CN111544316A - Fibroin nanofiber-bamboo leaf flavonoid composite material and application thereof in cosmetics - Google Patents
Fibroin nanofiber-bamboo leaf flavonoid composite material and application thereof in cosmetics Download PDFInfo
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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- A—HUMAN NECESSITIES
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
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Abstract
The invention discloses a silk fibroin nanofiber-bamboo leaf flavonoid composite material which comprises silk fibroin nanofibers, bamboo leaf flavonoid and water. On one hand, the physical and chemical properties of the bamboo leaf flavone can be improved, on the other hand, the advantages of the bamboo leaf flavone can be complemented in function, the bamboo leaf flavone has a slow release effect on the surface of skin, and the product function is enhanced; meanwhile, the transdermal performance of the original bamboo leaf flavone is improved. The invention also discloses the application of the composite material in the field of cosmetics. The experimental result shows that the transdermal effect of the bamboo leaf flavone in the emulsion can be effectively improved, and the emulsion has the antibacterial effect and wide application prospect in the field of cosmetics.
Description
Technical Field
The invention relates to a fibroin nanofiber-bamboo leaf flavonoid composite material and application thereof in cosmetics.
Background
The bamboo leaf extract mainly contains bamboo leaf flavone as an active ingredient, has the functions of diminishing inflammation, inhibiting bacteria, repairing skin and the like, is widely applied to textiles, has the function positioning matched with cosmetics, but is poor in solubility and transdermal capacity, difficult to apply to cream emulsion and limited in wide application and extension in cosmetics.
Nano/micro spheres are a microscopic form of biomaterial application, primarily for drug loading and release. Silk proteins contain a certain amount of tyrosine and therefore have a certain degree of reducibility. The large specific surface area and porous structure of the nano-fiber can be used for blood coagulation and skin wound repair. In addition, the fibroin nanofiber is proved to be capable of effectively promoting angiogenesis, and a structure similar to a micelle can be formed by the fibroin nanofiber and can be used as a drug carrier for drug transportation and sustained release. The silk protein drug carrier has amphiphilic property, and can effectively load hydrophilic or hydrophobic drugs. In addition, the silk protein drug carrier also has the advantages of pH responsiveness and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the silk protein nanofiber-bamboo leaf flavonoid composite material, which can improve the physicochemical property of the bamboo leaf flavonoid on one hand, and can form advantage complementation on the other hand on the function, thereby playing a role of slow release on the surface of the skin and enhancing the function of the product; meanwhile, the transdermal performance of the original bamboo leaf flavone is improved; and the bacteriostatic effect of the bamboo leaf flavone is improved.
The specific technical scheme is as follows:
the invention aims to provide a silk fibroin nanofiber-bamboo leaf flavonoid composite material.
A fibroin nanofiber-bamboo leaf flavone composite material comprises fibroin nanofiber, bamboo leaf flavone and water.
Further, the raw materials comprise the following components in parts by weight: 4-6 parts of silk protein nano-fibers, 8-12 parts of bamboo leaf flavones and 50-90 parts of water.
Further, the preparation method of the silk fibroin nanofiber-bamboo leaf flavonoid composite material comprises the following steps:
the raw materials are uniformly mixed and filtered, and the obtained filtrate is placed for 12-24 hours at 4-18 ℃ to obtain a gel product.
The gel product obtained by the invention has stable property, can contain more than 10 wt% of bamboo leaf flavone, and can stably exist in cosmetics such as emulsion, cream and cream; the solubility of bamboo leaf flavone in water is about 0.2 wt%, and the bamboo leaf flavone is easy to separate out and is unstable in a cosmetic system.
Still further, in the filtration, filtration is performed using quick filter paper. The aperture of the rapid filter paper is 80-120 mu m.
The bamboo leaf flavone in the invention is an ethanol extract of bamboo leaves.
The preparation method of the bamboo leaf flavone is preferably as follows: weighing 1 part of bamboo leaf powder, adding 20 parts of 85% ethanol, heating and refluxing for 2 hours, and filtering; repeating the above extraction conditions for extracting again, filtering, mixing filtrates, concentrating under reduced pressure, and freeze drying to obtain bamboo leaf flavone. The parts are parts by weight; the concentration of ethanol is the volume concentration.
The second purpose of the invention is to provide the application of the silk protein nanofiber-bamboo leaf flavonoid composite material.
Specifically, in the field of cosmetics, the fibroin nanofiber-bamboo leaf flavonoid composite material is applied to the formula of emulsion or cream cosmetics; also can be applied to oral care products.
Further, the amount of the fibroin nanofiber-bamboo leaf flavonoid composite material in the cosmetic formula is 1 wt% -10 wt% based on the total mass of the formula.
Wherein the dosage of the emulsion cosmetic is 1-10 wt% of the total mass of the formula; the dosage of the cream cosmetic in the formula is 1-10 wt% of the total mass of the formula.
The third purpose of the invention is to disclose the preparation method of the emulsion containing the fibroin nanofiber-bamboo leaf flavonoid composite material, which comprises the following steps:
weighing the component A in proportion: span 60, tween 60, a160 (2-methoxy-methyl-p-phenylenediamine), GTCC (caprylic/capric triglyceride), shea butter, squalane; mixing the component A and heating to 80-85 ℃;
weighing the component B: water, butanediol, glycerol, xanthan gum and sodium hyaluronate; mixing the component B, and heating to 80-85 ℃;
mixing the component A and the component B, homogenizing for 2-5 min, cooling to 25-45 ℃, adding the fibroin nanofiber-bamboo leaf flavonoid mixed material, and uniformly mixing.
The invention has the following beneficial effects:
the fibroin nanofiber-bamboo leaf flavonoid composite material disclosed by the invention can improve the physicochemical property of bamboo leaf flavonoid on one hand, and can form advantage complementation on the other hand, so that the composite material has a slow release effect on the skin surface and enhances the product function; meanwhile, the transdermal performance of the original bamboo leaf flavone is improved. In addition, the composite material provided by the invention also improves the bacteriostatic effect of the bamboo leaf flavone. The invention expands the application space of the phyllanthin in the cosmetics, not only can be applied to cream emulsion, but also can be widely applied to oral care products.
Drawings
FIG. 1 is a photograph of the mixture of bamboo leaf flavonoid and water in experiment 1;
FIG. 2 is a photograph of the fibroin nanofiber-bamboo leaf flavonoid composite aqueous solution in experiment 1;
fig. 3 is a graph comparing the transdermal effect of bamboo leaf flavonoid in example 1 and comparative example 1 in experiment 2.
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
The bamboo leaf flavone in the embodiment of the invention is extracted from Huzhou bamboo leaves; the silk fibroin nanofiber is a medical carrier material sold in the market; a160 purchased from heliochemistry corporation; GTCC was purchased from CRODA; the rest materials are common materials sold in the market.
Example 1
An emulsion containing fibroin nanofiber-bamboo leaf flavonoid composite materials comprises the following formula:
tween 60 2 wt%, span 60 15 wt%, a160 (2-methoxy-methyl-p-phenylenediamine) 10 wt%, shea butter 1 wt%, squalane 6 wt%, GTCC (caprylic/capric triglyceride), glycerol 6 wt%, butylene glycol 6 wt%, xanthan gum 0.3 wt%, sodium hyaluronate 0.1 wt%, fibroin nanofiber-bamboo leaf flavone 2 wt%, and water 49.6 wt%.
Wherein, span 60, Tween 60, A160, GTCC, shea butter and squalane are used as component A; water, butanediol, glycerin, xanthan gum and sodium hyaluronate are used as the component B.
The preparation method comprises the following steps:
1. preparing bamboo leaf flavone:
weighing 1 part of bamboo leaf powder, adding 20 parts of 85% ethanol, heating to 80 ℃, performing reflux extraction for 2 hours, and filtering; and adding 20 parts of 85% ethanol into the filter residue again, heating to 80 ℃, performing reflux extraction for 2 hours, filtering, combining the filtrates, concentrating under reduced pressure, and freeze-drying to obtain the bamboo leaf flavone.
2. Preparing a fibroin nanofiber-bamboo leaf flavonoid composite material:
uniformly mixing 4 parts of silk protein nanofiber, 8 parts of bamboo leaf flavone and 68 parts of water in parts by weight, filtering by using quick filter paper, and standing the obtained filtrate at 4 ℃ for 12 hours to obtain a gelatinous product, namely the silk protein nanofiber-bamboo leaf flavone.
3. Preparing an emulsion:
mixing the component A and heating to 80-85 ℃; mixing the component B, and heating to 80-85 ℃; mixing the component A and the component B, homogenizing at 14000rpm for 3min, cooling to 45 deg.C, adding fibroin nanofiber-bamboo leaf flavone mixed material, and mixing.
And (5) carrying out stability observation after preparing the emulsion. The emulsions obtained in example 1 were divided into three groups, which were placed at-18 deg.C, 45 deg.C, -18 deg.C and 45 deg.C alternately, and left for 1 month, all kept uniform in texture, and returned to room temperature without precipitation or delamination.
Example 2
An emulsion containing fibroin nanofiber-bamboo leaf flavonoid composite materials comprises the following formula:
tween 60 2 wt%, span 60 15 wt%, a160 (2-methoxy-methyl-p-phenylenediamine) 10 wt%, shea butter 1 wt%, squalane 6 wt%, GTCC (caprylic/capric triglyceride), glycerol 6 wt%, butylene glycol 6 wt%, xanthan gum 0.3 wt%, sodium hyaluronate 0.1 wt%, fibroin nanofiber 5 wt%, bamboo leaf flavone 46.6 wt% and water.
Wherein, span 60, Tween 60, A160, GTCC, shea butter and squalane are used as component A; water, butanediol, glycerin, xanthan gum and sodium hyaluronate are used as the component B.
The preparation method comprises the following steps:
1. preparing bamboo leaf flavone:
same as example 1
2. Preparing a fibroin nanofiber-bamboo leaf flavonoid composite material:
uniformly mixing 5 parts of silk protein nanofiber, 10 parts of bamboo leaf flavone and 50 parts of water in parts by weight, filtering by using quick filter paper, and standing the obtained filtrate at 10 ℃ for 20 hours to obtain a gel product, namely the silk protein nanofiber-bamboo leaf flavone.
3. Preparing an emulsion:
the same as in example 1.
And (5) carrying out stability observation after preparing the emulsion. The emulsions obtained in example 1 were divided into three groups, which were placed at-18 deg.C, 45 deg.C, -18 deg.C and 45 deg.C alternately, and left for 1 month, all kept uniform in texture, and returned to room temperature without precipitation or delamination.
Example 3
An emulsion containing fibroin nanofiber-bamboo leaf flavonoid composite materials comprises the following formula:
tween 60 2 wt%, span 60 15 wt%, a160 (2-methoxy-methyl-p-phenylenediamine) 10 wt%, shea butter 1 wt%, squalane 6 wt%, GTCC (caprylic/capric triglyceride), glycerol 6 wt%, butylene glycol 6 wt%, xanthan gum 0.3 wt%, sodium hyaluronate 0.1 wt%, fibroin nanofiber bamboo leaf flavone 8 wt%, and water 43.6 wt%.
Wherein, span 60, Tween 60, A160, GTCC, shea butter and squalane are used as component A; water, butanediol, glycerin, xanthan gum and sodium hyaluronate are used as the component B.
The preparation method comprises the following steps:
1. preparing bamboo leaf flavone:
same as example 1
2. Preparing a fibroin nanofiber-bamboo leaf flavonoid composite material:
uniformly mixing 4 parts of silk protein nanofiber, 12 parts of bamboo leaf flavone and 80 parts of water in parts by weight, filtering by using quick filter paper, and standing the obtained filtrate at 10 ℃ for 20 hours to obtain a gel product, namely the silk protein nanofiber-bamboo leaf flavone.
3. Preparing an emulsion:
the same as in example 1.
And (5) carrying out stability observation after preparing the emulsion. The emulsions obtained in example 1 were divided into three groups, which were placed at-18 deg.C, 45 deg.C, -18 deg.C and 45 deg.C alternately, and left for 1 month, all kept uniform in texture, and returned to room temperature without precipitation or delamination.
Comparative example 1
The difference from the example 1 is that the emulsion formula replaces 2 wt% of fibroin nanofiber-bamboo leaf flavone with 0.2 wt% of bamboo leaf flavone, and the amount of water is adjusted to 51.4 wt%; the remaining technical features are the same as those of example 1.
The specific formula of the emulsion comprises:
2 wt% of tween 60, 15 wt% of span 60, 10 wt% of A160 (2-methoxy-methyl-p-phenylenediamine), 1 wt% of shea butter, 6 wt% of squalane, 2 wt% of GTCC (caprylic/capric triglyceride), 6 wt% of glycerol, 6 wt% of butanediol, 0.3 wt% of xanthan gum, 0.1 wt% of sodium hyaluronate, 0.2 wt% of bamboo leaf flavone, and 51.4 wt% of water.
Note: in comparative example 1, 0.2% of bamboo leaf flavone was the maximum addition amount not affecting the appearance.
Experiment 1
And comparing the dissolving conditions of the bamboo leaf flavone and silk protein nanofiber-bamboo leaf flavone composite material in water.
The solubility of the bamboo leaf flavone in water is low, and precipitates appear when the solubility is more than 0.2 wt%; in the fibroin nanofiber-bamboo leaf flavone, the bamboo leaf flavone is stable in state and can be freely dissolved with water.
As shown in fig. 1: FIG. 1 shows the mixture of bamboo leaf flavone and water, the mass fractions are 0.5 wt% on the left side and 3 wt% on the right side, respectively, and macroscopic precipitates exist;
as shown in fig. 2: FIG. 2 shows the silk fibroin nanofiber-bamboo leaf flavonoid composite aqueous solution obtained in example 1, wherein the mass fractions of the bamboo leaf flavonoid in the aqueous solution are respectively 13 wt% on the left side and 5 wt% on the right side, and no precipitate is generated. As can be seen from the figure, the solubility of the bamboo leaf flavone of the composite material is greatly improved, and the solution is uniform and stable.
The emulsions obtained in example 1 and comparative example 1 were subjected to a percutaneous absorption test.
The experimental method is as follows: the skin of a female Kunming mouse is given with different emulsion products, and the influence of time and molecular weight on the transdermal absorption rate is respectively inspected by a transdermal absorption instrument.
The skin of the mice was held between the supply and receiving wells with the skin surface facing up. A transdermal experiment is carried out by adopting an improved Franz diffusion cell and taking physiological saline containing 0.5 percent of sodium azide as receiving liquid under the conditions of 32 ℃ and 600r/min of rotating speed. The transdermal area is 1.77cm2The volume of the receiving solution was 6 mL.
Selecting each experimental subject, smearing the lotion on the skin surface, and taking 1mL of the receiving solution after 2h, 4h, 6h, 8h, 10h and 24h, and supplementing with fresh receiving solution. Measuring the content of flavone in the receiving liquid, and calculating the cumulative permeation amount per unit area according to the following formula.
Qn: cumulative penetration per unit area (μ g/cm) of the sample at time t2)；A：Penetration area (1.77 cm)2) (ii) a Cn: time t concentration measurements; ci: a concentration measurement before time t; v: total volume of receiving solution (12 mL); v0: sample volume (1 mL); j: transdermal rate constant. And drawing a curve of Qn to t to obtain a regression equation, wherein the slope of the equation is the transdermal rate constant.
Fig. 3 is a graph of the transdermal permeability of example 1 and comparative example 1.
As can be seen from fig. 3, the transdermal absorption capacity of example 1 is superior to the skin absorption capacity of comparative example 1.
Experiment 3
Experiments for comparing the bacteriostatic effect of the fibroin nanofiber-bamboo leaf flavonoid composite material and the bamboo leaf flavonoid.
Culturing common bacteria of escherichia coli, pseudomonas aeruginosa and staphylococcus aureus to form a skin bacteria mixed bacteria biomembrane. 2 wt% of silk fibroin nanofiber-bamboo leaf flavonoid composite material (prepared in example 1) and 0.2 wt% of bamboo leaf flavonoid suspension bacteria water are respectively prepared and added into a small hole of a prepared biomembrane pore plate, and the mixture is kept for 3 min. Gently washed with physiological saline 3 times (1 mL/time). Saline was used as a control group. The biofilm culture was continued, and the solution was changed every 1h, i.e. all the solution in the system was aspirated, and 1mL of brain-heart extract broth (enriched medium, viable count on flat plate method was used for biofilm count on the bottom of wells at 0, 2, 4, 6 and 8h, respectively, with the results shown in Table 1.
TABLE 1 bacteriostatic effect table
As can be seen from the data in the table, the bacteriostatic effect of the composite material is obviously superior to that of the bamboo leaf flavone, probably because the composite material has a slow release effect, the bacteriostatic effect still shows a certain bacteriostatic ability after 8 hours.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A fibroin nanofiber-bamboo leaf flavonoid composite material is characterized in that raw materials comprise fibroin nanofibers, bamboo leaf flavonoid and water.
2. The silk fibroin nanofiber-bamboo leaf flavonoid composite material as claimed in claim 1, which comprises the following raw materials in parts by weight: 4-6 parts of silk protein nano-fibers, 8-12 parts of bamboo leaf flavones and 50-90 parts of water.
3. The silk fibroin nanofiber-bamboo leaf flavonoid composite material according to claim 1, wherein the preparation method comprises:
the raw materials are uniformly mixed and filtered, and the obtained filtrate is placed for 12-24 hours at 4-18 ℃ to obtain a gelatinous product.
4. The silk fibroin nanofiber-bamboo leaf flavonoid composite material according to claim 3, wherein filtration is performed using a quick filter paper.
5. The use of the fibroin nanofiber-bamboo leaf flavonoid composite material according to any one of claims 1 to 4, wherein the fibroin nanofiber-bamboo leaf flavonoid composite material is used in a formula of an emulsion, a cream cosmetic or an oral care product.
6. The use according to claim 5, wherein the amount of the silk fibroin nanofiber-bamboo leaf flavonoid composite in the cosmetic formulation is 1 wt% to 10 wt% based on the total mass of the formulation.
7. A method for preparing a cosmetic emulsion using the fibroin nanofiber-bamboo leaf flavonoid composite material according to any one of claims 1 to 4, characterized by comprising the steps of:
mixing the component A and heating to 80-85 ℃; mixing the component B, and heating to 80-85 ℃; mixing the component A and the component B, homogenizing for 2-5 min, cooling to 25-45 ℃, and adding a silk fibroin nanofiber-bamboo leaf flavonoid mixed material;
the component A comprises: span 60, tween 60, a160, GTCC, shea butter and squalane;
the component B comprises water, butanediol, glycerol, xanthan gum and sodium hyaluronate.
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