CN114886836B - Triple skin barrier repairing freeze-dried powder essence mask and preparation method thereof - Google Patents
Triple skin barrier repairing freeze-dried powder essence mask and preparation method thereof Download PDFInfo
- Publication number
- CN114886836B CN114886836B CN202210606389.9A CN202210606389A CN114886836B CN 114886836 B CN114886836 B CN 114886836B CN 202210606389 A CN202210606389 A CN 202210606389A CN 114886836 B CN114886836 B CN 114886836B
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- parts
- freeze
- dried powder
- triple
- emulsion
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Classifications
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Abstract
The invention provides a freeze-dried powder essence mask for triple repair of skin barriers and a preparation method thereof, wherein aiming at the characteristics of raw materials, dispersion emulsion and emulsion condensate are respectively prepared, and freeze-dried protective agents consisting of glycosylated extracellular matrix, sodium dodecyl sulfate, amino acid and polyethylene glycol are respectively added step by step to obtain semi-fluid condensate and freeze-dried liquid, so that the freeze-dried powder essence mask of a triple network interaction system of layer coating coated particles can be formed, the loss of core components is avoided, the stability of the interaction system is improved, and when the components exert effects, the freeze-dried powder mask has a sustained release effect of layer-by-layer release, can fully improve and promote the regulation effect of freeze-dried powder for triple repair of skin barriers on immune cells distributed in skin epidermis and dermis, plays the sustainable effects of relieving, anti-inflammatory, anti-allergic and the like, and has different degrees of inhibition effects on growth of malassezia furfur, staphylococcus epidermidis and staphylococcus aureus.
Description
Technical Field
The invention relates to the field of freeze-dried powder masks, in particular to a freeze-dried powder essence mask for triple skin barrier repair and a preparation method thereof.
Background
The skin is the largest organ of the human body, plays a role in effectively protecting tissues and organs in the body from being damaged by external substances such as pathogenic microorganisms, and avoids and repairs the mechanical damages such as physical and the like, and is a natural barrier for protecting the human body. When the natural barrier of the skin is damaged, the body resistance is reduced, and inflammatory reactions such as itching, redness, stinging and the like are easily caused. The immune barrier in the natural barrier refers to immune cells distributed in the epidermis and dermis of the skin, which have important regulatory effects in the immune response and inflammatory response of the body, wherein macrophages are immune cells which secrete inflammatory factors with inflammatory effects such as interleukin-6, tumor necrosis factor-alpha and the like when stimulated, and further exacerbate the inflammatory response and form complications. Thus, after the immune barrier of the skin is compromised, immune cells are further activated and activated, often resulting in prolonged sustained damage to the facial skin.
The freeze-dried powder mask is a solid dry film type mask prepared by fusing components such as mask stock solution, thickener, humectant and the like with mask cloth and performing vacuum freeze drying. However, after vacuum freeze drying, the added components are usually changed due to factors such as time and environment, so that the fusion degree and stability of the components are influenced during use, and even the functional activity of the core components is influenced, and further the problems of inferior use effect as compared with a liquid dressing mask, insignificant efficacy and the like are caused.
Disclosure of Invention
In view of the above, the present invention aims to provide a freeze-dried powder essence mask for triple skin barrier repair and a preparation method thereof, which solve the above problems.
The technical scheme of the invention is realized as follows:
a preparation method of a freeze-dried powder essence mask for triple skin barrier repair comprises the following steps:
s1, taking polyglycerol-10 oleate, hydroxyethyl urea, sodium hyaluronate and butanediol, adding mussel extract, tremella fruit body extract, centella asiatica leaf extract and beta-glucan after ultrasonic dispersion, and dispersing emulsion;
s2, adding a freeze-drying protective agent a into the dispersion emulsion, and stirring to obtain semi-fluid gel;
s3, mixing glycerol, polyglycerol-2 oleate, lecithin, 1, 2-pentanediol and acrylic acid (ester) copolymer sodium, and homogenizing to obtain an emulsion;
s4, adding palmitoyl tripeptide-8, 4-tertiary butyl cyclohexanol and squalane into water, stirring, adding an emulsion, and adding a semi-fluid gel while homogenizing after ultrasonic dispersion to obtain an emulsion gel;
s5, adding a freeze-drying protective agent b into the emulsified condensate to obtain freeze-drying liquid;
the lyoprotectant a and the lyoprotectant b consist of glycosylated extracellular matrix, sodium dodecyl sulfate, amino acid and polyethylene glycol;
s6, adding the freeze-dried liquid into mask cloth, and performing vacuum freeze drying to obtain the freeze-dried powder essence mask for triple skin barrier repair.
Further, the preparation method of the glycosylated extracellular matrix comprises the following steps: taking extracellular matrix, adding phosphate buffer solution, oscillating, carrying out low-temperature hydrolysis reaction, adding nanocellulose crystal, carrying out water bath reaction, and cooling to obtain glycosylated extracellular matrix.
Further, the preparation method of the glycosylated extracellular matrix comprises the following steps: taking extracellular matrix, adding phosphate buffer solution, oscillating, carrying out hydration reaction for 1-2h at 4-8 ℃, adding nano cellulose crystal, carrying out water bath reaction for 1-2h at 50-60 ℃, and cooling to obtain glycosylated extracellular matrix.
Further, the mass ratio of the extracellular matrix, the phosphate buffer solution and the nanocellulose crystal is 1:3-4:0.08-0.1; the extracellular matrix is taken from adipose tissue of a mammal.
Further, the lyoprotectant a and the lyoprotectant b consist of 20-28 parts of glycosylated extracellular matrix, 12-16 parts of sodium dodecyl sulfate, 9-14 parts of amino acid and 4-7 parts of polyethylene glycol according to parts by weight; the amino acid is at least one of proline, L-tryptophan, sarcosine, L-tyrosine, phenylalanine and arginine;
further, the addition amount of the freeze-drying protective agent a is 1-3% of the weight of the dispersion emulsion; the addition amount of the freeze-drying protective agent b is 3-5% of the weight of the emulsified condensate.
Further, adding semi-fluid gel while homogenizing under 10-20MPa and 3000-5000 r/min; and adding the semi-fluid gel liquid every 30-60s for 5 times.
Further, by weight, 8-12 parts of mussel extract, 4-7 parts of palmitoyl tripeptide-8, 3-6 parts of beta-glucan, 6-9 parts of tremella fruit body extract, 6-9 parts of centella asiatica leaf extract, 7-10 parts of 4-tert-butylcyclohexanol, 4-9 parts of squalane, 4-6 parts of jojoba seed oil, 8-15 parts of polyglycerol-10 oleate, 10-14 parts of hydroxyethyl urea, 12-19 parts of sodium hyaluronate, 6-8 parts of sodium (ester) acrylic acid copolymer, 3-4 parts of butanediol, 6-8 parts of polyglycerol-2 oleate, 3-5 parts of lecithin, 5-9 parts of 1, 2-pentanediol, 10-17 parts of glycerol and 30-50 parts of water.
Further, by weight, 10 parts of mussel extract, 5 parts of palmitoyl tripeptide-8, 4 parts of beta-glucan, 7 parts of tremella fruit body extract, 8 parts of centella asiatica leaf extract, 8 parts of 4-tert-butylcyclohexanol, 6 parts of squalane, 5 parts of jojoba seed oil, 12 parts of polyglycerol-10 oleate, 12 parts of hydroxyethyl urea, 15 parts of sodium hyaluronate, 7 parts of sodium acrylate copolymer, 3 parts of butanediol, 7 parts of polyglycerol-2 oleate, 4 parts of lecithin, 7 parts of 1, 2-pentanediol, 13 parts of glycerol and 40 parts of water.
An application of lyophilized powder essence facial mask for triple skin barrier repair in improving skin inflammation, allergy and pruritus is provided.
Compared with the prior art, the invention has the beneficial effects that:
aiming at the characteristics of raw materials, the invention respectively prepares dispersion emulsion and emulsion condensate, and then respectively obtains semi-fluid gel and freeze-dried liquid by adding freeze-dried protective agent composed of glycosylated extracellular matrix, sodium dodecyl sulfate, amino acid and polyethylene glycol step by step, thus forming a triple network interaction system of layer coating and coating particles, the obtained freeze-dried powder essence mask for triple repairing skin barrier has the function of improving 4D barriers of permeability barrier, immune barrier, microorganism barrier and photoprotection barrier on facial skin, especially the immune barrier, can regulate immune cells distributed in skin epidermis and dermis, and can avoid the barrier dysfunction to further cause symptoms such as skin inflammation, allergy, inflammatory pruritus and the like.
Aiming at the characteristics of raw materials, the invention respectively prepares the dispersion emulsion and the emulsion condensate, and then the freeze-drying protective agent consisting of glycosylated extracellular matrix, sodium dodecyl sulfate, amino acid and polyethylene glycol is added step by step to respectively obtain semi-fluid gel and freeze-drying liquid, thus forming a freeze-dried powder essence mask of a triple network interaction system with layer coating and coating particles, being beneficial to avoiding the loss of core components and improving the stability of the interaction system, and having the slow release function of releasing layer by layer when the components play a role, fully improving and promoting the regulating function of the freeze-dried powder of triple repairing skin barrier on immune cells distributed in skin epidermis and dermis, playing the sustainable roles of relieving, anti-inflammatory, anti-allergic and the like, and having different degrees of inhibiting effects on the growth of malassezia furfur, staphylococcus epidermidis and staphylococcus aureus, having good regulating function on the microecological balance of skin epidermis, and being beneficial to maintaining and improving the microecological and skin health of skin.
In addition, the glycosylated extracellular matrix is prepared by adopting the nanocellulose crystal, so that the glycosylated extracellular matrix plays a role in supporting a triple network, the combination degree of components and immune cells is easier to promote after glycosylation treatment, and the regulation effect of freeze-dried powder for triple repairing skin barriers on the immune cells is promoted.
Detailed Description
In order to better understand the technical content of the present invention, the following provides specific examples to further illustrate the present invention.
The experimental methods used in the embodiment of the invention are conventional methods unless otherwise specified.
Materials, reagents, and the like used in the examples of the present invention are commercially available unless otherwise specified.
Example 1
10 parts of mussel extract, 5 parts of palmitoyl tripeptide-8, 4 parts of beta-glucan, 7 parts of tremella fruit body extract, 8 parts of centella asiatica leaf extract, 8 parts of 4-tert-butylcyclohexanol, 6 parts of squalane, 5 parts of jojoba seed oil, 12 parts of polyglycerol-10 oleate, 12 parts of hydroxyethyl urea, 15 parts of sodium hyaluronate, 7 parts of sodium acrylate copolymer, 3 parts of butanediol, 7 parts of polyglycerol-2 oleate, 4 parts of lecithin, 7 parts of 1, 2-pentanediol, 13 parts of glycerol and 40 parts of water;
the preparation method of the freeze-dried powder essence mask for triple skin barrier repair comprises the following steps:
s1, taking polyglycerol-10 oleate, hydroxyethyl urea, sodium hyaluronate and butanediol, adding mussel extract, tremella fruit body extract, centella asiatica leaf extract and beta-glucan after ultrasonic dispersion, and dispersing emulsion;
s2, adding a freeze-drying protective agent a accounting for 1% of the weight of the dispersion emulsion into the dispersion emulsion, and stirring to obtain semi-fluid gel;
s3, mixing glycerol, polyglycerol-2 oleate, lecithin, 1, 2-pentanediol and acrylic acid (ester) copolymer sodium, and homogenizing to obtain an emulsion;
s4, adding palmitoyl tripeptide-8, 4-tert-butylcyclohexanol, squalane and jojoba seed oil into water, stirring, adding an emulsion, performing ultrasonic dispersion, adding a semi-fluid gel while homogenizing at 15MPa and 4000r/min, and adding the semi-fluid gel every 30-60S for 5 times to obtain an emulsion;
s5, adding a freeze-drying protective agent b accounting for 3% of the weight of the emulsified condensate into the emulsified condensate to obtain freeze-drying liquid;
the freeze-drying protective agent a and the freeze-drying protective agent b consist of 20 parts of glycosylated extracellular matrix, 12 parts of sodium dodecyl sulfate, 9 parts of amino acid and 4 parts of polyethylene glycol; the amino acid is prepared from the following components in percentage by mass: 1:1, L-tryptophan and sarcosine;
the preparation method of the glycosylated extracellular matrix comprises the following steps: the mass ratio is 1:3:0.08, taking extracellular matrix in adipose tissue, adding phosphate buffer, oscillating, carrying out hydration reaction for 1h at 4-8 ℃, adding nanocellulose crystal, carrying out water bath reaction for 1h at 50-60 ℃, and cooling to obtain glycosylated extracellular matrix.
S6, adding the freeze-dried liquid into mask cloth, and performing vacuum freeze drying to obtain the freeze-dried powder essence mask for triple skin barrier repair.
Example 2
10 parts of mussel extract, 5 parts of palmitoyl tripeptide-8, 4 parts of beta-glucan, 7 parts of tremella fruit body extract, 8 parts of centella asiatica leaf extract, 8 parts of 4-tert-butylcyclohexanol, 6 parts of squalane, 5 parts of jojoba seed oil, 12 parts of polyglycerol-10 oleate, 12 parts of hydroxyethyl urea, 15 parts of sodium hyaluronate, 7 parts of sodium acrylate copolymer, 3 parts of butanediol, 7 parts of polyglycerol-2 oleate, 4 parts of lecithin, 7 parts of 1, 2-pentanediol, 13 parts of glycerol and 40 parts of water;
the preparation method of the freeze-dried powder essence mask for triple skin barrier repair comprises the following steps:
s1, taking polyglycerol-10 oleate, hydroxyethyl urea, sodium hyaluronate and butanediol, adding mussel extract, tremella fruit body extract, centella asiatica leaf extract and beta-glucan after ultrasonic dispersion, and dispersing emulsion;
s2, adding 3% of freeze-drying protective agent a by weight of the dispersion emulsion into the dispersion emulsion, and stirring to obtain semi-fluid gel;
s3, mixing glycerol, polyglycerol-2 oleate, lecithin, 1, 2-pentanediol and acrylic acid (ester) copolymer sodium, and homogenizing to obtain an emulsion;
s4, adding palmitoyl tripeptide-8, 4-tert-butylcyclohexanol, squalane and jojoba seed oil into water, stirring, adding an emulsion, performing ultrasonic dispersion, adding a semi-fluid gel while homogenizing at 15MPa and 4000r/min, and adding the semi-fluid gel every 30-60S for 5 times to obtain an emulsion;
s5, adding a freeze-drying protective agent b accounting for 5% of the weight of the emulsified condensate into the emulsified condensate to obtain freeze-drying liquid;
the lyoprotectant a and the lyoprotectant b consist of 28 parts of glycosylated extracellular matrix, 16 parts of sodium dodecyl sulfate, 14 parts of amino acid and 7 parts of polyethylene glycol; the amino acid is prepared from the following components in percentage by mass: 1:1:1:1, proline, L-tryptophan, sarcosine, L-tyrosine and phenylalanine;
the preparation method of the glycosylated extracellular matrix comprises the following steps: the mass ratio is 1:4:0.1, taking extracellular matrix in adipose tissue, adding phosphate buffer, oscillating, carrying out hydration reaction for 2 hours at 4-8 ℃, adding nanocellulose crystal, carrying out water bath reaction for 2 hours at 50-60 ℃, and cooling to obtain glycosylated extracellular matrix.
S6, adding the freeze-dried liquid into mask cloth, and performing vacuum freeze drying to obtain the freeze-dried powder essence mask for triple skin barrier repair.
Example 3
10 parts of mussel extract, 5 parts of palmitoyl tripeptide-8, 4 parts of beta-glucan, 7 parts of tremella fruit body extract, 8 parts of centella asiatica leaf extract, 8 parts of 4-tert-butylcyclohexanol, 6 parts of squalane, 5 parts of jojoba seed oil, 12 parts of polyglycerol-10 oleate, 12 parts of hydroxyethyl urea, 15 parts of sodium hyaluronate, 7 parts of sodium acrylate copolymer, 3 parts of butanediol, 7 parts of polyglycerol-2 oleate, 4 parts of lecithin, 7 parts of 1, 2-pentanediol, 13 parts of glycerol and 40 parts of water;
the preparation method of the freeze-dried powder essence mask for triple skin barrier repair comprises the following steps:
s1, taking polyglycerol-10 oleate, hydroxyethyl urea, sodium hyaluronate and butanediol, adding mussel extract, tremella fruit body extract, centella asiatica leaf extract and beta-glucan after ultrasonic dispersion, and dispersing emulsion;
s2, adding a freeze-drying protective agent a accounting for 2% of the weight of the dispersion emulsion into the dispersion emulsion, and stirring to obtain semi-fluid gel;
s3, mixing glycerol, polyglycerol-2 oleate, lecithin, 1, 2-pentanediol and acrylic acid (ester) copolymer sodium, and homogenizing to obtain an emulsion;
s4, adding palmitoyl tripeptide-8, 4-tert-butylcyclohexanol, squalane and jojoba seed oil into water, stirring, adding an emulsion, performing ultrasonic dispersion, adding a semi-fluid gel while homogenizing at 15MPa and 4000r/min, and adding the semi-fluid gel every 30-60S for 5 times to obtain an emulsion;
s5, adding a freeze-drying protective agent b accounting for 4% of the weight of the emulsified condensate into the emulsified condensate to obtain freeze-drying liquid;
the freeze-drying protective agent a and the freeze-drying protective agent b consist of 24 parts of glycosylated extracellular matrix, 14 parts of sodium dodecyl sulfate, 12 parts of amino acid and 5 parts of polyethylene glycol; the amino acid is prepared from the following components in percentage by mass: 1:1:1:1, proline, L-tryptophan, sarcosine, L-tyrosine and phenylalanine;
the preparation method of the glycosylated extracellular matrix comprises the following steps: the mass ratio is 1:3:0.09, taking extracellular matrix in adipose tissue, adding phosphate buffer, oscillating, carrying out hydration reaction for 2 hours at 4-8 ℃, adding nanocellulose crystal, carrying out water bath reaction for 2 hours at 50-60 ℃, and cooling to obtain glycosylated extracellular matrix.
S6, adding the freeze-dried liquid into mask cloth, and performing vacuum freeze drying to obtain the freeze-dried powder essence mask for triple skin barrier repair.
Comparative example 1
10 parts of mussel extract, 5 parts of palmitoyl tripeptide-8, 4 parts of beta-glucan, 7 parts of tremella fruit body extract, 8 parts of centella asiatica leaf extract, 8 parts of 4-tert-butylcyclohexanol, 6 parts of squalane, 5 parts of jojoba seed oil, 12 parts of polyglycerol-10 oleate, 12 parts of hydroxyethyl urea, 15 parts of sodium hyaluronate, 7 parts of sodium acrylate copolymer, 3 parts of butanediol, 7 parts of polyglycerol-2 oleate, 4 parts of lecithin, 7 parts of 1, 2-pentanediol, 13 parts of glycerol and 40 parts of water;
the preparation method of the freeze-dried powder essence mask for triple skin barrier repair comprises the following steps:
s1, taking polyglycerol-10 oleate, hydroxyethyl urea, sodium hyaluronate and butanediol, adding mussel extract, tremella fruit body extract, centella asiatica leaf extract and beta-glucan after ultrasonic dispersion, and dispersing emulsion;
s2, mixing glycerol, polyglycerol-2 oleate, lecithin, 1, 2-pentanediol and acrylic acid (ester) copolymer sodium, and homogenizing to obtain an emulsion;
s3, adding palmitoyl tripeptide-8, 4-tert-butylcyclohexanol, squalane and jojoba seed oil into water, stirring, adding an emulsion, adding a dispersion emulsion while homogenizing at 15MPa and 4000r/min after ultrasonic dispersion, and adding a semi-fluid gel every 30-60S for 5 times to obtain an emulsion gel;
s4, adding a freeze-drying protective agent b accounting for 5% of the weight of the emulsified condensate into the emulsified condensate to obtain freeze-drying liquid;
the freeze-drying protective agent b consists of 24 parts of glycosylated extracellular matrix, 14 parts of sodium dodecyl sulfate, 12 parts of amino acid and 5 parts of polyethylene glycol; the amino acid is prepared from the following components in percentage by mass: 1:1:1:1, proline, L-tryptophan, sarcosine, L-tyrosine and phenylalanine;
the preparation method of the glycosylated extracellular matrix comprises the following steps: the mass ratio is 1:3:0.09, taking extracellular matrix in adipose tissue, adding phosphate buffer, oscillating, carrying out hydration reaction for 2 hours at 4-8 ℃, adding nanocellulose crystal, carrying out water bath reaction for 2 hours at 50-60 ℃, and cooling to obtain glycosylated extracellular matrix.
S5, adding the freeze-dried liquid into mask cloth, and performing vacuum freeze drying to obtain the freeze-dried powder essence mask for triple skin barrier repair.
Comparative example 2
10 parts of mussel extract, 5 parts of palmitoyl tripeptide-8, 4 parts of beta-glucan, 7 parts of tremella fruit body extract, 8 parts of centella asiatica leaf extract, 8 parts of 4-tert-butylcyclohexanol, 6 parts of squalane, 5 parts of jojoba seed oil, 12 parts of polyglycerol-10 oleate, 12 parts of hydroxyethyl urea, 15 parts of sodium hyaluronate, 7 parts of sodium acrylate copolymer, 3 parts of butanediol, 7 parts of polyglycerol-2 oleate, 4 parts of lecithin, 7 parts of 1, 2-pentanediol, 13 parts of glycerol and 40 parts of water;
the preparation method of the freeze-dried powder essence mask for triple skin barrier repair comprises the following steps:
s1, mixing polyglycerol-10 oleate, hydroxyethyl urea, sodium hyaluronate, butanediol, glycerol, polyglycerol-2 oleate, lecithin, 1, 2-pentanediol and sodium acrylate copolymer, performing ultrasonic dispersion, adding mussel extract, tremella fruit body extract, centella asiatica leaf extract, beta-glucan, palmitoyl tripeptide-8, 4-tert-butylcyclohexanol, squalane, jojoba seed oil and water, and performing ultrasonic dispersion to obtain a dispersion emulsion;
s2, adding a freeze-drying protective agent b accounting for 5% of the weight of the dispersion emulsion into the dispersion emulsion, and stirring to obtain freeze-drying liquid;
the freeze-drying protective agent b consists of 24 parts of glycosylated extracellular matrix, 14 parts of sodium dodecyl sulfate, 12 parts of amino acid and 5 parts of polyethylene glycol; the amino acid is prepared from the following components in percentage by mass: 1:1:1:1, proline, L-tryptophan, sarcosine, L-tyrosine and phenylalanine;
the preparation method of the glycosylated extracellular matrix comprises the following steps: the mass ratio is 1:3:0.09, taking extracellular matrix in adipose tissue, adding phosphate buffer, oscillating, carrying out hydration reaction for 2 hours at 4-8 ℃, adding nanocellulose crystal, carrying out water bath reaction for 2 hours at 50-60 ℃, and cooling to obtain glycosylated extracellular matrix.
And S3, adding the freeze-dried liquid into mask cloth, and performing vacuum freeze drying to obtain the freeze-dried powder essence mask for triple skin barrier repair.
Comparative example 3
10 parts of mussel extract, 5 parts of palmitoyl tripeptide-8, 4 parts of beta-glucan, 7 parts of tremella fruit body extract, 8 parts of centella asiatica leaf extract, 8 parts of 4-tert-butylcyclohexanol, 6 parts of squalane, 5 parts of jojoba seed oil, 12 parts of polyglycerol-10 oleate, 12 parts of hydroxyethyl urea, 15 parts of sodium hyaluronate, 7 parts of sodium acrylate copolymer, 3 parts of butanediol, 7 parts of polyglycerol-2 oleate, 4 parts of lecithin, 7 parts of 1, 2-pentanediol, 13 parts of glycerol and 40 parts of water;
the preparation method of the freeze-dried powder essence mask for triple skin barrier repair comprises the following steps:
s1, taking polyglycerol-10 oleate, hydroxyethyl urea, sodium hyaluronate and butanediol, adding mussel extract, tremella fruit body extract, centella asiatica leaf extract and beta-glucan after ultrasonic dispersion, and dispersing emulsion;
s2, adding a freeze-drying protective agent a accounting for 2% of the weight of the dispersion emulsion into the dispersion emulsion, and stirring to obtain semi-fluid gel;
s3, mixing glycerol, polyglycerol-2 oleate, lecithin, 1, 2-pentanediol and acrylic acid (ester) copolymer sodium, and homogenizing to obtain an emulsion;
s4, adding palmitoyl tripeptide-8, 4-tert-butylcyclohexanol, squalane and jojoba seed oil into water, stirring, adding an emulsion, performing ultrasonic dispersion, adding a semi-fluid gel while homogenizing at 15MPa and 4000r/min, and adding the semi-fluid gel every 30-60S for 5 times to obtain an emulsion;
s5, adding a freeze-drying protective agent b accounting for 4% of the weight of the emulsified condensate into the emulsified condensate to obtain freeze-drying liquid;
the freeze-drying protective agent a and the freeze-drying protective agent b consist of 24 parts of extracellular matrix, 14 parts of sodium dodecyl sulfate, 12 parts of amino acid and 5 parts of polyethylene glycol; the amino acid is prepared from the following components in percentage by mass: 1:1:1:1, proline, L-tryptophan, sarcosine, L-tyrosine and phenylalanine;
s6, adding the freeze-dried liquid into mask cloth, and performing vacuum freeze drying to obtain the freeze-dried powder essence mask for triple skin barrier repair.
Comparative example 4
10 parts of mussel extract, 5 parts of palmitoyl tripeptide-8, 4 parts of beta-glucan, 7 parts of tremella fruit body extract, 8 parts of centella asiatica leaf extract, 8 parts of 4-tert-butylcyclohexanol, 6 parts of squalane, 5 parts of jojoba seed oil, 12 parts of polyglycerol-10 oleate, 12 parts of hydroxyethyl urea, 15 parts of sodium hyaluronate, 7 parts of sodium acrylate copolymer, 3 parts of butanediol, 7 parts of polyglycerol-2 oleate, 4 parts of lecithin, 7 parts of 1, 2-pentanediol, 13 parts of glycerol and 40 parts of water;
the preparation method of the freeze-dried powder essence mask for triple skin barrier repair comprises the following steps:
s1, taking polyglycerol-10 oleate, hydroxyethyl urea, sodium hyaluronate and butanediol, adding mussel extract, tremella fruit body extract, centella asiatica leaf extract and beta-glucan after ultrasonic dispersion, and dispersing emulsion;
s2, mixing glycerol, polyglycerol-2 oleate, lecithin, 1, 2-pentanediol and acrylic acid (ester) copolymer sodium, and homogenizing to obtain an emulsion;
s4, adding palmitoyl tripeptide-8, 4-tert-butylcyclohexanol, squalane and jojoba seed oil into water, stirring, adding an emulsion, performing ultrasonic dispersion, adding a semi-fluid gel while homogenizing at 15MPa and 4000r/min, and adding the semi-fluid gel every 30-60S for 5 times to obtain an emulsion;
s5, adding the emulsified condensate into mask cloth, and performing vacuum freeze drying to obtain the freeze-dried powder essence mask for triple skin barrier repair.
Test example 1-Effect of lyophilized powder for triple skin Barrier on macrophage secretion of inflammatory factors TNF-a, IL-6
(1) Macrophage culture liquid: culturing mouse RAW264.7 macrophage in DMEM medium containing 10% foetus calf serum to logarithmic phase, adding EDTA-containing pancreatin, centrifuging at 1000rpm for 4min, collecting precipitate, adding DMEM medium containing 10% foetus calf serum, and blowing uniformly to obtain cell concentration of 1×10 per hole 5 Individual/mL, 500. Mu.L was inoculated into 96-well ELISA plates at 37℃with 5% CO 2 Culturing for 12h in a constant temperature incubator to obtain macrophage culture solution;
(2) Sample to be measured: adding the obtained freeze-dried powder for triple skin barrier repair into a DMEM (DMEM) medium containing 10% of fetal calf serum for dissolution, and preparing a sample to be tested of 300 mu L/mL;
(3) Lipopolysaccharide-induced macrophage culture fluid: sucking out the culture medium of the ELISA plate macrophage culture liquid, adding 500 μl of sample to be detected, and heating at 37deg.C with 5% CO 2 Culturing in a constant temperature incubator for 4 hr, removing culture supernatant, adding DMEM medium containing 10% foetal calf serum, adding Lipopolysaccharide (LPS) with concentration of 500 μg/mL, adding at 37deg.C and 5% CO 2 Culturing in a constant temperature incubator for 36h, collecting supernatant, centrifuging at 5000rpm for 4min, and collecting supernatant to obtain lipopolysaccharide induced macrophage culture liquid;
(4) And (3) detection: the Interleukin-6 content is detected by using an Interleukin-6 detection kit, interleukin-6 (IL-6 for short) is detected by using a tumor necrosis factor-alpha detection kit, the tumor necrosis factor-alpha (tumor necrosis factor for short) is detected by using dexamethasone as a positive control, and a lipopolysaccharide-induced macrophage culture solution without a sample to be detected is used as a blank control, and the test results are shown in the following table:
| project | IL-6(ng/mL) | TNF-α(ng/mL) |
| Example 1 | 6.8 | 35.1 |
| Example 2 | 6.3 | 33.6 |
| Example 3 | 5.7 | 34.4 |
| Comparative example 1 | 10.5 | 38.5 |
| Comparative example 2 | 9.0 | 38.8 |
| Comparative example 3 | 11.8 | 40.5 |
| Comparative example 4 | 13.0 | 41.2 |
| Blank control | 22.9 | 52.0 |
| Positive control | 4.5 | 20.6 |
From the above table, examples 1 to 3 have different degrees of inhibition effects on inflammatory factors TNF-a and IL-6 secreted by macrophages, wherein the inhibition effect on inflammatory factors IL-6 is better, which shows that the invention aims at the characteristics of raw materials, respectively prepares dispersion emulsion and emulsion condensate, and then respectively obtains semi-fluid gel and freeze-dried liquid by adding freeze-dried protective agents composed of glycosylated extracellular matrix, sodium dodecyl sulfate, amino acid and polyethylene glycol step by step, thus forming a triple network interaction system of layer coating coated particles, which is beneficial to avoiding the loss of core components, improving the stability of the interaction system, and has a sustained release effect of layer-by-layer release, which can fully improve and promote the regulation effect of freeze-dried powder of triple repair skin barrier on immune cells distributed in skin epidermis and dermis, and plays the continuous roles of relieving, anti-inflammatory, anti-allergic, anti-inflammatory skin itch and the like.
By comparing example 3, comparative example 1 and comparative example 2, the comparative example 1 and comparative example 2 have higher content of inflammatory factors TNF-a and IL-6 secreted by lipopolysaccharide-induced macrophages, which indicates that the stepwise addition of the lyoprotectant not only helps to reduce the loss degree of the components in the process of preparation, but also can lead the components to have sustained release effect of releasing layer by utilizing a triple network interaction system of the lyoprotectant and the components forming a layer coating to coat the particles, thereby playing a role in continuously regulating macrophages.
As is clear from comparative examples 3 and 3, the preparation of glycosylated extracellular matrix with nanocellulose crystals not only plays a role in supporting triple network, but also facilitates the combination of components and immune cells after glycosylation treatment, and promotes the regulation of immune cells by lyophilized powder for triple repair of skin barrier.
As is clear from comparative examples 3 and 4, comparative example 4 shows that the lipopolysaccharide induces macrophages to secrete inflammatory factors TNF-a and IL-6, especially TNF-a, the stepwise addition of the lyoprotectant is helpful to forming a triple network interaction system of coating particles, thereby avoiding the loss of core components and improving the stability among the components.
Test example 2-inhibition of growth of Malassezia furfur, staphylococcus epidermidis, and the like by lyophilized powder for triple repair of skin Barrier
Malassezia furfur (Malassezia furfur) and staphylococcus epidermidis (Staphylococcus epiderm)Respectively culturing idis) and staphylococcus aureus (Staphylococcus aureus) into 96-well ELISA plates, adding 300 μl of culture solution, culturing in a constant temperature incubator at 37deg.C until OD value of bacterial solution is 0.2-0.35, adding 30 μl of lyophilized powder diluent for triple repairing skin barrier, and measuring absorbance value A at 600nm by spectrophotometry 1 Culturing in a constant temperature incubator at 37deg.C for 8 hr, and measuring absorbance A at 600nm 2 A sterile culture medium was used as negative control A 0 The inhibition rate calculation formula: inhibition (%) = (a) 0 -A 1 -A 2 )/A 0 X 100, results are given in the following table:
according to the characteristics of the raw materials, the invention respectively prepares the dispersion emulsion and the emulsion condensate, and then the freeze-drying protective agent consisting of glycosylated extracellular matrix, sodium dodecyl sulfate, amino acid and polyethylene glycol is added step by step to respectively obtain semi-fluid gel and freeze-drying liquid, so that the freeze-dried powder for triple repairing of the skin barrier of the triple network interaction system of the layer coating coated particles can be obtained.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (8)
1. The preparation method of the freeze-dried powder essence mask for triple skin barrier repair is characterized by comprising the following steps of:
s1, taking polyglycerol-10 oleate, hydroxyethyl urea, sodium hyaluronate and butanediol, adding mussel extract, tremella fruit body extract, centella asiatica leaf extract and beta-glucan after ultrasonic dispersion, and dispersing emulsion;
s2, adding a freeze-drying protective agent a into the dispersion emulsion, and stirring to obtain semi-fluid gel;
s3, mixing glycerol, polyglycerol-2 oleate, lecithin, 1, 2-pentanediol and acrylic acid (ester) copolymer sodium, and homogenizing to obtain an emulsion;
s4, adding palmitoyl tripeptide-8, 4-tertiary butyl cyclohexanol, squalane and jojoba seed oil into water, stirring, adding an emulsion, and adding a semi-fluid gel while homogenizing after ultrasonic dispersion to obtain an emulsion gel;
s5, adding a freeze-drying protective agent b into the emulsified condensate to obtain freeze-drying liquid;
the lyoprotectant a and the lyoprotectant b consist of glycosylated extracellular matrix, sodium dodecyl sulfate, amino acid and polyethylene glycol;
the preparation method of the glycosylated extracellular matrix comprises the following steps: taking extracellular matrix, adding phosphate buffer solution, oscillating, carrying out hydration reaction for 1-2h at 4-8 ℃, adding nanocellulose crystal, carrying out water bath reaction for 1-2h at 50-60 ℃, and cooling to obtain glycosylated extracellular matrix;
s6, adding the freeze-dried liquid into mask cloth, and performing vacuum freeze drying to obtain the freeze-dried powder essence mask for triple skin barrier repair.
2. The preparation method of the freeze-dried powder essence mask for triple skin barrier repair according to claim 1 is characterized in that the mass ratio of the extracellular matrix, the phosphate buffer solution and the nanocellulose crystal is 1:3-4:0.08-0.1; the extracellular matrix is taken from adipose tissue of a mammal.
3. The preparation method of the freeze-dried powder essence mask for triple skin barrier repair according to claim 1 is characterized in that the freeze-dried protectant a and the freeze-dried protectant b consist of 20-28 parts of glycosylated extracellular matrix, 12-16 parts of sodium dodecyl sulfate, 9-14 parts of amino acid and 4-7 parts of polyethylene glycol according to parts by weight; the amino acid is at least one of proline, L-tryptophan, sarcosine, L-tyrosine, phenylalanine and arginine.
4. The preparation method of the freeze-dried powder essence mask for triple skin barrier repair according to claim 1, wherein the addition amount of the freeze-dried protective agent a is 1-3% of the weight of the dispersion emulsion; the addition amount of the freeze-drying protective agent b is 3-5% of the weight of the emulsified condensate.
5. The method for preparing a freeze-dried powder essence mask for triple skin barrier repair according to claim 1, wherein the semi-fluid gel is added while homogenizing at 10-20MPa and 3000-5000 r/min; and adding the semi-fluid gel liquid every 30-60s for 5 times.
6. A freeze-dried powder essence mask for triple skin repair, which is obtained by adopting the preparation method of the freeze-dried powder essence mask for triple skin repair according to any one of claims 1-5, and is characterized by comprising, by weight, 8-12 parts of mussel extract, 4-7 parts of palmitoyl tripeptide-8, 3-6 parts of beta-glucan, 6-9 parts of tremella fruit body extract, 6-9 parts of centella asiatica leaf extract, 7-10 parts of 4-tert-butylcyclohexanol, 4-9 parts of squalane, 4-6 parts of jojoba seed oil, 8-15 parts of polyglycerol-10 oleate, 10-14 parts of hydroxyethyl urea, 12-19 parts of sodium hyaluronate, 6-8 parts of acrylic acid (ester) copolymer sodium, 3-4 parts of butanediol, 6-8 parts of polyglycerol-2 oleate, 3-5 parts of lecithin, 5-9 parts of 1, 2-pentanediol, 10-17 parts of glycerol and 30-50 parts of water.
7. The lyophilized powder essence mask for triple skin barrier repair according to claim 6, wherein the composition comprises, by weight, 10 parts of mussel extract, 5 parts of palmitoyl tripeptide-8, 4 parts of beta-glucan, 7 parts of tremella fruit body extract, 8 parts of centella asiatica leaf extract, 8 parts of 4-tert-butylcyclohexanol, 6 parts of squalane, 5 parts of jojoba seed oil, 12 parts of polyglycerol-10 oleate, 12 parts of hydroxyethyl urea, 15 parts of sodium hyaluronate, 7 parts of sodium (ester) acrylic copolymer, 3 parts of butanediol, 7 parts of polyglycerol-2 oleate, 4 parts of lecithin, 7 parts of 1, 2-pentanediol, 13 parts of glycerol and 40 parts of water.
8. Use of the lyophilized powder essence mask for triple skin barrier repair according to claim 6 in the preparation of medicines for improving skin inflammation, allergy and pruritus.
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