KR101157470B1 - Method for preparing nanoemulsion composition comprising chamaecyparis obtus - Google Patents

Abstract

PURPOSE: A manufacturing method of retinispora nano emulsion composition is provided to prevent layer separation. CONSTITUTION: A manufacturing method of retinispora nano emulsion composition comprises the following steps: separating and washing cypress leaf; desiccating the washed leaf at low temperature; providing steam on the dried cypress leaf; refrigerating and condensing steam which includes essential oil component extracted from the steam; separation refining the cypress oil and cypress water from the essential oil; homogenizing the refined cypress oil into nano-particles by using a high pressure liquid phase emulsifier; mixing the homogenized cypress oil and cypress water and emulsifying the mixture by using a high pressure liquid phase emulsifier.

Description

Method for preparing nanoemulsion composition comprising chamaecyparis obtus

The present invention relates to a method for preparing a protein-based emulsified composition, and more particularly, to a method for preparing a protein-based emulsified composition which can be used or stored for a long time without separation of layers, and which can maintain the protein intact without modification of flavor or function. It is about.

In general, sterilization is the addition of microorganisms to kill or remove microorganisms and keep them aseptic.

The fungicides may be extracted from nature (ie, natural fungicides), but most of them are easy to manufacture, low cost, and easy to mass-produce chemical synthetic materials (ie, chemical fungicides).

However, in the case of chemical fungicides, the use of the chemical disinfectant has been recently limited due to problems such as impaired lung function upon contact with the human body by inhalation, skin contact, ingestion, and the like, and eventually death.

Cypress, also called cypress, is 40m high and 2m in diameter. The branch of the cypress spreads horizontally to form a conical water pipe. The bark is reddish brown, fibrous, thinly peeled vertically. The leaves are opposite and thick, 1 ~ 1.5mm long, small like scales, and the pore ships on the back (the line where the leaves breathe and usually appear as white lines behind the leaves) are Y-shaped.

Cypress, such as phytoncushion is a substance called phytoncide, phytoncide (phytoncide) is a fragrant substance that the tree sheds to protect itself from various pests or bacteria, itself contains bactericidal, pesticidal components. Phytoncide is a terpene-based organic compound and is known to have antibacterial, sedative, deodorant and stress relief effects.

When humans inhale phytoncide, studies have reported that the concentration of the stress hormone cortisol is reduced by less than half. In addition, the central nervous system soothing action to have a pleasant feeling, helps to get a good night's sleep. In addition, it has been found to be effective in hyperlipidemia and thrombotic heart failure by improving the blood circulation system, and is also known as a strong antibacterial action that does not cause resistance in the human body. In addition, natural phytoncide has been known to be effective in preventing allergens without side effects by avoiding dust mites.

Such phytoncide is known to have a stress relief effect, strong antibacterial action, deodorant action, fatigue sedation effect, allergy and skin disease improvement action and immune function enhancement effect.

Many studies are being conducted to scientifically reveal the effects of phytoncide with various functions. Especially, in order to be able to easily enjoy the forest bath in urban space, various aroma products made by extracting phytoncide ingredients are sold nowadays. .

As a method of obtaining a phytoncide product using a conventional cypress, there is a method of obtaining a phytoncide essential oil by grinding cypress leaves in alcohol or water, heating them, and then collecting and recovering the vapor generated therefrom.

However, essential oils obtained by using the conventional alcohol as described above must be diluted and used. At this time, the essential oil is not diluted with water due to the alcohol used in the manufacturing process. There was a problem to be done.

In addition, even when water is used to obtain an essential oil, the separation of the protein oil contained in the essential oil and the protein (or water used by dilution) occurs, resulting in layer separation when used as a cosmetic, pharmaceutical, or humidifier additive. Separation phenomenon is inevitably appeared, and thus, when the product containing the protein is not mixed, the effect of the protein may not be maximized without a separate mixing treatment, and there is an inconvenience in that it must be shaken every time it is used. .

As a result, the use of the proteinaceous oil as a natural disinfectant or a natural additive was inevitably limited. Inevitably, a chemical emulsifier was used to prepare a product mixed with oil and water.

Domestic Patent No. 10-0868801

In order to solve the problems of the prior art as described above, the present invention provides a method for preparing a one-pack nanoemulsion composition that does not occur even after long-term use or storage to prevent the layer separation phenomenon occurs immediately when mixing the natural raw materials. It aims to do it.

In addition, an object of the present invention is to provide a method for producing a protein-based emulsified composition capable of maintaining and storing the protein-containing oil for a long time without modification of flavor or function.

In addition, the present invention is to prevent the separation of the layer can be expressed to the maximum effect of the protein oil without using a separate mixing treatment when using the product is a method of manufacturing a protein nano-emulsion composition suitable for use as an additive in cosmetics, pharmaceuticals, humidifiers It aims to provide.

In order to achieve the above object, the present invention is to collect the (S1) cypress, separating the leaves and washing; (S2) low-temperature drying the washed leaves; (S3) putting the dried cypress leaves into a distillation tank and supplying steam using heating means; (S4) cooling and condensing water vapor containing the essential oil component extracted by the steam; (S5) separating the cypress oil and cypress water from the essential oil cooled and condensed by the cooling water; (S6) homogenizing the separated cypress oil into nanoparticles using a high pressure liquid emulsion; And (S7) mixing the homogenized one-pack nanoparticle oil and one-piece water and emulsifying using a high-pressure liquid-phase emulsifier.

The homogenization of the step (S6) is preferably carried out to operate the two cycles at a pressure of 12,000 ~ 18,000 psi using a high-pressure liquid emulsion so that the particle size of the white liquor oil is 250 ~ 350nm.

In step (S7) it is preferable that the one-sided nanoparticle oil and the one-sided water are mixed in a weight ratio of 1:10 to 35.

In addition, the emulsification of the step (S7) is preferably performed by operating two cycles at a pressure of 12,000 ~ 18,000psi using a high pressure liquid emulsion.

In another aspect, the present invention provides a one-pack nano emulsified composition is prepared by the above method is mixed with a one-pack nanoparticle oil and the number of cycads in a weight ratio of 1:10 ~ 35.

The emulsified nanoemulsion composition may be used as a natural additive in cosmetics, pharmaceuticals, humidifiers and the like.

According to the present invention, it is possible to use and store the layer separation phenomenon and the fragrance or function for a long time by preventing the layer separation phenomenon which occurs immediately when mixing the natural raw materials, the product has no separate mixing treatment when using the product It can express the effect to the maximum and is harmless to the human body and is safe to use as an additive for cosmetics, medicines, humidifiers and the like.

Hereinafter, the present invention will be described in detail.

The present invention is a result obtained by a multi-faceted study in order to prevent the separation and separation of cypress oil and cypress water from cypress essential oil, and homogenizes the homogenous oil using a high pressure liquid emulsion under specific conditions. It was possible to effectively prevent layer separation by emulsifying the unrecovered proteinaceous nanoparticle oil and the unrecovered water using a high pressure liquid emulsifier, and finding the optimum mixing ratio of the reclaimed oil and the reclaimed water.

Referring to the method for producing a one-pack nanoemulsion composition prevented layer separation of the present invention in detail.

First, the cypress is harvested, the leaves are separated and washed.

The harvest time of the cypress is suitable for spring and spring, March and April, autumn and October and November, and winter and January and February. The moisture content of the leaves is about 48% in spring, about 62% in summer and winter. Is about 57%. In the present invention, the target of the cypress growing in Jangheung-gun, Jeonnam, was used to collect the leaves of July-August that can be supplied immediately.

To collect the cypress leaves, cut off the branches about 2m high from the ground, separate the leaves, collect them, and wash the collected leaves with clean water to remove foreign substances on the leaves.

Subsequently, the washed leaves are preferably dried for 25 to 30 hours in a low temperature dryer at 32 to 37 ° C, and more preferably at low temperature for 28 hours at 35 ° C. When the drying temperature and time are out of the above range, the extraction yield of cypress essential oil (cypress oil and cypress water) may be maximized without damaging the cypress leaves.

In addition, the drying is preferably such that the moisture content of the cypress leaves is up to 5%, wherein the moisture content of more than 5% may not be performed smoothly after the extraction of the cypress essential oil.

The dried cypress leaves are then put in a distillation tank and supplied with steam at 95-110 ° C. using heating means.

At this time, it is preferable in terms of extraction efficiency that the dried cypress leaves are cut to a size of about 3 mm as a pretreatment process.

After cutting the cypress leaves into the collection network of the distillation tank, open the lid of the distillation tank, supply the cypress leaves contained in the collection network to the inner space of the distillation tank, and then supply distilled water to the inside of the distillation tank. . And close the lid and operate the heating means installed in the distillation tank to increase the internal temperature of the distillation tank.

At this time, the distillation tank is a conventional distillation tank used in the art, a device for increasing the temperature of the distillation tank by applying heat such as gas, electricity, steam as a heating means is used burner, electric furnace, heater, steam boiler, etc. Of course, it is obvious that they do not limit the scope of the present invention.

The distilled water supplied into the distillation tank is preferably supplied about 20L, heated distilled water to about 95 ~ 110 ℃ to supply steam for about 4 hours to pass through the cypress leaves.

The water vapor containing the essential oil component extracted by the high temperature steam supplied into the distillation tank is then supplied to a cooler of about -5 ° C to be separated into cypress oil and cypress water.

That is, the water vapor containing the essential oil component is moved to the cooler by pressure, and the thus moved water vapor is condensed by heat exchange by the cooler. The condensed water vapor is supplied to the refinery tank, and the essential oil components contained in the water vapor are collected by the collector as a liquid refinery and separated into layers to separate cypress oil and cypress water.

Then, the separated cypress oil is homogenized into nanoparticles using a high pressure liquid emulsion.

In the present invention, the two cycles are operated using a high pressure liquid emulsion for the homogeneous mixing of the cypress oil separated from the cypress leaves, and specifically, the nanoparticles of the protein powder separated by the first cycle in the high pressure liquid emulsion. Homogenize to the level, and homogenize the emulsified homogenized nanoparticle oil and cyanomegaly water through the first cycle in a second cycle. The reason for this two-cycle operation is that the emulsification itself becomes difficult without this process because the cyanotropic oil and the cyanowater are not nano homogenized due to their own layer separation.

A high pressure microfluidizer is a machine that performs emulsification using high pressure, and finely emulsifies the particles by cavitation and collision force caused by pressure fluctuations generated when the oil is inferred by normal pressure and 1 atm using high pressure. It is a machine that makes use of the principle.

In the present invention, by applying pressure to the cypress oil extracted from the cypress leaves to a high-pressure liquid emulsion it is possible to obtain fine and uniform emulsion particles of the nanoparticle level. In addition, since the one-sided nanoparticle oil obtained as described above is fine and uniform emulsion particles, a separate chemical emulsifier is not required when the composition of the present invention is used as an additive such as cosmetics, medicines, and humidifiers.

That is, in the present invention, at 12,000 to 18,000 psi pressure, more preferably at 15,000 psi pressure in the high pressure liquid emulsion, it is possible to operate the first cycle to nanoparticle granulated oil. When the pressure is out of the range, the homogenization of the cypress oil may not be performed smoothly, which may result in layer separation with the water component, and due to the high pressure, the chemical structure of the oil may be broken and emulsified. In order to ensure the stability when manufacturing the product must be used a separate emulsifier.

It is more preferable that the homogenized one-pack nanoparticle oil has a particle size of 250 to 350 nm for preventing delamination with the water component.

This homogenized proteinaceous nanoparticle oil is mixed with the separated cyanowater above and emulsified by operating the cycle once more by a high-pressure liquid emulsion.

The cyanoparticle nanoparticle oil and cyanobacterial water are preferably mixed in a weight ratio of 1:10 to 35, more preferably in a weight ratio of 1:15 to 20, and most preferably in a weight ratio of 1:19. Will be. When the mixing ratio is out of the above range, the separation of the cyanoparticle nanoparticle oil and the cyanowater may occur.

The mixed cynic nanoparticle oil and the cyanowater are then emulsified in a high pressure liquid emulsion, where the second cycle is operated at a pressure of 12,000 psi to 18,000 psi, more preferably at a pressure of 15,000 psi. If the pressure range is out of the above range, emulsification of the one-pack nanoparticle oil and the one-packed water may not be performed smoothly, and layer separation may occur.

Particularly, in the present invention, the homogenization of the protein oil, the mixing of homogenized protein nanoparticle oil and protein water, and the treatment in a high-pressure liquid-emulsifier must be followed in order to obtain the desired effect in the present invention. However, when the order is changed or premixed or processed the cypress oil and the cypress water, it is also difficult to obtain the effect to be achieved in the present invention.

In another aspect, the present invention provides a one-sided nano emulsified composition prepared by the above method, the one-sided nano emulsified composition of the present invention prepared through the above steps is a long-term use as a natural raw material mixed uniformly oil and cypress number Even when stored, layer separation does not occur.

In addition, the emulsification nano emulsification composition of the present invention does not occur in the separation of the liquor oil and cypress water, so it is usefully applied to cosmetics, medicines, humidifier additives, etc. It is possible to exert effects such as disease improvement and immune function enhancement.

In particular, the use of the emulsified nanoemulsion composition of the present invention is particularly noteworthy as a humidifier additive. In the case of conventional humidifier additives, the bactericidal components (ethoxyethyl guanidine (PGH), polyhexamethylene guanidine (PHMG) chloride) used in the respiratory When inhaled by the lung tissue, which causes enormous damage to life, its use is limited, and the use of the respiratory inhalation as well as the contact with the skin or the mouth are harmless to the human body.

Thus, the one-sided nanoemulsion composition of the present invention is harmless and safe to the human body while fully exerting the effect of the existing humidifier additive, and further improves the phenomenon of separation of the conventional one-sided oil and cypress water without the need for a separate treatment or additive for mixing. Efficacy will be able to exhibit the effect that cypress has.

Hereinafter, the present invention will be described in more detail with reference to examples. These embodiments are for purposes of illustration only and are not intended to limit the scope of protection of the present invention.

Example 1

The leaves of the Cypress growing in Jangheung-gun, Jeonnam were collected from July to August. For harvesting leaves, the leaves were collected after cutting branches around 2m from the ground. The separated leaves were washed and dried in a low temperature dryer at 35 ° C. for 28 hours to obtain a maximum water content of 5%. Then, the dried cypress leaves are cut into particles of about 3 mm, and 7 kg of the cypress leaves thus cut are put in a collecting network, and a collecting network containing cypress leaves is put in a distillation tank, and then inside a distillation tank. Was fed to distilled water. At this time, distilled water was supplied to about 20L, and heated to 102 ℃ to supply steam for 4 hours to pass through the cypress leaves. Thus, the steam containing the essential oil component extracted by the steam was moved to a cooler of -5 ℃ separated into cypress oil and cypress water.

Then, the separated protein oil is homogenized into nanoparticles of about 300 nm by operating two cycles at a pressure of 15,000 psi in a high-pressure liquid emulsion, and then, 5 weight% of the homogenized protein powder and 95 weight% of cypress water. After mixing, the mixture was operated in a high pressure liquid emulsifier at 15,000 psi to operate two cycles to prepare a protein-based nanoemulsion composition in which the protein-containing oil and the protein-containing water were mixed.

Comparative Example 1

The same procedure was carried out in the same manner as in Example 1 except that the separated protein oil was not homogenized in a high pressure liquid emulsion.

Comparative Example 2

The same procedure as in Example 1 was carried out except that 10 wt% of homogenized cyanoparticle nanoparticle oil and 90 wt% of cyanowater were mixed.

Comparative Example 3

After mixing 5% by weight of the separated protein oil and 95% by weight of the cypress, the mixture was homogenized with about 300 nm of nanoparticles by operating two cycles at a pressure of 15,000 psi in a high pressure liquid emulsion, and then using a high pressure liquid emulsion. The same procedure as in Example 1 was conducted except that the two cycles were operated at 15,000 psi.

Comparative Example 4

After mixing 5 wt% of cypress oil and 95 wt% of cypress water, the mixture is emulsified in the high pressure liquor at 15,000 psi at 15,000 psi to emulsify the protein and oil, and then the emulsion is The same procedure as in Example 1 was carried out except that the two cycles were operated at 15,000 psi and homogenized to about 300 nm of nanoparticles.

After leaving the compositions prepared in Example 1 and Comparative Examples 1 to 4 for 72 hours at room temperature, the presence or absence of layer separation was visually observed, and the results are shown in Table 1 below.

division Layer separation Example 1 No delamination after 72 hours Comparative Example 1 Immediate delamination occurs Comparative Example 2 Delamination after 72 hours Comparative Example 3 Immediate delamination occurs Comparative Example 4 Immediate delamination occurs

As shown in Table 1, in the case of the protein-back emulsified composition prepared by sequentially performing the production method of the present invention, even after 72 hours of manufacture, the separation of the protein-backed oil and cypress water did not occur. In the case of Comparative Examples 1 to 4 in which the order was changed or mixed and processed in advance, it was confirmed that delamination occurred immediately upon preparation.

Through these results, it can be seen that when the protein composition is prepared according to the preparation method of the present invention, a composition of a stable formulation can be prepared while preventing layer separation of the existing protein composition. It could be predicted that it would be suitable for application to humidifier additives.

In addition, the sterilization performance was measured using a humidifier additive comprising the one-pack nanoemulsion composition of Example 1 prepared according to the present invention and the conventional ethoxyethyl guanidine (PGH) or polyhexamethylene guanidine (PHMG) as a sterilization component. .

A blank sample was added to the same cell culture plate (diameter 10 cm) and cultured with 0.04 ml (377 bacteria) of culture medium containing Streptococcus aureus ( Staphylococcus aureus , ATCC 6538). And a sample containing 0.2 ml of the one-pack nanoemulsion composition of Example 1, and a sample containing 0.2 ml of an existing humidifier additive (containing PGH or PHMG components) were prepared, and then cultured for 24 hours. The number of bacteria and colonies after incubation are shown in Table 2 below, and the reduction rate was calculated according to Equation 1 below.

[Equation 1]

% Reduction = {(Number of colonies in blank sample-number of colonies in test sample) / Number of colonies in blank sample} × 100

division Number of bacteria per 0.4 ml Colony count % Reduction Incubation time (hr) 0 24 - blank 377 1659 - Example 1 377 23 96.8 Conventional Humidifier Additive 377 20 98.8

As shown in Table 2, the one-pack nano-emulsion composition of Example 1 prepared according to the present invention was markedly reduced in the number of colonies compared to the blank sample, the bacterium reduction rate after 9 hours culture was 96.8%, such sterilization The effect was found to be similar to that of the humidifier additive containing a conventional sterilization component.

Through these results, the protein-based emulsified composition prepared according to the present invention uses ethoxyethyl guanidine chloride (PGH) or polyhexamethylene, which is a chemical component used in an existing humidifier additive, by using a natural raw material mixed with protein and oil. Without the use of guanidine (PHMG) can exhibit a similar degree of bactericidal effect, it can be expected that the natural ingredients can be used safely and harmless to the human body.

Although the present invention has been described as the preferred embodiment mentioned above, it is possible to make various modifications or variations without departing from the spirit and scope of the invention. The appended claims also cover such modifications and variations as fall within the spirit of the invention.

Claims (11)

(S1) collecting the cypress to separate the leaves and wash;
(S2) low-temperature drying the washed leaves;
(S3) putting the dried cypress leaves into a distillation tank and supplying steam using heating means;
(S4) cooling and condensing water vapor containing the essential oil component extracted by the steam;
(S5) separating and purifying cypress oil and cypress water from the cold condensed essential oils;
(S6) homogenizing the separated purified cypress oil into nanoparticles using a high pressure liquid emulsion; And
(S7) mixing the homogenized one-pack nanoparticle oil and one-piece water and emulsifying using a high pressure liquid emulsion;
Method of producing a one-sided nano-emulsion composition prevented layer separation comprising a. The method of claim 1,
Before the step (S3) before the step of cutting the dried cypress leaves to a size of about 3mm further comprising the step of producing a layered prevented cyano nanoemulsion composition. The method of claim 1,
The low temperature drying of the step (S2) is a method for producing a single-walled nano-emulsion composition prevented layer separation, characterized in that carried out for 25 to 30 hours at 32 ~ 37 ℃ so that the moisture content is up to 5%. The method of claim 1,
The step (S3) is a method for producing a single-walled emulsified composition prevented layer separation, characterized in that for supplying steam of 95 ~ 110 ℃. The method of claim 1,
Cooling condensation of the step (S4) is a method of producing a separation-prevented one-pack nano-emulsion composition, characterized in that carried out at about -5 ℃. The method of claim 1,
The homogenization of the step (S6) is a method of producing a separation-prevented one-pack nano-emulsion composition, characterized in that is performed by operating the first cycle at a pressure of 12,000 ~ 18,000psi using a high pressure liquid emulsion. The method of claim 1,
Homogenization of the step (S6) is a method of producing a separation-prevented protein-backed emulsified composition, characterized in that the particle size of the protein-based oil is performed so that 250 ~ 350nm. The method of claim 1,
In step (S7), the method of producing a separable nano emulsified composition, characterized in that the one-sided nanoparticle oil and the number of cyanobacteria are mixed in a weight ratio of 1:10 to 35. The method of claim 1,
The emulsification of the step (S7) is a method of producing a separation-prevented one-pack nano-emulsion composition, characterized in that is performed by operating a second cycle at a pressure of 12,000 ~ 18,000psi using a high pressure liquid emulsion. The method of claim 1 to 9 is prepared by the method of any one of claim 1, characterized in that the separation of the one-sided nano-emulsion composition, characterized in that the mixture of the one-to-one nanoparticle oil and the number of cyanomers in a weight ratio of 1:10 to 35. The method of claim 10,
The protein-based emulsifying composition is prevented from separating layers, characterized in that used as a natural preservative in cosmetics, medicines or humidifiers.