KR102102156B1 - manufacturing method of cosmetic composition with zeta potential controlling - Google Patents

Abstract

Disclosed is a method for manufacturing a cosmetic composition to which a zeta potential difference control is applied. According to the method for preparing a cosmetic composition to which the zeta potential difference control according to the present invention is applied, it is possible to provide a more homogeneous and stable cosmetic composition by achieving a change in physical properties such as a zeta potential and a particle size distribution without chemical additives, and product functions such as cosmetic use and adhesion Improvement can be achieved.
In addition, it is possible to increase the absorption of the active ingredient through a change in particle size distribution and zeta potential, and improve productivity by improving production yield more usefully when producing liposome particles through improved dispersibility.

Description

Manufacturing method of cosmetic composition with zeta potential difference control

The present invention relates to a method for manufacturing a cosmetic composition to which a zeta potential difference adjustment is applied, and more specifically, to provide a more homogeneous and stable cosmetic composition by changing the zeta potential and particle size distribution in a desired direction without chemical additives, and to improve the usability and adhesion of the cosmetic. It relates to a method for manufacturing a cosmetic composition to which the zeta potential difference control can be improved.

Women's instinct to pursue beauty is not the thing of yesterday, but in recent years, the interest in body shape management or beauty or cosmetics to make herself look prettier is increasing.

In addition, as women and men are interested in cosmetics for skin care, the cosmetics market continues to expand, and various types of cosmetics are launched on the market.

In general, cosmetics can be largely divided into basic cosmetics, makeup bases, and color cosmetics, and are made of solid, liquid, or gel-like cosmetics, and cosmetic containers for storing them are also variously applied.

Recently, functional cosmetics that can perform various functions such as moisturizing, whitening, wrinkle improvement, UV protection, acne relief, atopy relief, anti-inflammatory and keratin dissolution are also widely used.

On the other hand, skin cells often supply a material needed by the cell from the outside in order to maintain life or improve problems. Accordingly, in the industry related to cosmetics or pharmaceuticals, a formulation technology using a drug delivery system (DDS) as a method for efficiently moving a desired substance desired by cells into cells has been continuously studied.

In addition, in order to apply it to cosmetics, a stabilization technology is essential to maintain the original activity without deterioration in the manufacturing and distribution process.

Recently, a capsule formulation is mentioned as a skin transdermal absorption system capable of absorbing the active ingredient of a cosmetic product to the skin most safely while maximally protecting it.

Carriers of these encapsulations are classified into Microsphere (MIS), Microcapsules (MIC), and Liposome (LIP) according to their nature and origin. Among these, liposomes are effectively used to stably absorb natural physiologically active ingredients used as raw materials for functional cosmetics as carriers of various drugs into skin cells.

Specifically, the liposome formulation is a concept of encapsulation that can contain useful cosmetic ingredients, and has been in the spotlight as a medium that delivers natural ingredients for the efficacy of anti-aging and anti-aging whitening to the skin relatively stably. The furnace is also being studied.

As a prior art for a cosmetic composition using such a liposome formulation, there is Korean Patent Registration No. 10-0654102.

(Patent Document 1) KR10-0654102 B1

However, in general, it is important that liposomes are manufactured to have a homogeneous distribution as an appropriate size because the stability decreases when the size is too large, while the capacity of the nutrient decreases when the size is too small.

In addition, liposomes have problems such as physical instability of the lipid bilayer film constituting the liposome, low emulsion stability, and low collection efficiency of the active ingredient. In addition, the skin penetration of the active material is not achieved as expected, so its effect is often limited, and various methods have been studied to improve these problems.

Therefore, the present invention provides a more homogeneous and stable cosmetic composition by changing the zeta potential and the particle size distribution in a desired direction without chemical additives by solving the problems of the existing liposomes, and controlling the zeta potential difference that can improve the usability and adhesion of the cosmetic. It is intended to present a method of manufacturing the applied cosmetic composition.

The embodiments of the present invention seek to provide a more homogeneous and stable cosmetic composition by achieving a change in physical properties such as zeta potential and particle size distribution without chemical additives.

In addition, it aims to achieve improved product functions such as the use and adhesion of cosmetics.

In addition, it is intended to increase the absorption power of the active ingredient through a change in particle size distribution and zeta potential.

In addition, it is intended to improve productivity by more effectively increasing the production yield when producing liposome particles through improved dispersibility.

According to an aspect of the present invention, preparing a phospholipid solution; Forming liposome particles by irradiating low-frequency ultrasound and high-frequency ultrasound to the phospholipid solution; Forming a liquid carrier containing the liposome particles; And adjusting the zeta potential difference of the liposome particles by irradiating an energy carrier of a specific frequency to the liquid carrier. A method of manufacturing a cosmetic composition to which the zeta potential difference control is applied may be provided.

The method for preparing a cosmetic composition to which the zeta potential difference control according to the present invention is applied may be further comprised of a step of lyophilizing the liquid carrier.

The lyophilization can be made in the range of -70 ℃ to -90 ℃.

Ethanol may be applied to the phospholipid solution.

The step of forming the liposome particles may be configured to irradiate low-frequency ultrasound at least once, and then irradiate high-frequency ultrasound at least once.

The liquid carrier may be made of any one of water, isopropyl alcohol, ethanol, liquefied carbon dioxide and liquefied hydrocarbon, or a mixed solution thereof.

The frequency of the energy carrier may be determined according to the natural frequency of a specific mineral.

According to another aspect of the present invention, a cosmetic composition to which a zeta potential difference control manufactured by the above-described manufacturing method is applied can be provided.

Embodiments of the present invention can provide a more homogeneous and stable cosmetic composition by achieving a change in physical properties such as zeta potential and particle size distribution without chemical additives.

In addition, it is possible to achieve improvement in product functions such as a feeling of use and adhesion of a cosmetic.

In addition, it is possible to increase the absorption of the active ingredient through a change in particle size distribution and zeta potential.

In addition, when the liposome particles are produced through improved dispersibility, productivity can be improved by more effectively increasing the production yield.

1 is a flow chart showing a cosmetic composition manufacturing process is applied to the zeta potential difference control according to an embodiment of the present invention
Figure 2 is a block diagram showing a liposome manufacturing apparatus according to an embodiment of the present invention
Figure 3 is a perspective view showing a liquid carrier comprising a liposome prepared according to an embodiment of the present invention
4 is a block diagram showing an energy carrier irradiation apparatus according to an embodiment of the present invention
Figure 5 is a graph showing the zeta potential difference distribution of a cosmetic composition containing liposomes prepared according to an embodiment of the present invention
6 is a graph evaluating the skin penetration rate of a cosmetic composition comprising liposomes prepared according to an embodiment of the present invention
7 is a graph showing the Turbiscan stability test results of a cosmetic composition containing liposomes prepared according to an embodiment of the present invention

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the present invention is not limited to the embodiments described herein and may be embodied in other forms. Rather, the embodiments introduced herein are provided to ensure that the disclosed contents are thorough and complete, and that the spirit of the present invention is sufficiently conveyed to those skilled in the art. Throughout the specification, the same reference numbers indicate the same components.

1 is a flow chart showing a cosmetic composition manufacturing process is applied zeta potential difference control according to an embodiment of the present invention, Figure 2 is a block diagram showing a liposome manufacturing apparatus according to an embodiment of the present invention, Figure 3 is It is a perspective view showing a liquid carrier including liposomes prepared according to an embodiment of the present invention. 4 is a block diagram showing an energy carrier irradiation device according to an embodiment of the present invention, Figure 5 is a graph showing the zeta potential difference distribution of a cosmetic composition containing liposomes prepared according to an embodiment of the present invention, 6 is a graph evaluating the skin penetration rate of a cosmetic composition containing liposomes prepared according to an embodiment of the present invention. 7 is a graph showing the Turbiscan stability test results of a cosmetic composition containing liposomes prepared according to an embodiment of the present invention.

1 to 7, a method for preparing a cosmetic composition to which a zeta potential difference control according to an embodiment of the present invention is applied includes preparing a phospholipid solution (S10); Forming liposome particles by irradiating low-frequency ultrasound and high-frequency ultrasound to the phospholipid solution (S20); Forming a liquid carrier accommodating the liposome particles (S30); And adjusting the zeta potential difference of the liposome particles by irradiating an energy carrier of a specific frequency to the liquid carrier (S40).

First, a method for preparing a cosmetic composition according to an embodiment of the present invention prepares a phospholipid solution (S10). Phospholipids in this example were phosphatidylcholine derived from egg yolk (Sigma, P3556), but are not limited thereto.

Specifically, a certain amount of the phospholipid in the powder state is added to the cleaned test tube and dissolved by adding an organic solvent, and then the solvent is evaporated to dry the phospholipid to form a thin layer on the bottom surface of the test tube. Then, after a certain amount of the buffer solution is added, the mixture is stirred with a vibrating mixer to disperse and dilute the phospholipids to form a phospholipid solution, followed by ultrasonic irradiation. In this case, the phospholipid solution may be composed of ethanol by applying ethanol as the buffer solution.

As described above, ultrasound irradiation of the phospholipid solution is performed by irradiating low-frequency ultrasound and high-frequency ultrasound having different frequencies (S20).

Specifically, in this embodiment, as two different frequencies of ultrasonic waves, low-frequency ultrasonic waves that are easy to increase amplitude and high-frequency ultrasonic waves that increase acceleration are used in combination.

Here, the low-frequency ultrasound is determined in the range of 20 kHz to 60 kHz, preferably 30 kHz to 40 kHz. Low-frequency ultrasound is easy to use an ultrasonic horn that amplifies the vibration amplitude, and in this case, it can be amplified to about 10 to 20 times. Under such a large amplitude, an operation of miniaturizing the liposome raw material may be performed by the action of a shock wave generated by cavitation bubbles or shear force due to vortex.

At this time, due to the strong ultrasonic field, metal fragments may be generated and introduced from the ultrasonic horn. In order to prevent this, indirect irradiation may be performed by applying a connecting member between the phospholipid solution and the ultrasonic horn.

Such a connecting member should have little loss of ultrasonic energy, should not be damaged by a powerful ultrasonic field, and should not be harmful to the living body. To this end, flexible polymer materials such as silicone and rubber are used as the connecting member.

If only low-frequency ultrasound is applied for the micronization operation, an oxidizing agent may be formed by expansion and contraction of cavitation bubbles, and the oxidizing agent may damage the liposome raw material.

Therefore, it is possible to suppress the generation of the oxidizing agent and homogenize the liposome particles to some extent by irradiating ultrasonic waves having a higher frequency than the frequency range in which the oxidizing agent is generated. The high frequency ultrasound is determined in the range of 500 kHz to 20 MHz, and preferably in the range of 1 MHz to 5 MHz.

As shown in Figure 2, the liposome manufacturing apparatus according to an embodiment of the present invention is arranged in a three-way valve (V1, V2, V3) for changing the flow path at each branch point with a circuit constituting the circulation flow path.

In addition, a low-frequency ultrasonic irradiation device 30 and a high-frequency ultrasonic irradiation device 40 are disposed in each flow path and connected to the receiving portion 10 containing the phospholipid solution. The phospholipid solution accommodated in the accommodating part 10 is returned to the accommodating part 10 after circulating the circulating flow path by a pump 20, and at this time, low-frequency ultrasound and high-frequency ultrasound may be irradiated to the phospholipid solution.

Specifically, first, the phospholipid solution accommodated in the receiving portion 10 is guided to the low-frequency ultrasound irradiation device 30 by the pump 20, and the low-frequency ultrasound is irradiated to the phospholipid solution. At this time, by operating a 3-way valve (V1, V2) to form a circulating flow path including the low-frequency ultrasound irradiation device 30, low-frequency ultrasound irradiation of the phospholipid solution can be performed multiple times. That is, if necessary, low-frequency ultrasound irradiation can be performed once or multiple times.

Thereafter, the phospholipid solution is guided to the high frequency ultrasound irradiation device 40 to irradiate the high frequency ultrasound. At this time, low-frequency ultrasound irradiation of the phospholipid solution can be performed multiple times by operating a 3-way valve (V1, V2, V3) to form a circulating flow path including the high-frequency ultrasound irradiation device 40. That is, if necessary, high-frequency ultrasound irradiation can be performed once or multiple times.

Of course, it is also possible to configure the flow path to irradiate high-frequency ultrasound immediately after irradiation with low-frequency ultrasound to the phospholipid solution and recover it to the receiving unit 10.

After ultrasonic irradiation, as shown in Figure 3, to form a liquid carrier 50 for receiving the liposome particles (S30). At this time, the liquid carrier 50 may be made of any one of water, isopropyl alcohol, ethanol, liquefied carbon dioxide and liquefied hydrocarbon or a mixed solution thereof.

On the other hand, the method for manufacturing a cosmetic composition according to an embodiment of the present invention changes the zeta potential (Zeta Potential) and particle diameter (Particle Diameter, 粒 徑) of the liposome particles to change the physical properties of the liquid carrier with an energy carrier of a specific frequency. Irradiation to regulate the zeta potential difference of the liposome particles (S40).

The zeta potential difference adjustment may be performed through the energy carrier irradiation device 100 as shown in FIG. 4, and the energy carrier irradiation device 100 may achieve desired physical property changes by adjusting the frequency of the energy carrier to be irradiated. have.

And the frequency of the energy carrier can be determined according to the natural frequency of a specific mineral. Specifically, the energy carrier irradiation device 100 generates a unique signal having a desired natural frequency by irradiating a control signal to a specific mineral, and amplifies it through an amplifying circuit unit provided therein.

Here, various kinds of mineral materials such as silicon, crystal, amethyst, and copper may be applied to the mineral material.

The energy carrier can be irradiated by synthesizing and outputting the amplified intrinsic signal to a carrier signal in a specific region so as to transmit it to the liposome particles contained in the liquid carrier 50. The carrier signal may be, for example, a signal in a visible light region, but is not limited thereto, and it is possible to apply a carrier signal in various region.

In this way, the physical properties of the liposome particles, that is, the zeta potential and the particle diameter, may be adjusted according to the user's intention by the energy carriers irradiated to the energy carrier irradiation device 100.

Meanwhile, the method for manufacturing a cosmetic composition according to an embodiment of the present invention may further include the step of freeze-drying the liquid carrier 50 (S50).

The liposomes to which the aforementioned zeta potential difference control is applied can be used as a liquid, but can be applied by powdering through lyophilization. In the lyophilization process, trehalose and sucrose may be used as a cryoprotectant. And the lyophilization can be made in the range of -70 ℃ to -90 ℃.

Specifically, in the present embodiment, the liquid carrier 50 containing the liposome is cooled to -80 ° C in a deep freezer and freeze-dried for 48 hours using a freeze dryer. At this time, when cooling in a deep freezer to prevent the collapse of the liposome structure during lyophilization, it is desirable to lower the temperature constantly and gently.

The particle size, zeta potential difference measurement, and skin penetration effect and stability evaluation were performed on the liposome particles thus prepared.

First, it was confirmed that nanoscale particles were well formed at 110 nm as a result of particle size measurement. In the case of the zeta potential difference, as shown in FIG. 5, since a value of −40 mV or less was found at −72.89 mV, it can be confirmed that the stable state was maintained.

In relation to the skin penetration effect, a general liposome and a liposome prepared according to the present invention were compared under the same experimental conditions.

Specifically, the experiment was conducted by attaching the neoderm of the artificial skin, Taego Science, to the Franz-type diffusion cell (Lab fine instruments, Korea).

After introducing 50mM phosphate buffer (pH7.4, 0.1M NaCl) into the Receptor container (5ml) of the Franz-type diffusion cell, the diffusion cells were mixed and dispersed at 32 ° C and 600rpm, and the liposomes according to the present invention. 50 ul of the normal liposome was placed in a donor container and absorbed and diffused according to a predetermined time, and the portion where absorption and diffusion occurred was set to 0.64 cm ² of the skin.

After absorption and diffusion of the active ingredient is finished, it is not absorbed with dried kimwipes or 10 ml of ethanol, and the remaining oil is washed, and the tip-type equalizer is used to grind the skin where the active ingredient is absorbed and diffused, and then inside the skin. The amount of Retinal absorbed by was extracted using 4 ml of dichloromethane.

The extract was filtered with a 0.45um nylon membrane filtration membrane, and the content was measured by HPLC to show the results.

As a result, as shown in Figure 6, it was confirmed that the liposome according to the present invention has a 1.6 times higher skin penetration rate than the normal liposome.

The stability evaluation was performed using Turbiscan, and the stability was confirmed under high temperature conditions by the emulsion itself without diluting the concentration of the solution. Specifically, the stability was confirmed at 40 ° C., 4 hours, and 50 scan conditions using Turbiscan (TurbiscanLAB, Formulation, France). As shown in FIG. 7, there was no significant change in the graph, and it was confirmed that it is in a stable state. .

According to the method for preparing a cosmetic composition to which the zeta potential difference control according to the embodiments of the present invention described so far is applied, it is possible to provide a more homogeneous and stable cosmetic composition by achieving changes in physical properties such as zeta potential and particle size distribution without chemical additives It can achieve the improvement of product functions such as the feeling of use and adhesion.

In addition, it is possible to increase the absorption of the active ingredient through a change in particle size distribution and zeta potential, and improve productivity by increasing production yield more usefully when producing liposome particles through improved dispersibility.

Although described above with reference to one embodiment of the present invention, those skilled in the art variously modify and change the present invention without departing from the spirit and scope of the present invention as set forth in the claims below. You will be able to. Therefore, if the modified implementation basically includes the components of the claims of the present invention, it should be considered that all are included in the technical scope of the present invention.

10: receiving section 20: pump
30: low frequency ultrasonic irradiation device 40: high frequency ultrasonic irradiation device
50: liquid carrier 100: energy carrier irradiation device

Claims (8)

Preparing a phospholipid solution;
Forming liposome particles by irradiating low-frequency ultrasound of 20 kHz to 60 kHz and high-frequency ultrasound of 500 kHz to 20 MHz to the phospholipid solution;
Forming a liquid carrier containing the liposome particles;
Adjusting the zeta potential difference of the liposome particles by irradiating an energy carrier wave having a frequency determined according to the natural frequency of the applied mineral material to the liquid carrier; And
Including the step of lyophilizing the liquid carrier; includes,
The lyophilizing step,
The liquid carrier containing the liposome is cooled by lowering the temperature constantly within a range of -70 ° C to -90 ° C to prevent the liposome from collapsing in a deep freezer, and then frozen using a freeze dryer. Dry,
In the lyophilization process, trehalose and sucrose are used as cryoprotectants,
A method for preparing a cosmetic composition having a zeta potential difference control applied, characterized in that the zeta potential difference of the liposome particles is made smaller than -40 mV. delete delete According to claim 1,
The phospholipid solution is a method of manufacturing a cosmetic composition applied zeta potential difference is characterized in that applying ethanol. According to claim 1,
The step of forming the liposome particles is a method of manufacturing a cosmetic composition having a zeta potential difference control, characterized in that after irradiating low-frequency ultrasound at least once, and then irradiating high-frequency ultrasound at least once. According to claim 1,
The liquid carrier is water, isopropyl alcohol, ethanol, liquefied carbon dioxide and any one of liquefied hydrocarbons, or a mixture composition of zeta potential control method characterized in that it is made of a mixed solution. delete Claim 1, claim 4 to claim 6, wherein the cosmetic composition is applied to control the zeta potential difference produced by the method according to any one of claims.

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