moisturizer and linoleamidopropyl PG-dimonium chloride phosphate as softener. Household article comprising the natural preservative composition of claim 1 or 2.

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