CN115068368B - Light guide gel and preparation method thereof - Google Patents

Abstract

The invention discloses a light guide gel which comprises the following substances in parts by weight: carbomer 940 0.1-10 parts, glycerin 5-30 parts, sodium ethyl p-hydroxybenzoate 0.001-2 parts, triethanolamine 0.05-15 parts, water for injection 1-95 parts, nano silicon dioxide 0.1-3 parts, hexagonal boron nitride 0.05-0.5 part and amino functional hyaluronic acid 0.1-0.8 part. The invention also discloses a preparation process of the light guide gel, which adopts a natural swelling method, so that on one hand, the molecular structure of the high polymer material is preserved and is not destroyed, and on the other hand, the production efficiency of the product is improved.

Description

Light guide gel and preparation method thereof

Technical Field

The invention relates to the technical field of medical cosmetology, in particular to a light guide gel and a preparation method thereof.

Background

At present, the main product in the market is photon cold gel, which is mainly used for being matched with photon treatment equipment, has the functions of heat insulation and light guide, can prevent skin from being scalded, and can also relieve pain of patients. In the plastic and cosmetic scheme, the photon cryogel can be used as a leading-in product for protecting in operation, has good light transmittance, and has stronger heat conduction performance and no stimulation to skin, so that the protection of a skin barrier system can be ensured, the light guide ratio is uniform, and the stability of therapeutic dosage is ensured. Besides, the use of the gel can also protect the probe, thereby protecting expensive instruments and equipment, being convenient to use, free from corrosion, stimulation, pollution and easy to clean, and being used for cold gel in the cosmetic projects of photons, E light skin tendering, dehairing, freckle removing, electric wave skin pulling and the like.

However, photon cryogels on the market at present have the problem of easily generating skin allergy after being used.

Disclosure of Invention

The invention aims to provide a light guide gel which has the advantages of safe use and good protection effect.

The technical aim of the invention is realized by the following technical scheme:

a light guiding gel comprising the following substances in parts by weight:

the nano silicon dioxide is gas phase silicon dioxide.

By adopting the technical scheme, carbomer is used as a main gel component, gel is formed by utilizing the mutual exclusion of carboxyl ions, a gel skeleton is formed, and the carbomer has better biocompatibility and small skin irritation; the sodium parahydroxybenzoate is used as a preservative, and has small addition amount, low use cost and high safety in the pH neutral range of the light guide gel system; the triethanolamine and the carbomer are neutralized by carboxyl, and the PH is regulated to form a stable high molecular structure, so that the thickening and moisturizing effects are achieved.

The gel system of the light guide gel forms a non-Newtonian fluid, and the modulus, the yield stress and the thixotropic property of the linear viscoelastic region of the light guide gel are increased by adding the silicon dioxide, so that the fluidity of the light guide gel is promoted, and the light guide gel is conveniently and uniformly smeared on the face.

The hexagonal boron nitride has high thermal conductivity, improves the thermal conductivity of the light guide gel, and can quickly transfer local heat through the light guide gel in the photon treatment process, thereby avoiding local burn in the treatment process.

The fumed silica has better dispersibility in water than the precipitated silica, so that the effect of better controlling the dynamic viscoelasticity of the gel can be achieved under the condition of smaller addition amount.

Further set up: the amino functional hyaluronic acid is hyaluronic acid-dopamine graft,

the preparation method comprises the following steps: adding hyaluronic acid into deionized water for dissolution, adding catalysts EDC and NHS, fully stirring, adding dopamine hydrochloride, reacting for 18-36h under the condition of vacuumizing, and removing the catalysts and unreacted monomers to obtain the hyaluronic acid-dopamine graft.

By adopting the technical scheme, the dopamine groups are introduced into the main chain of the hyaluronic acid to change the solution property of pure HA, especially the intermolecular and intermolecular interactions among hyaluronic acid chain segments are changed, and the hydrophobic benzene ring element on the dopamine endows the hyaluronic acid with certain amphiphilicity, so that the hyaluronic acid-dopamine graft contacts with the water phase and the oil phase in the light guide gel respectively and is distributed on the surface of the light guide gel, thereby contacting with the skin, penetrating into the skin surface layer, facilitating the supply of nutrient substances and the discharge of metabolic products, preventing skin aging and playing a role in nourishing the skin.

Further set up: the hexagonal boron nitride is alanine modified hexagonal boron nitride, and the preparation method comprises the following steps:

adding hexagonal boron nitride, alanine and alkaline solution into a ball mill, sieving to remove ball milling beads after ball milling, neutralizing to neutrality by hydrochloric acid, filtering, washing, and vacuum drying to obtain alanine modified hexagonal boron nitride.

Through adopting the technical scheme, interaction between amino groups of alanine and boron atoms of hexagonal boron nitride is promoted by utilizing a ball milling mode, a hexagonal boron nitride sheet layer is thinned, and a layer of carboxyl-containing organic compound is covered on the surface of hexagonal boron nitride, so that compatibility between modified hexagonal boron nitride and a high polymer material is greatly improved, and the modified hexagonal boron nitride can be better combined with a gel system.

Further set up: the light guide gel comprises the following substances in parts by weight:

another object of the present invention is to provide a method for preparing a light guide gel, which has the advantages of high product quality and high production efficiency.

The technical aim of the invention is realized by the following technical scheme:

the preparation method of the light guide gel comprises the following steps:

sp1, putting carbomer 940 into glycerol, and uniformly stirring to obtain carbomer solution;

sp2, adding water into carbomer solution, stirring uniformly, soaking for 6-10h, and fully swelling to obtain pre-gel;

sp3, sequentially dissolving sodium ethyl p-hydroxybenzoate, nano silicon dioxide and amino-functionalized hyaluronic acid in a proper amount of water, and slowly adding the mixture into the pre-gel under the stirring condition to obtain pre-mixed gel;

sp4, adding triethanolamine and hexagonal boron nitride into the premixed gel, and slowly stirring uniformly in vacuum.

By adopting the technical scheme, when the sodium parahydroxybenzoate is used, white precipitate is easy to separate out, namely the parahydroxybenzoate ions capture hydrogen ions in the solution in acidity or weak acidity, the parahydroxybenzoate is restored again, and the parahydroxybenzoate precipitate is separated out under the condition of local over-concentration, so that the solution is prepared before adding, and the solution is slowly added under stirring, so that the precipitation of the parahydroxybenzoate precipitate caused by local over-concentration is prevented.

In summary, the invention has the following beneficial effects: the invention adopts the food preservative sodium ethyl p-hydroxybenzoate, thereby increasing the safety of the product and solving the defects of the current product. Innovations are made in the production process, and the general production process is stirring and shearing through a homogenizer, so that the molecular structure of the high polymer material is broken under the high-speed shearing of the homogenizer, and the viscosity is reduced. The natural swelling method is adopted, so that the molecular structure of the high polymer material is not damaged, and the production efficiency of the product is improved.

Detailed Description

Example 1:

a light guiding gel comprising the following substances by weight: (Unit: g)

The nano silicon dioxide is fumed silica, the amino functional hyaluronic acid is hyaluronic acid-dopamine graft, and the hexagonal boron nitride is alanine modified hexagonal boron nitride.

The preparation method comprises the following steps:

sp1, putting carbomer 940 into glycerol, and uniformly stirring to obtain carbomer solution;

sp2, adding water into carbomer solution, stirring uniformly, soaking for 6-10h, and fully swelling to obtain pre-gel;

sp3, sequentially dissolving sodium ethyl p-hydroxybenzoate, nano silicon dioxide and amino-functionalized hyaluronic acid in a proper amount of water, and slowly adding the mixture into the pre-gel under the stirring condition to obtain pre-mixed gel;

sp4, adding triethanolamine and hexagonal boron nitride into the premixed gel, and slowly stirring uniformly in vacuum.

Example 2:

a light guiding gel comprising the following substances by weight: (Unit: g)

The nano silicon dioxide is fumed silica, the amino functional hyaluronic acid is hyaluronic acid-dopamine graft, and the hexagonal boron nitride is alanine modified hexagonal boron nitride.

The preparation method comprises the following steps:

sp1, putting carbomer 940 into glycerol, and uniformly stirring to obtain carbomer solution;

sp2, adding water into carbomer solution, stirring uniformly, soaking for 6-10h, and fully swelling to obtain pre-gel;

sp3, sequentially dissolving sodium ethyl p-hydroxybenzoate, nano silicon dioxide and amino-functionalized hyaluronic acid in a proper amount of water, and slowly adding the mixture into the pre-gel under the stirring condition to obtain pre-mixed gel;

sp4, adding triethanolamine and hexagonal boron nitride into the premixed gel, and slowly stirring uniformly in vacuum.

Example 3:

a light guiding gel comprising the following substances by weight: (Unit: g)

The nano silicon dioxide is fumed silica, the amino functional hyaluronic acid is hyaluronic acid-dopamine graft, and the hexagonal boron nitride is alanine modified hexagonal boron nitride.

The preparation method comprises the following steps:

sp1, putting carbomer 940 into glycerol, and uniformly stirring to obtain carbomer solution;

sp2, adding water into carbomer solution, stirring uniformly, soaking for 6-10h, and fully swelling to obtain pre-gel;

sp3, sequentially dissolving sodium ethyl p-hydroxybenzoate, nano silicon dioxide and amino-functionalized hyaluronic acid in a proper amount of water, and slowly adding the mixture into the pre-gel under the stirring condition to obtain pre-mixed gel;

sp4, adding triethanolamine and hexagonal boron nitride into the premixed gel, and slowly stirring uniformly in vacuum.

Example 4:

a light guiding gel comprising the following substances by weight: (Unit: g)

The nano silicon dioxide is fumed silica, the amino functional hyaluronic acid is hyaluronic acid-dopamine graft, and the hexagonal boron nitride is alanine modified hexagonal boron nitride.

The preparation method comprises the following steps:

sp1, putting carbomer 940 into glycerol, and uniformly stirring to obtain carbomer solution;

sp2, adding water into carbomer solution, stirring uniformly, soaking for 6-10h, and fully swelling to obtain pre-gel;

sp3, sequentially dissolving sodium ethyl p-hydroxybenzoate, nano silicon dioxide and amino-functionalized hyaluronic acid in a proper amount of water, and slowly adding the mixture into the pre-gel under the stirring condition to obtain pre-mixed gel;

sp4, adding triethanolamine and hexagonal boron nitride into the premixed gel, and slowly stirring uniformly in vacuum.

Example 5:

a light guiding gel comprising the following substances by weight: (Unit: g)

The nano silicon dioxide is fumed silica, the amino functional hyaluronic acid is hyaluronic acid-dopamine graft, and the hexagonal boron nitride is alanine modified hexagonal boron nitride.

The preparation method comprises the following steps:

sp1, putting carbomer 940 into glycerol, and uniformly stirring to obtain carbomer solution;

sp2, adding water into carbomer solution, stirring uniformly, soaking for 6-10h, and fully swelling to obtain pre-gel;

sp3, sequentially dissolving sodium ethyl p-hydroxybenzoate, nano silicon dioxide and amino-functionalized hyaluronic acid in a proper amount of water, and slowly adding the mixture into the pre-gel under the stirring condition to obtain pre-mixed gel;

sp4, adding triethanolamine and hexagonal boron nitride into the premixed gel, and slowly stirring uniformly in vacuum.

Comparative example 1:

a light guiding gel comprising the following substances by weight: (Unit: g)

Wherein the nano silicon dioxide is precipitated silicon dioxide, the amino functional hyaluronic acid is hyaluronic acid-dopamine graft, and the hexagonal boron nitride is alanine modified hexagonal boron nitride.

The preparation method comprises the following steps:

sp1, putting carbomer 940 into glycerol, and uniformly stirring to obtain carbomer solution;

sp2, adding water into carbomer solution, stirring uniformly, soaking for 6-10h, and fully swelling to obtain pre-gel;

sp3, sequentially dissolving sodium ethyl p-hydroxybenzoate, nano silicon dioxide and amino-functionalized hyaluronic acid in a proper amount of water, and slowly adding the mixture into the pre-gel under the stirring condition to obtain pre-mixed gel;

sp4, adding triethanolamine and hexagonal boron nitride into the premixed gel, and slowly stirring uniformly in vacuum.

Comparative example 2:

a light guiding gel comprising the following substances by weight: (Unit: g)

Wherein the nano silicon dioxide is gas phase silicon dioxide, the amino functional hyaluronic acid is hyaluronic acid-dopamine graft, and the hexagonal boron nitride is unmodified hexagonal boron nitride.

The preparation method comprises the following steps:

sp1, putting carbomer 940 into glycerol, and uniformly stirring to obtain carbomer solution;

sp2, adding water into carbomer solution, stirring uniformly, soaking for 6-10h, and fully swelling to obtain pre-gel;

sp3, sequentially dissolving sodium ethyl p-hydroxybenzoate, nano silicon dioxide and amino-functionalized hyaluronic acid in a proper amount of water, and slowly adding the mixture into the pre-gel under the stirring condition to obtain pre-mixed gel;

sp4, adding triethanolamine and hexagonal boron nitride into the premixed gel, and slowly stirring uniformly in vacuum.

Comparative example 3:

a light guiding gel comprising the following substances by weight: (Unit: g)

The nano silicon dioxide is fumed silica, the amino functional hyaluronic acid is hyaluronic acid-dopamine graft, and the hexagonal boron nitride is alanine modified hexagonal boron nitride.

The preparation method comprises the following steps:

sp1, putting carbomer 940 into glycerol, and uniformly stirring to obtain carbomer solution;

sp2, sequentially dissolving sodium ethyl p-hydroxybenzoate, nano silicon dioxide and amino-functionalized hyaluronic acid in a proper amount of water, mixing a carbomer solution with the sodium p-hydroxybenzoate, nano silicon dioxide and amino-functionalized hyaluronic acid, stirring the mixture in a high-speed homogenizer, and swelling the mixture to obtain premixed gel;

sp4, adding triethanolamine and hexagonal boron nitride into the premixed gel, and slowly stirring uniformly in vacuum.

And (3) performance detection:

the hydrogels of the examples and comparative examples were selected for the following tests, respectively:

rotational viscosity detection: the measurement was performed by a third method of rotational viscometer, which is a method of measuring viscosity in the fourth department 0633 of pharmacopoeia of the people's republic of China (2015 edition).

Skin sensitization test: the test solution was used for skin sensitization test according to the method specified in GB/T16886.10-2017.

And (3) light transmittance detection: the hydrogel was cut into small pieces of 20 mm. Times.10 mm. Times.5 mm, placed in a cuvette of 40 mm. Times.10 mm. Times.5 mm, and distilled water was injected into the cuvette. The transmittance of the gel was measured at 500nm using a model 721B visible spectrophotometer.

And (3) heat conduction coefficient detection: the thermal conductivity was measured using a TC3000 thermal conductivity meter. The above test results are recorded in table 1 below.

Table 1 light guide gel test results record table

	Rotational viscosity (cp)	Skin sensitization test	Transmittance of light	Coefficient of thermal conductivity (W/(m.K))
					Example 1	10000-15000	Grade 1 or less	88％	0.675
Example 2	10000-15000	Grade 1 or less	89％	0.684
					Example 3	10000-15000	Grade 1 or less	91％	0.701
Example 4	10000-15000	Grade 1 or less	87％	0.694
					Example 5	10000-15000	Grade 1 or less	86％	0.669
Comparative example 1	15000-20000	Grade 1 or less	88％	0.596
					Comparative example 2	10000-15000	Grade 1 or less	89％	0.537
Comparative example 3	＜10000	Level 2	82％	0.567

As can be seen from table 1, the light guide gel of the embodiment of the invention has better light transmittance, lower skin irritation, higher heat conductivity coefficient, safe use and good light guide and heat dissipation effects; compared with the viscosity of the embodiment, the viscosity of the comparative example 1 is obviously increased, and the fumed silica has better dispersion and lubrication effects compared with the precipitated silica, and simultaneously the heat conductivity coefficient is reduced, mainly because the hexagonal boron nitride is not sufficiently dispersed in the light guide gel, and the heat conductivity is not fully exerted; the hexagonal boron nitride in comparative example 2 has poor bonding ability with gel due to unmodified, and the light guide gel has poor heat conduction performance; comparative example 3 the gel material was damaged in the molecules and the performance was significantly reduced by stirring with a conventional high-speed homogenizer.

The above-described embodiments do not limit the scope of the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the above embodiments should be included in the scope of the present invention.

Claims (5)

1. The light guide gel is characterized by comprising the following substances in parts by weight:

the nano silicon dioxide is gas phase silicon dioxide.

2. The light-guiding gel according to claim 1, wherein the amino-functional hyaluronic acid is a hyaluronic acid-dopamine graft,

the preparation method comprises the following steps: adding hyaluronic acid into deionized water for dissolution, adding catalysts EDC and NHS, fully stirring, adding dopamine hydrochloride, reacting for 18-36h under the condition of vacuumizing, and removing the catalysts and unreacted monomers to obtain the hyaluronic acid-dopamine graft.

3. The light guide gel of claim 1, wherein the hexagonal boron nitride is alanine modified hexagonal boron nitride, and the preparation method comprises:

adding hexagonal boron nitride, alanine and alkaline solution into a ball mill, sieving to remove ball milling beads after ball milling, neutralizing to neutrality by hydrochloric acid, filtering, washing, and vacuum drying to obtain alanine modified hexagonal boron nitride.

4. The light guide gel of claim 1, wherein the light guide gel comprises the following substances in parts by weight:

5. a method for preparing the light guide gel according to any one of claims 1 to 4, comprising the steps of:

sp1, putting carbomer 940 into glycerol, and uniformly stirring to obtain carbomer solution;

sp2, adding water into carbomer solution, stirring uniformly, soaking for 6-10h, and fully swelling to obtain pre-gel;

sp3, sequentially dissolving sodium ethyl p-hydroxybenzoate, nano silicon dioxide and amino-functionalized hyaluronic acid in a proper amount of water, and slowly adding the mixture into the pre-gel under the stirring condition to obtain pre-mixed gel;

sp4, adding triethanolamine and hexagonal boron nitride into the premixed gel, and slowly stirring uniformly in vacuum.