CN112675096B - Bacteriostatic and bactericidal plant composite composition and preparation method thereof - Google Patents
Bacteriostatic and bactericidal plant composite composition and preparation method thereof Download PDFInfo
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Abstract
The application relates to the field of skin care products, and particularly discloses an antibacterial and bactericidal plant composite composition and a preparation method thereof; the bacteriostatic and bactericidal plant composite composition is prepared from the following raw materials in parts by weight: extracting herba Solidaginis, scutellariae radix, folium Perillae, herba Rosmarini officinalis, flos Lonicerae, coptidis rhizoma and folium Artemisiae Argyi; the preparation method comprises the following steps: weighing and mixing the solidago virgaurea extract and the scutellaria baicalensis extract to obtain a mixed solution, preparing the mixed solution into dry powder, putting the dry powder into chitosan membrane solution, mixing and stirring, adding glutaraldehyde, standing, drying in vacuum and crushing to obtain coated dry powder; weighing perilla leaf extract, rosemary extract, honeysuckle extract, coptis extract and folium artemisiae argyi extract, mixing and preparing a stirring solution; mixing the modified bacterial cellulose, the coated dry powder, the stirring liquid, glycerol and water to obtain a finished composite composition; the surface layer of the skin has good antibacterial and bacteriostatic effects.
Description
Technical Field
The application relates to the field of skin care products, in particular to a bacteriostatic and bactericidal plant composite composition and a preparation method thereof.
Background
The skin care product acts on the face in a smearing mode, can enable the face to be ruddy in color, and has the effects of replenishing water, preserving moisture and repairing; however, because the face of people is often exposed to the external environment, bacteria and microorganisms in the environment are easily attached to the surface of the skin, and the bacteria on the surface of the skin easily cause skin infection and allergy, and even suppuration and pathological changes, the antibacterial and bacteriostatic properties of the skin care product are deeply concerned by people.
The antibacterial and bacteriostatic properties of the existing skin care products are mainly the functions of active ingredients of antibacterial substances added in the skin care products, but for sensitive skin, the strong antibacterial activity of the antibacterial substances easily affects the sensitive skin.
Disclosure of Invention
In order to enable the skin surface layer to have good antibacterial and bacteriostatic effects, the application provides an antibacterial and bactericidal plant composite composition and a preparation method thereof.
In a first aspect, the application provides an antibacterial and bactericidal plant composite composition, which adopts the following technical scheme: the bacteriostatic and bactericidal plant composite composition is prepared from the following raw materials in parts by weight: 32-45 parts of solidago virgaurea extract, 24-36 parts of scutellaria baicalensis extract, 10-15 parts of perilla leaf extract, 6-14 parts of rosemary extract, 6-15 parts of honeysuckle extract, 5-10 parts of coptis chinensis extract and 4-8 parts of folium artemisiae argyi extract.
By adopting the technical scheme, the antibacterial and bactericidal plant composite composition has good antibacterial and bacteriostatic effects by matching the solidago virgaurea, the scutellaria baicalensis and the perilla leaves; the folium artemisiae argyi, the honeysuckle and the scutellaria baicalensis are matched, so that the antibacterial and bactericidal plant composite composition has a good relieving effect, and the irritation influence of stronger antibacterial and bactericidal activity components in solidago virgaurea, the scutellaria baicalensis, the perilla leaves and the folium artemisiae argyi on skin can be relieved; the perilla leaf and the coptis are matched, so that the synthesis of skin collagen can be promoted, and a skin protection barrier is formed; the rosemary, the perilla leaf and the honeysuckle are matched, so that the antibacterial plant composite composition has good smell; the antibacterial and bactericidal plant composite composition is prepared by matching solidago virgaurea, scutellaria baicalensis, perilla leaves, rosemary, honeysuckle, coptis chinensis and folium artemisiae argyi, has good antibacterial and bacteriostatic effects and also has good calming and relieving effects, so that people with sensitive skin cannot generate irritation influence on skin when using the antibacterial and bactericidal plant composite composition.
Preferably, the solidago virgaurea extracting solution is prepared by the following method:
weighing 9-11 parts of all-grass-leaved yellowhorn, drying, crushing, degreasing, adding 90-120 parts of 92-97% ethanol by mass, performing reflux extraction for 1-3h, and taking filtrate to prepare an initial extract;
mixing the filter residues of the first step with 100-120 parts of 95-97% by mass of ethanol, performing reflux extraction for 2-4 hours, taking the filtrate as a re-extraction solution, mixing the re-extraction solution with the primary extraction solution prepared by the first step, and concentrating for 5-10 hours to prepare the solidago virgaurea extract.
By adopting the technical scheme, through primary extraction and secondary extraction, a large amount of flavonoid substances in the solidago virgaurea are extracted, the extraction efficiency is improved, the flavonoid substance content in the bacteriostatic and bactericidal plant composite composition is improved, and the bactericidal and bacteriostatic effects of the finished product composition are improved.
Preferably, the temperature is limited to 60-75 ℃ during the first reflux extraction, and 92-97% of ethanol in mass fraction is continuously supplemented during the first reflux extraction so that the total amount of ethanol is not changed.
By adopting the technical scheme, the ethanol can be accelerated to permeate into the solidago virgaurea by limiting the extraction temperature, so that the extraction efficiency is improved, the extraction rate of flavonoid substances in the solidago virgaurea is improved, and the finished product composition has good sterilization and bacteriostasis effects.
In a second aspect, the application provides a preparation method of the bacteriostatic and bactericidal plant composite composition, which adopts the following technical scheme:
a preparation method of a bacteriostatic and bactericidal plant composite composition comprises the following steps:
s1, weighing a solidago virgaurea extract and a scutellaria baicalensis extract, mixing to prepare a mixed solution, performing spray drying on 20-35 parts of the mixed solution to prepare dry powder, putting the dry powder into 75-85 parts of chitosan membrane solution, mixing and stirring for 35-45min, adding 3-8 parts of glutaraldehyde within 60S, standing for 2-4h, performing vacuum drying, and crushing to prepare coated dry powder;
s2, weighing perilla leaf extract, rosemary extract, honeysuckle extract, coptis extract and folium artemisiae argyi extract, mixing and preparing a stirring solution;
s3, weighing 3-8 parts of modified bacterial cellulose, 2-5 parts of coating dry powder prepared by S1, 12-18 parts of stirring liquid prepared by S2, 10-20 parts of glycerol and 5-10 parts of water, and mixing to obtain a finished product of the composite composition.
By adopting the technical scheme, when the skin care product is used at night, because the skin is in a deep breathing state at night, the antibacterial and bacteriostatic active ingredient micromolecules easily enter the inside of the skin, and the antibacterial and bacteriostatic effects of the skin surface layer are deteriorated, so that the resistance effect of sensitive skin on bacteria and fungi is influenced.
The chitosan coated dry powder is matched with the modified bacterial cellulose, so that when the composite composition is applied to a skin care product, the chitosan coated dry powder can be attached to the surface of a composite bracket structure of the modified bacterial cellulose, active ingredients in the chitosan coated dry powder can be slowly released and can be stably attached to the surface layer of the skin, when the skin is in a deep breathing state, antibacterial and bacteriostatic active small molecules cannot enter the inside of the skin and can be stopped on the surface layer of the skin, and the surface layer of the sensitive skin has a good antibacterial and bacteriostatic effect.
The active ingredients in the solidago virgaurea extract and the scutellaria baicalensis extract are mainly flavonoids, the flavonoids are prepared into dry powder, and the dry powder is soaked in chitosan membrane liquid and matched with the cross-linking effect of glutaraldehyde, so that chitosan membrane liquid is coated on the surface of the dry powder; the bacterial cellulose has a good water absorption effect, the relatively strong hydrophilicity of chitosan is utilized, the bonding effect of glycerol is matched, the coated dry powder particles can be stably attached to the surface of the modified bacterial cellulose composite bracket structure, the modified bacterial cellulose composite bracket structure cannot move along with the breathing of skin, and the modified bacterial cellulose, the coated dry powder and the glycerol are matched, so that the coated dry powder is stably attached to the surface layer of the skin.
Preferably, the modified bacterial cellulose in S3, the coated dry powder prepared in S1 and glycerol are stirred for 3-8min at the rotating speed of 100-130r/min, then the stirring liquid prepared in S2 is added within 30S, and the mixture is stirred for 10-20min at 350-450r/min, so that a finished product of the composite composition is prepared.
By adopting the technical scheme, the stirring speed of the mixed modified bacterial cellulose, the coated dry powder and the glycerol is limited, so that the glycerol can adhere the coated dry powder to the modified bacterial cellulose composite bracket structure, and the phenomenon that the composite bracket structure of the modified bacterial cellulose is damaged due to the overhigh stirring speed to influence the adhesion effect of the coated dry powder is avoided; and the stirring liquid is limited to be added within 30s, and the modified bacterial cellulose is uniformly dispersed in the stirring liquid by slowly adding the stirring liquid to be mixed with the modified bacterial fiber and the coating dry powder, so that the finished product of the composite composition has good antibacterial and bacteriostatic properties.
Preferably, the modified bacterial cellulose in S3 is prepared by the following method:
s31, weighing 1-2 parts of bacterial cellulose and 8-15 parts of water, mixing and stirring to obtain a bacterial cellulose suspension, adding 0.3-0.7 part of gelatin, and heating and dissolving at 35-45 ℃ to obtain a mixed solution;
and S32, pre-freezing and freezing the mixed solution prepared in the step S31 to prepare a semi-finished product, soaking the semi-finished product in the cross-linking solution for 4-8h, taking out the semi-finished product, washing the semi-finished product for 2-4 times, and pre-freezing and freeze-drying the semi-finished product to prepare the modified bacterial cellulose.
Through adopting above-mentioned technical scheme, the composite support structure that bacterial cellulose and gelatin cooperate and prepare, it utilizes its micron order porous structure to cooperate bacterial cellulose nanometer porous to use gelatin as the base member, thereby form stable in structure's composite support structure, composite support structure has good hydroscopicity, and composite support structure has great specific surface area, thereby make chitosan coating dry powder can a large amount of attached to composite support structure surface, not only play good antibiotic antibacterial effect, can also avoid skin respiration in-process, antibiotic antibacterial active ingredient in the dry powder gets into inside the skin, influence sensitive skin top layer to the bacterium, the resistant effect of fungi.
Preferably, 0.3-0.7 part of gelatin is added while the S31 bacterial cellulose is subjected to ultrasonic dispersion.
By adopting the technical scheme, the composite bracket structure of the modified bacterial cellulose is prevented from being damaged by limiting the stirring speed of the composite bracket structure, and the composite bracket structure can be maintained under the condition of low-speed stirring, so that the composite bracket structure is more stable, and the coated dry powder is more stably attached to the surface of the composite bracket structure of the modified bacterial cellulose.
Preferably, the chitosan membrane liquid in S1 is prepared by the following method:
taking 60-70 parts of chitosan solution with mass fraction of 2%, adding 5-10 parts of glycerol and 3-5 parts of span 80, mixing and stirring for 30-45min, and then carrying out vacuum defoaming for 2-5min to obtain the chitosan membrane solution.
By adopting the technical scheme, the chitosan solution is matched with the glycerol, so that the chitosan film has good plasticity, the mechanical property of the chitosan film is improved, and the chitosan film is prevented from being broken in the coating process.
In summary, the present application has the following beneficial effects:
1. the antibacterial and bactericidal plant composite composition prepared by matching the solidago virgaurea, the scutellaria baicalensis, the perilla leaf, the rosemary, the honeysuckle, the coptis chinensis and the folium artemisiae argyi has good antibacterial and bacteriostatic effects and also has good calming and relieving effects, so that people with sensitive skin can not irritate the skin when using the antibacterial and bactericidal plant composite composition.
2. The bacterial cellulose, the coated dry powder, the folium artemisiae argyi extract and the perilla leaf extract are matched, so that the antibacterial effect of the composite composition is enhanced, and the influence of bacteria and microorganisms in the external environment on the surface layer of sensitive skin can be better isolated.
3. The chitosan coated dry powder has a slow release effect, the dry powder is released into the composite composition liquid, the flavonoid substances are slowly released, when the composite composition is added into a skin care product, the skin care product can keep the antibacterial and bacteriostatic activity of the skin care product for a long time, the chitosan coated dry powder not only acts on the surface of the skin and has the long-acting antibacterial and bacteriostatic effect, but also can prolong the storage time of the antibacterial and bacteriostatic active ingredients of the skin care product, so that the skin care product still has good antibacterial and bacteriostatic effects after being used for a period of time.
4. Modified bacterial cellulose is prepared in a freeze drying mode, so that the modified bacterial cellulose can be dehydrated more thoroughly, and meanwhile, the modified bacterial cellulose has a better rehydration effect, when the modified bacterial cellulose is contacted with water molecules, water can be absorbed quickly, and partial water-soluble active ingredients are firmly locked on the surface of a composite bracket structure of the modified bacterial cellulose, so that the antibacterial and bacteriostatic active ingredients in the composite composition are locked, and the water-soluble antibacterial and bacteriostatic active ingredients are prevented from entering skin cells along with water when skin breathes and affecting the skin.
Detailed Description
The present application is further described in detail in connection with the following examples.
Preparation example of Solidago hirsuta extract
The raw material Solidago virgaurea is bought in a Solidago virgaurea sheet shape produced by the Chang-Fu national drug Co., ltd in Bozhou city; other raw materials and equipment are all sold in the market.
Preparation example 1: the solidago virgaurea extract is prepared by the following method:
weighing 10kg of all-grass-fruit yellowtop, drying and then crushing to obtain particle sizes of 2-6mm, degreasing, adding 100kg of ethanol with the mass fraction of 95%, performing reflux extraction for 2h at 70 ℃, continuously supplementing the ethanol with the mass fraction of 95% in the process, ensuring that the total amount of the ethanol is 100kg, and taking filtrate to prepare an initial extract;
mixing the filter residues of the mao fruit and 110kg of ethanol with the mass fraction of 96%, performing reflux extraction for 3 hours, taking filtrate as a re-extraction solution, mixing the re-extraction solution with the initial extraction solution prepared in the process of the mao fruit and goldenrod flower extraction solution, and concentrating for 8 hours to prepare the mao fruit and goldenrod flower extraction solution.
Preparation example 2: the solidago virgaurea extract is prepared by the following method:
the method comprises the steps of weighing 9kg of all-grass-fruit goldenrod herb, drying and then crushing the all-grass-fruit goldenrod herb into particles with the particle size of 2-6mm, adding 90kg of 92% by mass ethanol into the all-grass-fruit goldenrod herb after degreasing, performing reflux extraction for 1h at the temperature of 60 ℃, continuously supplementing 92% by mass ethanol into the all-grass-fruit goldenrod herb during the reflux extraction, ensuring that the total amount of the ethanol is 90kg, and taking filtrate to prepare primary extract;
mixing the filter residues of the first step with 100kg of 95% ethanol in mass fraction, performing reflux extraction for 2 hours, taking filtrate as re-extraction liquid, mixing the re-extraction liquid with the prepared primary extraction liquid, and concentrating for 5 hours to obtain the solidago virgaurea extract.
Preparation example 3: the solidago virgaurea extract is prepared by the following method:
firstly, weighing 11kg of all-grass-fruit goldenrod herb, drying and crushing the all-grass-fruit goldenrod herb into particles with the particle size of 2-6mm, degreasing, adding 120kg of 97% ethanol, performing reflux extraction for 3 hours at 75 ℃, continuously supplementing 97% ethanol in the process, ensuring the total amount of the ethanol to be 120kg, and taking filtrate to prepare primary extract;
mixing the filter residues of the first step with 120kg of 97% ethanol in mass fraction, performing reflux extraction for 4 hours, taking filtrate as re-extraction liquid, mixing the re-extraction liquid with the primary extraction liquid prepared, and concentrating for 10 hours to obtain the solidago virgaurea extract.
Preparation example of bacterial cellulose
The yeast in the raw materials of the following preparation examples was purchased from Ningbo boat Biotechnology Co., ltd, acetobacter xylinum was purchased from Goodel chemical Co., ltd, and other raw materials were all generally commercially available.
Preparation example 4: the bacterial cellulose is prepared by the following method:
(1) weighing 120kg of coconut juice, inoculating 0.4kg of yeast, fermenting at 28 ℃ for 26 hours, sterilizing at 121 ℃ for 20min to obtain a yeast culture solution, inoculating 8kg of acetobacter xylinum into the yeast culture solution, performing aeration culture for 18 hours, standing and culturing for 5.5 days, taking out suspended substances on the surface of the culture solution, and obtaining bacterial cellulose.
Preparation example 5: the bacterial cellulose is prepared by the following method:
(1) weighing 110kg of coconut juice, inoculating 0.4kg of yeast, fermenting at 28 ℃ for 26 hours, sterilizing at 121 ℃ for 20min to obtain a yeast culture solution, inoculating 8kg of acetobacter xylinum into the yeast culture solution, performing aeration culture for 18 hours, standing and culturing for 5.5 days, taking out suspended substances on the surface of the culture solution, and obtaining bacterial cellulose.
Preparation example 6: the bacterial cellulose is prepared by the following method:
(1) weighing 130kg of coconut juice, inoculating 0.4kg of yeast, fermenting at 28 ℃ for 26 hours, sterilizing at 121 ℃ for 20min to obtain a yeast culture solution, inoculating 8kg of acetobacter xylinum into the yeast culture solution, performing aeration culture for 18 hours, standing and culturing for 5.5 days, taking out suspended substances on the surface of the culture solution, and obtaining bacterial cellulose.
Preparation example of modified bacterial cellulose
The gelatin in the following raw materials is purchased from food-grade gelatin produced by Zhengzhou Wangbao chemical products Limited company, and has the freezing power of 160; other raw materials and equipment are all sold in the market.
Preparation example 7: the modified bacterial cellulose is prepared by the following method:
s31, weighing 1.6kg of the bacterial cellulose prepared in the preparation example 4, mixing and stirring 12kg of water to prepare a bacterial cellulose suspension, adding 0.5kg of gelatin while performing ultrasonic dispersion on the suspension at 35kHz, and stirring at the rotating speed of 650r/min for 12min at 40 ℃ to prepare a mixed solution;
s32, pre-freezing the mixed solution prepared in the step S31 for 24 hours at the temperature of minus 25 ℃, and then freezing for 48 hours at the temperature of minus 40 ℃ to prepare a semi-finished product;
s33, weighing 5kg of 0.15mol/L anhydrous citric acid and 10kg of 0.25mol/L trisodium citrate, mixing, and performing ultrasonic dispersion for 5min under the condition of 25kHz to prepare a cross-linking liquid;
and S34, soaking the semi-finished product prepared in the S32 in the cross-linking liquid prepared in the S33 for 6 hours, taking out the semi-finished product, washing with water for 3 times, pre-freezing for 24 hours at the temperature of minus 25 ℃, and then freezing for 48 hours at the temperature of minus 40 ℃ to prepare the modified bacterial cellulose.
Preparation example 8: the modified bacterial cellulose is prepared by the following method:
s31, weighing 1kg of the bacterial cellulose prepared in the preparation example 5, mixing 8kg of water and stirring to obtain a bacterial cellulose suspension, performing ultrasonic dispersion on the suspension under the condition of 20kH0z, adding 0.3kg of gelatin, and stirring at the rotating speed of 650r/min for 12min at the temperature of 35 ℃ to obtain a mixed solution;
s32, pre-freezing the mixed solution prepared in the step S31 for 24 hours at the temperature of 0 ℃, and then freezing for 48 hours at the temperature of-20 ℃ to prepare a semi-finished product;
s33, weighing 5kg of 0.15mol/L anhydrous citric acid and 10kg of 0.25mol/L trisodium citrate, mixing, and performing ultrasonic dispersion for 5min under the condition of 25kHz to prepare a cross-linking liquid;
and S34, soaking the semi-finished product prepared in the step S32 in the cross-linking liquid prepared in the step S33 for 4 hours, taking out the semi-finished product, washing with water for 2 times, pre-freezing for 24 hours at the temperature of 0 ℃, and then freezing for 48 hours at the temperature of-20 ℃ to obtain the modified bacterial cellulose.
Preparation example 9: the modified bacterial cellulose is prepared by the following method:
s31, weighing 2kg of the bacterial cellulose prepared in the preparation example 6, mixing and stirring 15kg of water to prepare a bacterial cellulose suspension, adding 0.7kg of gelatin while performing ultrasonic dispersion on the suspension at 40kHz, and stirring at a rotating speed of 650r/min for 12min at 45 ℃ to prepare a mixed solution;
s32, pre-freezing the mixed solution prepared in the step S31 for 24 hours at the temperature of minus 30 ℃, and then freezing for 48 hours at the temperature of minus 50 ℃ to prepare a semi-finished product;
s33, weighing 5kg0.15mol/L anhydrous citric acid and 10kg0.25mol/L trisodium citrate, mixing, and performing ultrasonic dispersion for 5min at 25kHz to prepare a crosslinking solution;
and S34, soaking the semi-finished product prepared in the S32 in the cross-linking liquid prepared in the S33 for 8 hours, taking out the semi-finished product, washing with water for 4 times, pre-freezing for 24 hours at the temperature of minus 30 ℃, and then freezing for 48 hours at the temperature of minus 50 ℃ to prepare the modified bacterial cellulose.
Preparation example of chitosan membrane solution chitosan in the following raw materials was purchased from zhengzhou jiuting chemical products limited, and the content of active substances was 99%; glycerol was purchased from Yulongxiang biotechnology Limited on Hebei with a content of 99%; other raw materials and equipment are all sold in the market.
Preparation example 10: the chitosan film liquid is prepared by the following method:
weighing 2g of chitosan, placing the chitosan into 100g of acetic acid with the mass fraction of 2%, stirring for 8min at the rotating speed of 500r/min to prepare a chitosan solution with the mass fraction of 2%, taking 66kg of chitosan solution with the mass fraction of 2%, adding 8kg of glycerol, stirring for 5min at the stirring speed of 650r/min, then heating to 60 ℃, adding 4kg of span 80, continuing stirring for 36min, and then carrying out vacuum defoaming for 3.6min to prepare the chitosan membrane solution.
Preparation example 11: the chitosan film liquid is prepared by the following method:
weighing 2g of chitosan, placing the chitosan into 100g of acetic acid with the mass fraction of 2%, stirring for 8min at the rotating speed of 500r/min to prepare a chitosan solution, taking 60kg of chitosan solution with the mass fraction of 2%, adding 5kg of glycerol, stirring for 4min at the stirring speed of 550r/min, then heating to 55 ℃, adding 3kg of span 80, continuing stirring for 30min, and then carrying out vacuum deaeration for 2min to prepare the chitosan membrane solution.
Preparation example 12: the chitosan film liquid is prepared by the following method:
weighing 2g of chitosan, placing the chitosan into 100g of acetic acid with the mass fraction of 2%, stirring for 8min at the rotating speed of 500r/min to prepare a chitosan solution, taking 70kg of the chitosan solution with the mass fraction of 2%, adding 10kg of glycerol, stirring for 7min at the stirring speed of 750r/min, then heating to 65 ℃, adding 5kg of span 80, continuing stirring for 45min, and then carrying out vacuum deaeration for 5min to prepare the chitosan membrane solution.
Examples
The scutellaria baicalensis extracting solution in the following raw materials is purchased from Guangzhou American-exemplary Biotechnology limited company, and the content is 99 percent; glutaraldehyde is purchased from Zhengzhou Youran food ingredient Co., ltd, and the content is 75%; the folium Perillae extractive solution is purchased from Hongxin chemical company, inc. of Guangzhou city, and has a content of 100%; the rosemary extract is purchased from Guangzhou Yongbo chemical industry Co., ltd, and the content is 99 percent; the honeysuckle extract is purchased from Pterocarpus marsupium chemical Co., ltd, guangzhou, with the content of 99%; the coptis chinensis extract is purchased from Shaanxi Kangyun Biotech limited company, and the content is 99 percent; the folium artemisiae argyi extract is purchased from the Bomo chemical industry Co., ltd, guangzhou city, and the content is 99%; other raw materials and equipment are all sold in the market.
Example 1: a preparation method of a bacteriostatic and bactericidal plant composite composition comprises the following steps:
s1, weighing 40kg of solidago virgaurea extract prepared in preparation example 1 and 30kg of scutellaria baicalensis extract, stirring for 5min at the rotating speed of 650r/min to prepare a mixed solution, taking 28kg of the mixed solution, performing spray drying to prepare a dry powder, placing the dry powder in 80kg of chitosan membrane solution prepared in preparation example 10, stirring for 40min at the rotating speed of 840r/min, then adding 5kg of glutaraldehyde within 60S, standing for 3h, performing vacuum drying, and then crushing to obtain coated dry powder with the particle size of 5-10 mu m;
s2, weighing 12kg of perilla leaf extract, 10kg of rosemary extract, 10kg of honeysuckle extract, 8kg of coptis extract and 6kg of folium artemisiae argyi extract, mixing, and stirring at the rotating speed of 600r/min for 15min to prepare a stirring solution;
s3, weighing 5kg of modified bacterial cellulose prepared in preparation example 7, coating dry powder prepared from 3.5kg of S1, 15kg of glycerol and 8kg of water, mixing, stirring for 5min at the rotating speed of 110r/min, adding stirring liquid prepared from 15kgS2 in 30S, and stirring for 16min at the rotating speed of 410r/min to obtain a finished product of the composite composition.
Example 2: a preparation method of a bacteriostatic and bactericidal plant composite composition comprises the following steps:
s1, weighing 32kg of solidago virgaurea extract prepared in preparation example 2 and 24kg of scutellaria baicalensis extract, stirring for 5min at the rotating speed of 650r/min to prepare a mixed solution, taking 20kg of the mixed solution, performing spray drying to prepare a dry powder, placing the dry powder in 75kg of chitosan membrane solution prepared in preparation example 11, stirring for 35min at the rotating speed of 840r/min, then adding 3kg of glutaraldehyde within 60S, standing for 2h, performing vacuum drying, and then crushing to obtain a coated dry powder with the particle size of 5-10 microns;
s2, weighing 10kg of perilla leaf extract, 6kg of rosemary extract, 6kg of honeysuckle extract, 5kg of coptis extract and 4kg of folium artemisiae argyi extract, mixing, and stirring at the rotating speed of 600r/min for 15min to prepare a stirring solution;
s3, weighing 3kg of the modified bacterial cellulose prepared in the preparation example 8, the coating dry powder prepared from 2kgS, 10kg of glycerol and 5kg of water, mixing, stirring for 3min at the rotating speed of 100r/min, adding the stirring liquid prepared from 12kgS within 30S, and stirring for 10min at the rotating speed of 350r/min to obtain a finished product of the composite composition.
Example 3: a preparation method of a bacteriostatic and bactericidal plant composite composition comprises the following steps:
s1, weighing 45kg of solidago virgaurea extract prepared in preparation example 3 and 36kg of scutellaria baicalensis extract, stirring at a rotation speed of 650r/min for 5min to prepare a mixed solution, taking 35kg of the mixed solution, performing spray drying to prepare a dry powder, placing the dry powder in 85kg of chitosan membrane solution prepared in preparation example 12, stirring at a rotation speed of 840r/min for 45min, then adding 8kg of glutaraldehyde within 60S, standing for 4h, performing vacuum drying, and then crushing to obtain coated dry powder with a particle size of 5-10 microns;
s2, weighing 15kg of perilla leaf extracting solution, 14kg of rosemary extracting solution, 15kg of honeysuckle extracting solution, 10kg of coptis extracting solution and 8kg of folium artemisiae argyi extracting solution, mixing, and stirring at the rotating speed of 600r/min for 15min to prepare a stirring solution;
s3, weighing 8kg of the modified bacterial cellulose prepared in the preparation example 9, the coating dry powder prepared from 5kgS, 20kg of glycerol and 10kg of water, mixing, stirring for 8min at the rotating speed of 130r/min, adding the stirring liquid prepared from 18kgS within 30S, and stirring for 20min at the rotating speed of 450r/min to obtain a finished product of the composite composition.
Comparative example
Comparative example 1: the comparative example differs from example 1 in that: the raw materials are replaced by the perilla leaf extract with the same mass for the solidago virgaurea extract and the scutellaria extract.
Comparative example 2: this comparative example differs from example 1 in that: the honeysuckle extract and the scutellaria extract are replaced by the artemisia leaf extract with the same mass in the raw materials.
Comparative example 3: this comparative example differs from example 1 in that: the raw materials are replaced by the extractive solution of scutellaria baicalensis with the same mass as the extractive solution of artemisia argyi and the extractive solution of honeysuckle.
Comparative example 4: the comparative example differs from example 1 in that: s1, weighing 40kg of the solidago virgaurea extract prepared in preparation example 1, 30kg of the scutellaria baicalensis extract, 12kg of the perilla leaf extract, 10kg of the rosemary extract, 10kg of the honeysuckle extract, 8kg of the coptis chinensis extract and 6kg of the folium artemisiae argyi extract, mixing, and stirring at a rotating speed of 600r/min for 15min to prepare a stirring solution.
Comparative example 5: the comparative example differs from example 1 in that: s3, weighing and mixing the coated dry powder prepared from 3.5kg of S1, 20kg of glycerol and 8kg of water, stirring for 5min at the rotating speed of 110r/min, then adding the stirring liquid prepared from 15kgS2 in 30S, and stirring for 16min at the rotating speed of 410r/min to obtain a finished product of the composite composition.
Comparative example 6: this comparative example differs from example 1 in that: weighing 5kg of the modified bacterial cellulose prepared in preparation example 7 and the coating dry powder prepared from 3.5kg of S1, mixing, stirring at the rotating speed of 110r/min for 5min, then adding the stirring liquid prepared from 15kgS2 within 30s, and stirring at the rotating speed of 410r/min for 16min to obtain a finished composite composition.
Comparative example 7: this comparative example differs from example 1 in that: weighing 5kg of the modified bacterial cellulose prepared in preparation example 7, 3.5kg of the coated dry powder prepared from S1, 15kg of glycerol and 8kg of water, mixing, stirring for 5min at the rotating speed of 350r/min, adding the stirring liquid prepared from 15kgS2 within 30s, and stirring for 16min at the rotating speed of 410r/min to obtain a finished product of the composite composition.
Comparative example 8: the present embodiment is different from embodiment 1 in that: when the modified bacterial cellulose is prepared, gelatin is not added in the raw materials.
Performance test
1. Composite composition sensitivity performance test
Respectively preparing a finished product of the composite composition by adopting the preparation methods of the embodiments 1-3 and the comparative examples 1-8, weighing 4g of the plant composite composition, 6g of glycerol and 0.03g of hyaluronic acid, putting the plant composite composition, the glycerol and the hyaluronic acid into 100g of water, heating to 60 ℃, stirring for 5min at the rotating speed of 450r/min, and cooling to room temperature to obtain finished product essence water; selecting 110 sensitive skin volunteers, averagely dividing into 11 groups, using finished product essence water by 10 persons in each group and 11 groups of volunteers respectively, and after using for 30 days and 60 days, scoring the finished product essence water.
The scoring criteria were as follows: 7-10 minutes, the essence is mild in water and free of stimulation, the skin surface is smooth and fine, and no anaphylaxis symptom occurs; 4-7 minutes, the essence water is mild, the skin surface is smooth, and the local part has allergy symptoms; 0-4 points, essence water irritation, severe skin surface allergy.
2. Composite composition antibacterial property test
The preparation methods of examples 1-3 and comparative examples 1-8 are respectively adopted to prepare finished composite compositions, 4g of the plant composite composition, 8g of glycerol, 0.03g of hyaluronic acid and 2g of propylene glycol are weighed and placed in 90g of water, the temperature is raised to 70 ℃, the mixture is stirred for 5min at the rotating speed of 450r/min, and after the mixture is cooled to the room temperature, the face cream is prepared.
Selecting a strain: staphylococcus aureus ATCC100817 (identified as strain a); staphylococcus epidermidis ATCC12228 (noted as bacterium B);
preparing a culture medium: beef extract medium (staphylococcus aureus and staphylococcus epidermidis): mixing 3g of beef extract, 10g of peptone, 15g of NaCl, 15g of agar, 1000mL of water and pH7.0-7.2, shaking up, heating and stirring on the surface of an electric heating furnace until the culture medium solution boils slightly, keeping the state for 5-10min, placing the mixture into a sterilization pot, sterilizing at 121 ℃ for 20min, and taking out the mixture for later use when the mixture is cooled to 60 ℃;
activating strains: the method comprises the following steps of (1) purchasing a strain as freeze-dried powder filled in an ampoule tube, carrying out aseptic treatment on the top of the ampoule tube, then dropwise adding about 0.1mL of liquid culture medium and the ampoule tube into a liquid transfer gun, shaking up, then picking up the strain by using a strain receiving ring, uniformly inoculating the strain into a corresponding flat plate and a corresponding inclined plane for activation, and placing the strain in a constant-temperature incubator at 37 ℃ for culturing for 24 hours;
preparation of bacterial suspension: taking a plurality of activated strains, and under the aseptic condition, selecting a ring of activated strains, putting the activated strains into 9mL of sterile water, shaking up, and preparing a bacterial suspension;
determination of bacteriostatic efficacy: shaking the culture medium uniformly, pouring the culture medium into flat plates, cooling and solidifying, dripping a certain proportion of bacterial suspension on the flat plates, uniformly coating the surfaces of the flat plates for 3 times by using a coating rod, rotating the flat plates for 60 degrees every time of coating, finally coating the bacterial suspension on the flat plates for a circle by using the coating rod, covering the flat plates, drying the flat plates for 5min at room temperature, lightly placing an oxford cup with the inner diameter of 6mm on the solidified culture medium by using tweezers, and uniformly placing three flat plates; sucking a sample by using a 1mL disposable needle, injecting the sample into an Oxford cup, adding about 400 microliters of sample (the samples are respectively the essence water prepared in examples 1-3 and comparative examples 1-8) into each cup, respectively culturing staphylococcus aureus and staphylococcus epidermidis in an incubator at 37 ℃ for 12 hours, measuring the diameter of a bacteriostatic ring by using a vernier caliper, selecting a bacteriostatic ring mark with uniform and complete aseptic growth when measuring the bacteriostatic ring, and taking the outside of the bacteriostatic ring as a limit for measuring the diameter.
Taking 200g male rats, cutting off the neck of the rat, shaving off the abdominal hair of the rat by using a hair cutter, cutting off the abdominal skin, removing subcutaneous fat layer, blood vessels and residues, cleaning with physiological saline, detecting the integrity of the rat, rinsing with the physiological saline, and freezing and storing in a refrigerator at the temperature of-10 ℃ for later use; the cream is smeared on the surface of a rat cutin layer, the rat cutin layer is stored for 2 hours at 28 ℃ under the condition that the relative humidity is 55%, the residual cream on the rat epidermis is hung, and the antibacterial and bacteriostatic effects of the cream are detected according to the method.
TABLE 1 composite composition Performance test Table
As can be seen by combining examples 1-3 and comparative examples 1-8 and combining table 1, the perilla leaf extract with the same mass is used in the raw material of comparative example 1 to replace the solidago virgaurea extract and the scutellaria baicalensis extract, compared with example 1, the score of the essence water prepared in comparative example 1 is smaller than that of the essence water prepared in example 1 after 30 days and 60 days of use, and the diameters of inhibition rings of the cream bacteria a and the cream bacteria B prepared in comparative example 1 at 0h and 2h are smaller than those of the inhibition rings corresponding to example 1; the matching of the perilla leaf extracting solution, the solidago virgaurea extracting solution and the scutellaria baicalensis extracting solution is proved to ensure that the composite composition has good antibacterial and bacteriostatic properties and can relieve the uncomfortable influence of antibacterial and bacteriostatic small molecules on the surface of sensitive skin.
Compared with the raw materials of the example 1, the evaluation of the essence water prepared in the comparative examples 2 and 3 after the essence water is used for 30 days and 60 days is smaller than that of the essence water prepared in the example 1, and the diameters of inhibition rings of the cream bacteria A and B prepared in the comparative examples 2 and 3 in 0h and 2h are smaller than those of the inhibition rings corresponding to the example 1; the folium artemisiae argyi extract, the honeysuckle extract and the scutellaria baicalensis extract are matched, so that the composite composition has good antibacterial and bacteriostatic properties and a good relieving effect, and discomfort influence of antibacterial and bacteriostatic active ingredients on the surface of sensitive skin can be effectively avoided.
Comparative example 4, the goldenrod lanuginose extract and the scutellaria baicalensis extract are not prepared into chitosan coated dry powder, the raw material of comparative example 5 is replaced by glycerol with equal mass, compared with example 1, the scores of the essence water prepared in comparative examples 4 and 5 are smaller than the score of the essence water prepared in example 1 after the essence water is used for 30 days and 60 days, and the diameters of inhibition rings of cream bacteria A and B prepared in comparative examples 4 and 5 in 0h and 2h are smaller than the diameters of the inhibition rings corresponding to example 1; the chitosan coated dry powder can be matched with the modified bacterial cellulose, so that the coated dry powder is attached to the surface of the composite bracket structure of the modified bacterial cellulose, antibacterial and bacteriostatic active molecules in the coated dry powder are attached to the surface of the skin, and the antibacterial and bacteriostatic effect of the surface of the skin is prevented from being influenced by the fact that the antibacterial and bacteriostatic active molecules enter the inside of the skin under the skin respiration action.
Comparative example 6 raw materials are not added with glycerol and water, compared with example 1, the evaluation of the essence water prepared in comparative example 6 is less than that of the essence water prepared in example 1 after 30 days and 60 days, and the diameters of inhibition rings of cream bacteria A and cream bacteria B prepared in comparative example 6 in 0h and 2h are less than the diameters of the inhibition rings corresponding to example 1; the cooperation of the glycerol, the modified bacterial cellulose and the chitosan coated dry powder is illustrated, so that the chitosan coated dry powder is more stably attached to the surface of the modified bacterial cellulose composite bracket structure, and antibacterial and bacteriostatic active molecules are attached to the surface of the skin and cannot enter the inside of the skin to influence the antibacterial and bacteriostatic effects of the surface layer of the skin.
Comparative example 7 after mixing the modified bacterial cellulose, the coated dry powder, the glycerol and the water, stirring at a rotating speed of 350r/min, comparing with example 1, after the essence water prepared in comparative example 7 is used for 30 days and 60 days, the scores of the essence water are smaller than those of the essence water prepared in example 1, and the diameters of inhibition rings of the cream bacteria A and the cream bacteria B prepared in comparative example 7 in 0h and 2h are smaller than those of the inhibition rings corresponding to example 1; the higher stirring speed can damage the composite bracket structure of the modified bacterial cellulose, thereby affecting the adhesion effect of the coated dry powder and finally affecting the antibacterial and bacteriostatic effect on the surface of the skin.
Compared with the embodiment 1, the diameters of the bacteriostatic rings of the cream bacteria A and the cream bacteria B prepared in the comparative example 8 in 0h and 2h are smaller than the diameters of the bacteriostatic rings corresponding to the embodiment 1; the stable composite bracket structure can be formed by matching the bacterial cellulose and the gelatin, so that the stable attachment of the antibacterial and bacteriostatic active ingredients on the skin surface is ensured.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (1)
1. The preparation method of the bacteriostatic and bactericidal plant composite composition is characterized by comprising the following steps of:
s1, weighing 40kg of solidago virgaurea extract and 30kg of scutellaria baicalensis extract, stirring for 5min at the rotating speed of 650r/min to prepare a mixed solution, taking 28kg of the mixed solution, performing spray drying to prepare a dry powder, placing the dry powder in 80kg of chitosan membrane solution, stirring for 40min at the rotating speed of 840r/min, then adding 5kg of glutaraldehyde within 60S, standing for 3h, performing vacuum drying, and then crushing to obtain the coated dry powder with the particle size of 5-10 mu m;
s2, weighing 12kg of perilla leaf extract, 10kg of rosemary extract, 10kg of honeysuckle extract, 8kg of coptis extract and 6kg of folium artemisiae argyi extract, mixing, and stirring at the rotating speed of 600r/min for 15min to prepare a stirring solution;
s3, weighing 5kg of modified bacterial cellulose, coating dry powder prepared from 3.5kg of S1, 15kg of glycerol and 8kg of water, mixing, stirring for 5min at the rotating speed of 110r/min, then adding stirring liquid prepared from 15kgS2 in 30S, and stirring for 16min at the rotating speed of 410r/min to obtain a finished product of the composite composition;
the solidago virgaurea extract is prepared by the following method:
weighing 10kg of all-grass-fruit yellowtop, drying and then crushing to obtain particle sizes of 2-6mm, degreasing, adding 100kg of ethanol with the mass fraction of 95%, performing reflux extraction for 2h at 70 ℃, continuously supplementing the ethanol with the mass fraction of 95% in the process, ensuring that the total amount of the ethanol is 100kg, and taking filtrate to prepare an initial extract;
mixing the filter residues of the first step with 110kg of ethanol with the mass fraction of 96%, performing reflux extraction for 3 hours, taking filtrate as re-extraction liquid, mixing the re-extraction liquid with the prepared primary extraction liquid, and concentrating for 8 hours to obtain a solidago virgaurea extract;
the bacterial cellulose is prepared by the following method:
(1) weighing 120kg of coconut juice, inoculating 0.4kg of yeast, fermenting at 28 ℃ for 26 hours, sterilizing at 121 ℃ for 20min to obtain a yeast culture solution, inoculating 8kg of acetobacter xylinum into the yeast culture solution, performing aeration culture for 18 hours, standing and culturing for 5.5 days, and taking out suspended substances on the surface of the culture solution to obtain bacterial cellulose;
the modified bacterial cellulose is prepared by the following method:
s31, weighing 1.6kg of bacterial cellulose and 12kg of water, mixing and stirring to obtain a bacterial cellulose suspension, adding 0.5kg of gelatin while performing ultrasonic dispersion on the suspension at 35kHz, and stirring at the rotating speed of 650r/min for 12min at 40 ℃ to obtain a mixed solution;
s32, pre-freezing the mixed solution prepared in the step S31 for 24 hours at the temperature of minus 25 ℃, and then freezing for 48 hours at the temperature of minus 40 ℃ to prepare a semi-finished product;
s33, weighing 5kg of 0.15mol/L anhydrous citric acid and 10kg of 0.25mol/L trisodium citrate, mixing, and performing ultrasonic dispersion for 5min under the condition of 25kHz to prepare a cross-linking liquid;
s34, placing the semi-finished product prepared in the S32 into the cross-linking liquid prepared in the S33, soaking for 6 hours, taking out, washing with water for 3 times, pre-freezing for 24 hours at the temperature of minus 25 ℃, and then freezing for 48 hours at the temperature of minus 40 ℃ to prepare modified bacterial cellulose;
the chitosan film liquid is prepared by the following method:
weighing 2g of chitosan, placing the chitosan into 100g of acetic acid with the mass fraction of 2%, stirring for 8min at the rotating speed of 500r/min to prepare a chitosan solution with the mass fraction of 2%, taking 66kg of the chitosan solution with the mass fraction of 2%, adding 8kg of glycerol, stirring for 5min at the stirring speed of 650r/min, then heating to 60 ℃, adding 4kg of span 80, continuing stirring for 36min, and then carrying out vacuum deaeration for 3.6min to prepare the chitosan film liquid.
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