CN111904877A - Nanoemulsion preparation based on hyaluronic acid micro molecules and preparation method thereof - Google Patents

Abstract

The invention discloses a nano-emulsion preparation based on hyaluronic acid micro-molecules and a preparation method thereof, wherein the preparation comprises 0.1-3% of hyaluronic acid, 0.1-10% of surfactant, 0.1-20% of cosurfactant, 0.1-10% of solvent, 0.5-20% of oil phase, 0.01-1% of preservative, 0.01-1% of spice and 54-95% of distilled water. The nanometer emulsion preparation has the advantages of reduced particle size of hyaluronic acid molecules, improved transdermal property, simple preparation process, and low cost.

Description

Nanoemulsion preparation based on hyaluronic acid micro molecules and preparation method thereof

Technical Field

The invention relates to the technical field of cosmetics, in particular to a nano-emulsion preparation based on hyaluronic acid micro-molecules and a preparation method thereof.

Background

Hyaluronic acid, also known as hyaluronic acid, is widely used as a wrinkle-removing filling material in the field of cosmetic surgery. In the field of skin care, hyaluronic acid is always a good moisturizing and anti-aging component, but the development of hyaluronic acid in the field of skin care cosmetics is limited due to overlarge molecular weight, poor transdermal property and the like.

Disclosure of Invention

In view of the above disadvantages, it is an object of the present invention to provide a nano-emulsion preparation based on hyaluronic acid micro-molecules and a method for preparing the same.

In order to solve the technical problems, the invention adopts the following technical scheme:

the invention provides a hyaluronic acid nanoemulsion preparation, which consists of 0.1-3% of hyaluronic acid, 0.1-10% of surfactant, 0.1-20% of cosurfactant, 0.1-10% of solvent, 0.5-20% of oil phase, 0.01-1% of preservative, 0.01-1% of spice and 54-95% of distilled water.

Preferably, the molecular weight of the hyaluronic acid is 800-.

Preferably, the surfactant is any one or combination of more of Tween-80, Tween-60, triglyceride, sodium lauryl sulfate, polyoxyethylene lauryl ether and polyoxyethylene hydrogenated castor oil.

Preferably, the cosurfactant is any one or combination of sorbitan monostearate, propylene glycol monostearate, glyceryl monostearate, span 20, span 60 and span 80.

Preferably, the oil is any one or combination of edible tricaprylin, caprylic/capric triglyceride, soybean oil, medicinal liquid paraffin, edible salad oil, castor oil, isopropyl myristate and ethyl oleate.

Preferably, the solvent is any one or combination of anhydrous ethanol, pentanediol, n-butanol, glycerol and 1, 3-butanediol.

Preferably, the preservative is any one or combination of phenoxyethanol, ethylhexyl glycerol, benzoic acid, sodium benzoate, sorbic acid, potassium sorbate and calcium propionate.

Preferably, the perfume is one or more combination of daily chemical perfumes.

More preferably, the emulsion preparation is any one of essence, toner and spray.

The preparation method of the hyaluronic acid nanoemulsion preparation comprises the following steps:

(1) firstly, dissolving hyaluronic acid by redistilled acetone;

(2) mixing the oil phase, the surfactant, the cosurfactant and the solvent, adding absolute ethyl alcohol which is equal to the total amount of the oil phase, the surfactant, the cosurfactant and the solvent, mixing according to a ratio of 1:1, magnetically stirring for 4 hours, and cooling to below 45 ℃;

(3) slowly adding the hyaluronic acid acetone solution obtained in the step (1) into the solution obtained in the step (2), uniformly stirring by using a high-pressure homogenizer with 1.38 × 108Pa-4.13 × 108Pa, then decompressing to 1.0 × 10-2Pa-1.0 × 104Pa, distilling, removing acetone and ethanol, and cooling to room temperature for later use;

(4) adding water, antiseptic and perfume to obtain hyaluronic acid nanoemulsion.

The invention has the beneficial effects that: the nanometer emulsion preparation has the advantages of reduced particle size of hyaluronic acid molecules, improved transdermal property, simple preparation process, and low cost.

Detailed Description

The technical solutions of the present invention will be described clearly and completely in the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

A hyaluronic acid nanoemulsion preparation comprises 0.1% of hyaluronic acid, 0.4% of Tween-80, 0.5% of sorbitan monostearate, 1.99% of absolute ethyl alcohol, 1.99% of edible tricaprylin, 0.01% of phenoxyethanol, 0.01% of spice and 95% of distilled water.

The preparation method comprises the following steps:

(1) firstly, dissolving hyaluronic acid by redistilled acetone;

(2) mixing the oil phase, the surfactant, the cosurfactant and the solvent, adding absolute ethyl alcohol which is equal to the total amount of the oil phase, the surfactant, the cosurfactant and the solvent, mixing according to a ratio of 1:1, magnetically stirring for 4 hours, and cooling to below 45 ℃;

(3) slowly adding the hyaluronic acid acetone solution obtained in the step (1) into the solution obtained in the step (2), uniformly stirring by using a high-pressure homogenizer with 1.38 × 108Pa-4.13 × 108Pa, then decompressing to 1.0 × 10-2Pa-1.0 × 104Pa, distilling, removing acetone and ethanol, and cooling to room temperature for later use;

(4) adding water, antiseptic and perfume to obtain hyaluronic acid nanoemulsion.

Example 2

A hyaluronic acid nanoemulsion preparation comprises 1% hyaluronic acid, 3% triglyceride, 8% glyceryl monostearate, 3% n-butanol, 7% soybean oil, 0.03% benzoic acid, 0.03% perfume, and 77.94% distilled water.

The preparation method is the same as that of example 1.

Example 3

A hyaluronic acid nanoemulsion preparation is composed of 2% of hyaluronic acid, 7% of polyoxyethylene lauryl ether, 12% of span 60, 8% of glycerol, 13% of medicinal liquid paraffin, 0.05% of potassium sorbate, 0.05% of spice and 57.9% of distilled water.

Example 4

A hyaluronic acid nanoemulsion preparation is composed of 3% of hyaluronic acid, 10% of polyoxyethylene hydrogenated castor oil, 15% of span 80, 4% of 1, 3-butanediol, 12% of ethyl oleate, 1% of calcium propionate, 1% of perfume and 54% of distilled water.

The preparation method is the same as that of example 1.

Comparative example 1

Selecting best example 1 of CN201210434701.7(CN102871936A), referring to the composition and preparation method thereof, the rhodiola root extract is replaced by salidroside of the invention, which comprises the following specific steps:

specific components	Weight ratio (%)
		Salidroside	0.1
Polyglycerol monooleate	0.5
		Tween 80	0.5
Polyoxyethylene Castor oil	0.5
		Polyethylene glycol caprylic/capric glycerides	0.5
Soybean lecithin	3.5
		Caprylic/capric glycerides	5
Glycerol	69.4
		Water (W)	20

The preparation method comprises the following steps: respectively dissolving phospholipid in 70ml chloroform-n-hexane solution (chloroform: n-hexane, 5: 7, v/v), dissolving salidroside in 10ml distilled water, stirring, mixing the two solutions, performing ultrasonic treatment, and freeze drying the obtained emulsion to obtain salidroside-phospholipid complex; mixing salidroside-phospholipid complex, caprylic/capric glyceride, polyglycerol monooleate, tween 80, polyoxyethylene castor oil, and polyethylene glycol caprylic/capric glyceride, and shearing at 8000rpm until no visible solid matter exists in the system; adding glycerol and water into the product obtained in the step 2), and shearing at high speed under 12000rpm to obtain primary emulsion, treating the primary emulsion by a high-pressure homogenizer at 800bar, and circulating for 5 times to obtain transparent clear nanoscale emulsion.

In vitro transdermal test:

first, test sample

Samples 1 to 4: the products prepared in examples 1-4; control 1: the product of comparative example 1. Before testing, the different sample concentrations were normalized to 0.1% by dilution.

Second, test method

A (25 + -5) g male mouse was removed of abdominal hair with 6% Na2S solution, and immediately after neck amputation, abdominal skin was excised, and subcutaneous tissue and fat were removed and washed repeatedly with purified water. The skin was fixed on a diffusion cell with stratum corneum facing up, purified water was used as a receiving solution, the rotational speed was 180rpm, the diffusion area was 3.3cm, the total volume of the receiving cell was 18ml, and water bath circulation was carried out at 37 ℃. Taking 1 g of sample, placing the sample on rat skin, taking 2ml of receiving solution in 1h, 2h, 4h, 6h and 8h respectively, supplementing blank receiving solution with the same volume, measuring the content of each sample by an HPLC method, and calculating the cumulative permeation quantity Q per unit area, wherein the calculation formula is as follows:

q ═ Σ CnV/a (where CN represents the sample concentration of the sample sampled n times, V represents the liquid in the receiving cell, and a represents the diffusion area).

After the third month, the last test was repeated with the product of the invention. The preservation method for 3 months comprises the following steps: placing at 37 deg.C, sealing and standing.

Third, test results

The cumulative permeation per unit area for the different samples is shown in table 1.

TABLE 1 cumulative permeation per unit area for different samples

Name (R)	Sample 1	Sample 2	Sample 3	Sample No. 4	Reference 1
						Content (wt.)	240.1	258.3	258.9	243.2	113.5

As can be seen from Table 1, the skin penetration of the experimental groups 1-4 was significantly better than that of the control 1.

The cumulative permeation per unit area for the different samples after three months is shown in table 2.

TABLE 2 cumulative permeation per unit area for different samples three months later

The results in table 2 show that the emulsions provided by the present invention still maintain good absorption after three months.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Accordingly, the scope of the invention is to be determined by the claims that follow.

Claims (10)

1. A hyaluronic acid nanoemulsion preparation is characterized by comprising 0.1% -3% of hyaluronic acid, 0.1% -10% of surfactant, 0.1% -20% of cosurfactant, 0.1% -10% of solvent, 0.5% -20% of oil phase, 0.01% -1% of preservative, 0.01% -1% of spice and 54% -95% of distilled water.

2. The milk formulation of claim 1, wherein the hyaluronic acid has a molecular weight of 800-.

3. The emulsion formulation of claim 1, wherein the surfactant is any one or a combination of tween-80, tween-60, triglycerides, sodium lauryl sulfate, polyoxyethylene lauryl ether, polyoxyethylene hydrogenated castor oil.

4. The milk formulation of claim 1, wherein the co-surfactant is any one or a combination of sorbitan monostearate, propylene glycol monostearate, glyceryl monostearate, span 20, span 60 and span 80.

5. The emulsion formulation of claim 1, wherein the oil is one or more of edible tricaprylin, caprylic/capric triglyceride, soybean oil, medicinal liquid paraffin, edible salad oil, castor oil, isopropyl myristate, and ethyl oleate.

6. The emulsion formulation of claim 1, wherein the solvent is any one or a combination of anhydrous ethanol, pentane diol, n-butanol, glycerol, 1, 3-butanediol.

7. The milk preparation of claim 1, wherein the preservative is any one or a combination of phenoxyethanol, ethylhexyl glycerol, benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, and calcium propionate.

8. The milk preparation of claim 1, wherein the flavor is one or more combinations of flavors commonly used in daily use.

9. The emulsion according to any one of claims 1 to 8, wherein the emulsion is a liquid preparation selected from the group consisting of essence, toner, and spray.

10. A process for the preparation of a milk preparation as claimed in claim 9, comprising the steps of:

(1) firstly, dissolving hyaluronic acid by redistilled acetone;

(2) mixing the oil phase, the surfactant, the cosurfactant and the solvent, adding absolute ethyl alcohol which is equal to the total amount of the oil phase, the surfactant, the cosurfactant and the solvent, mixing according to a ratio of 1:1, magnetically stirring for 4 hours, and cooling to below 45 ℃;

(3) slowly adding the hyaluronic acid acetone solution obtained in the step (1) into the solution obtained in the step (2), uniformly stirring by using a high-pressure homogenizer with 1.38 × 108Pa-4.13 × 108Pa, then decompressing to 1.0 × 10-2Pa-1.0 × 104Pa, distilling, removing acetone and ethanol, and cooling to room temperature for later use;

(4) adding water, antiseptic and perfume to obtain hyaluronic acid nanoemulsion.