CN112516031B - Plant extraction multi-effect composition and preparation method thereof - Google Patents

Plant extraction multi-effect composition and preparation method thereof Download PDF

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CN112516031B
CN112516031B CN202011484911.8A CN202011484911A CN112516031B CN 112516031 B CN112516031 B CN 112516031B CN 202011484911 A CN202011484911 A CN 202011484911A CN 112516031 B CN112516031 B CN 112516031B
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extract
plant
effect composition
composition
effect
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CN112516031A (en
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张军
刘健
张晓琮
孟庆浩
龚明嘉
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Guangzhou Aizhuo Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10General cosmetic use
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
    • A61K2800/522Antioxidants; Radical scavengers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
    • A61K2800/524Preservatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18

Abstract

The invention discloses a plant extraction multi-effect composition and a preparation method thereof, and is characterized in that the composition comprises plant source antibacterial and antioxidant components and a solvent, wherein the plant source antibacterial and antioxidant components are selected from at least three of the following substances: herba Artemisiae Scopariae extract, flos Caryophylli extract, cortex Cinnamomi extract, and semen Sojae Atricolor extract. The plant extraction multi-effect composition can be used in cosmetics and has the advantages of low dosage, safety, effectiveness, naturalness, no stimulation and the like.

Description

Plant extraction multi-effect composition and preparation method thereof
Technical Field
The application belongs to the field of cosmetics, and particularly relates to a plant extraction multi-effect composition and a preparation method thereof.
Background
With the improvement of living standard, cosmetics gradually become an indispensable part of the life of people, and people use cosmetics more and more commonly and pay more and more attention to the safety of the cosmetics. Most cosmetics are rich in nutrients required for the growth of microorganisms, and once microorganisms in the environment enter, the microorganisms can rapidly proliferate, the sense and quality of the product are damaged, and the health of consumers is damaged, so that the inhibition of the proliferation of the microorganisms in the cosmetics is important. Currently, the most common means for inhibiting the proliferation of microorganisms in cosmetics is to add preservatives to cosmetics, and according to the technical safety code of cosmetics (2015 edition), there are 51 types of currently approved preservatives for cosmetics, including phenols, esters, halides, quaternary ammonium salts, and the like, wherein parabens (parabens), isothiazolinones, imidazolidinyl urea, and bronopol are the most commonly used preservatives, but chemical preservatives are liable to cause skin problems, for example: isothiazolinones cause irritative hypersensitivity and bronopol may lead to the formation of carcinogens, and therefore, the type and amount of the isothiazolinones are strictly limited in many countries. Traditional chemical preservatives have not been able to meet the needs of people, and research on alternative products is receiving more and more attention.
The Chinese patent publication No. CN105213250A uses vine tea extract, natural perfume and the mixed solution of propylene glycol and water to compound natural antibacterial agent, has broad-spectrum and high-efficiency antibacterial effect on common bacteria in cosmetics, and can reduce irritation of the product and improve safety of the product. CN103767884B discloses a plant preservative composition consisting of veratryl alcohol, a synergistic agent and a solvent, which has a synergistic antibacterial effect and can reduce the addition of veratryl alcohol. Although the existing plant extract preservative has a plurality of advantages, the obvious defects of large preservative dosage, weak bacteriostatic performance, short bacteriostatic aging, single effect and the like still exist.
Disclosure of Invention
The invention aims to provide a plant extraction multi-effect composition, which improves the antibacterial and antioxidant effects by fully exerting the synergistic effect among the components in the composition, achieves the aims of quick sterilization and long-acting bacteriostasis, and has the advantages of wide antibacterial spectrum, low dosage, safety and no stimulation.
The plant extraction multi-effect composition is characterized in that: comprises plant source antibacterial and antioxidant components and solvent. Wherein the plant-derived antibacterial and antioxidant components are selected from at least three of the following substances: herba Artemisiae Scopariae extract, flos Caryophylli extract, cortex Cinnamomi extract, and semen Sojae Atricolor extract.
The plant source antibacterial and antioxidant component comprises the following components in percentage by mass: 0.5-30% of artemisia capillaris extract, 0.5-50% of flos caryophyllata extract, 1-40% of cinnamon extract and 1-40% of black soybean extract, wherein the mass percentage is expressed by the mass of each component relative to the total mass of the plant extraction multi-effect composition.
The plant source antibacterial and antioxidant component is selected from: 0.5-30% of artemisia capillaris extract, 0.5-30% of flos caryophyllata extract and 1-40% of cinnamon extract.
The plant source antibacterial and antioxidant component is selected from: 0.5-30% of artemisia capillaris extract, 0.5-30% of flos caryophyllata extract and 1-40% of black soybean extract.
The plant source antibacterial and antioxidant component is selected from: 0.5-30% of flos caryophyllata extract, 1-40% of cinnamon extract and 1-40% of black soybean extract.
The plant source antibacterial and antioxidant component is selected from: 0.5-30% of artemisia capillaris extract, 1-40% of cinnamon extract and 1-40% of black soybean extract.
The plant source antibacterial and antioxidant component is selected from: 0.5-30% of artemisia capillaris extract, 0.5-30% of flos caryophyllata extract, 1-40% of cinnamon extract and 1-40% of black soybean extract.
The solvent is selected from one or more than one of 1, 2-propylene glycol, 1, 3-propylene glycol, 1, 2-butylene glycol, 1, 3-butylene glycol, 1, 4-butylene glycol, 1, 2-pentanediol, 1, 5-pentanediol, isoprene glycol, 1, 2-hexanediol, 1, 6-hexanediol, methoxybutanol, ethanol, menthol, ethyl acetate, laurocapram, polyvinylpyrrolidone, water, glycerol, methyl propylene glycol and ethyl hexyl glycerol.
Preferably, the plant-derived antibacterial and antioxidant component comprises the following components in percentage by mass: 20% of artemisia capillaris extract, 15% of flos caryophyllata extract and 15% of cinnamon extract.
Preferably, the plant-derived antibacterial and antioxidant component comprises the following components in percentage by mass: 20% of artemisia capillaris extract, 15% of flos caryophyllata extract and 15% of black soybean extract.
Preferably, the plant-derived antibacterial and antioxidant component comprises the following components in percentage by mass: 15% of flos caryophyllata extract, 20% of cinnamon extract and 15% of black soybean extract.
Preferably, the plant-derived antibacterial and antioxidant ingredient is selected from: 20% of artemisia capillaris, 15% of cinnamon and 15% of black soybean.
Preferably, the plant-derived antibacterial and antioxidant component comprises the following components in percentage by mass: 15% of artemisia capillaris extract, 10% of flos caryophyllata extract, 15% of cinnamon extract and 10% of black soybean extract.
The plant extract multi-effect composition of the present invention can be prepared by the conventional methods in the field: adding plant-derived antibacterial and antioxidant components and solvent into container, stirring, heating to 40-60 deg.C, stirring to dissolve completely, cooling to room temperature, filtering, and packaging.
The plant extraction multi-effect composition can be used in cosmetics. The cosmetic comprises: facial mask liquid, lotion, cream, toner, essence, stock solution, face cleanser, lotion, perfume, makeup remover, foundation solution, foundation cream, concealer, rouge, lipstick, eye shadow, blush, etc.
Further, the plant extraction multi-effect composition is added into the mask liquid in a mass percentage of 0.1-5%, preferably 0.5-2%.
Furthermore, the plant extraction multi-effect composition is added into the emulsion in a mass percentage of 0.1-5%, preferably 0.5-2%.
Furthermore, the plant extraction multi-effect composition is added into the cream in a mass percentage of 0.1-5%, preferably 0.5-2%.
Furthermore, the plant extraction multi-effect composition is added into the toner in a mass percentage of 0.1-5%, preferably 0.5-2%.
Furthermore, the plant extraction multi-effect composition is added into the cleansing milk in a mass percentage of 0.1-5%, preferably 0.5-2%.
Compared with the prior art, the method has the following beneficial effects:
1. the plant extraction multi-effect composition provided by the invention has the advantages that each component is a common plant extract, can replace the traditional chemical preservative, and is safe and non-irritant.
2. The plant extraction multi-effect composition provided by the invention has a synergistic interaction effect among the components, can improve the antibacterial and antioxidant effects, has a wide antibacterial spectrum, takes effect quickly, has a long antibacterial effect, and can clear DPPH free radicals.
3. The plant extraction multi-effect composition provided by the invention can achieve the effects of high-efficiency bacteriostasis and antioxidation under a lower dosage.
Detailed Description
The present invention is further illustrated with reference to the following examples, which are not intended to limit the invention in any way.
Example 1
The clove extraction process comprises the following steps:
210kg of flos caryophylli is taken and crushed by a traditional Chinese medicine crusher, and is sieved by a 50-mesh sieve to obtain fine powder. Taking 200kg of flos Caryophylli powder, adding 5-10 times of distilled water, adding corresponding volume of sodium chloride solution, rapidly stirring, simultaneously using high-power dual-frequency ultrasonic device (25kHz and 40kHz), ultrasonically extracting for 2h, transferring into steam distillation device, rapidly heating with high power, reducing heating power after steam is generated, and continuously extracting for 4 h. After extraction, the oily extract of the flos caryophyllata is separated by an oil-water separator, and a small amount of anhydrous sodium sulfate is added for dehydration and then is stored at low temperature in a dark place.
Example 2
The cinnamon extraction process comprises the following steps:
taking 55kg of cinnamon bark, crushing by using a traditional Chinese medicine crusher, and sieving by using a 50-mesh sieve to obtain cinnamon bark powder. Taking 50kg of sieved cortex Cinnamomi powder, adding 5-15 times of distilled water, soaking for 18-24h, putting into a steam distillation device, rapidly heating at high power, reducing heating power after steam is generated, and continuously extracting for 4 h. Extracting the distillate with 50L diethyl ether twice, mixing the two extracted diethyl ether layers, adding small amount of anhydrous sodium sulfate, drying, heating for 20min, and steaming to remove diethyl ether to obtain oily extract of cortex Cinnamomi.
Example 3
The extraction process of the artemisia capillaris comprises the following steps:
160kg of dried artemisia capillaris are taken, crushed by a traditional Chinese medicine crusher and sieved by a 30-mesh sieve for later use. Taking 150kg of sieved herba Artemisiae Scopariae powder, mixing the powder with extractive solution (water: ethanol: butanediol: 1:8:1)1:10, stirring, and extracting for 2-3 hr at 65-70 deg.C. After leaching, the extraction mixture is transferred to ultrasonic extraction equipment, and is subjected to ultrasonic extraction for 2 hours by a high-power double-frequency ultrasonic device (25kHz and 40 kHz). After extraction, filtering by plate pressure to remove insoluble substances, adding activated carbon with the mass of 3% of the filtrate into the residual filtrate, keeping the temperature at 45-50 ℃, stirring for 30min, and then filtering by plate pressure to remove the activated carbon. Adding activated carbon with the mass of 2% of the filtrate into the residual filtrate again for secondary decolorization, keeping the temperature at 45-50 ℃, stirring for 30min, and then filtering under plate pressure to remove the activated carbon. After the treatment, nearly colorless artemisia capillaris extraction liquid can be obtained, nanofiltration is carried out on the extraction liquid to remove impurities, water and ethanol are removed under the environment of not higher than 60 ℃, and the artemisia capillaris-butanediol extraction liquid is further ultrafiltered, purified and refined to obtain the artemisia capillaris extract required by the plant extraction multi-effect composition.
Example 4
The extraction process of the black soybean comprises the following steps:
pulverizing 55kg semen Sojae Atricolor with traditional Chinese medicine pulverizer, and sieving with 50 mesh sieve. Taking 50kg of sieved semen Sojae Atricolor powder, mixing the powder with extractive solution (water: ethanol: butanediol: 3:6:1)1:10, stirring, and extracting for 4-6 hr at 45-50 deg.C. After leaching, the pH value of the extraction mixture is adjusted to 4.5, and then the extraction mixture is transferred to ultrasonic extraction equipment, and is subjected to ultrasonic extraction for 2 hours by a high-power double-frequency ultrasonic device (25kHz and 40 kHz). And after extraction, removing bean dregs and insoluble substances by plate pressure filtration, adding activated carbon accounting for 2% of the mass of the filtrate into the residual filtrate, preserving the heat at 45-50 ℃, stirring for 30min, and then removing the activated carbon by plate pressure filtration. Adding activated carbon with the mass of 2% of the filtrate into the residual filtrate again for secondary decolorization, keeping the temperature at 45-50 ℃, stirring for 30min, and then filtering under plate pressure to remove the activated carbon. After the treatment, nearly colorless black soybean extract liquid can be obtained, nanofiltration is carried out on the extract liquid to remove impurities, water and ethanol are removed under the environment of not higher than 55 ℃, and the residual black soybean-butanediol extract liquid is further ultrafiltered, purified and refined to obtain the black soybean extract required by the plant extraction multi-effect composition.
Example 5
And (3) in a 250mL flask with a thermometer and a stirrer, adding 50g of glycerin into the above extracts, namely 20g of artemisia capillaries extract, 15g of flos caryophyllata extract and 15g of cinnamon extract, heating to 40 ℃, stirring for 50min until the extracts are basically completely dissolved, cooling to room temperature, and filtering to remove insoluble impurities to obtain the plant extraction multi-effect composition.
Example 6
And (3) in a 250mL flask with a thermometer and a stirrer, adding 20g of artemisia capillaries extract, 15g of flos caryophyllata extract and 15g of black soybean extract into 50g of glycerol, heating to 40 ℃, stirring for 50min until the extracts are basically completely dissolved, cooling to room temperature, and filtering to remove insoluble impurities to obtain the plant extraction multi-effect composition.
Example 7
And (2) in a 250mL flask with a thermometer and a stirrer, adding 50g of glycerin into the extracts, namely 15g of flos caryophyllata extract, 20g of cinnamon extract and 15g of black soybean extract, heating to 40 ℃, stirring for 50min until the mixture is basically completely dissolved, cooling to room temperature, and filtering to remove insoluble impurities to obtain the plant extraction multi-effect composition.
Example 8
And (2) in a 250mL flask with a thermometer and a stirrer, extracting 20g of the extracts, namely artemisia capillaris, 15g of cinnamon extract and 15g of black soybean extract, adding 50g of glycerol, heating to 40 ℃, stirring for 50min until the extracts are basically completely dissolved, cooling to room temperature, and filtering to remove insoluble impurities to obtain the plant extraction multi-effect composition.
Example 9
And (2) adding 50g of glycerin into the extracts, namely 15g of artemisia capillaries extract, 10g of flos caryophylli extract, 15g of cinnamon extract and 10g of black soybean extract in a 250mL flask with a thermometer and a stirrer, heating to 40 ℃, stirring for 50min until the extracts are basically completely dissolved, cooling to room temperature, and filtering to remove insoluble impurities to obtain the plant extraction multi-effect composition.
Comparative example 1
Adding 50g flos Caryophylli extract and 50g glycerol into a 250mL flask equipped with thermometer and stirrer, heating to 40 deg.C, stirring for 50min to dissolve, cooling to room temperature, and filtering to remove insoluble impurities to obtain single component composition.
Comparative example 2
Adding 50g of herba Artemisiae Scopariae extract and 50g of glycerol into a 250mL flask equipped with a thermometer and a stirrer, heating to 40 deg.C, stirring for 50min until all the components are dissolved, cooling to room temperature, and filtering to remove insoluble impurities to obtain single component composition.
Comparative example 3
Adding 50g of cortex Cinnamomi extract and 50g of glycerol into a 250mL flask equipped with a thermometer and a stirrer, heating to 40 deg.C, stirring for 50min until all the extract is dissolved, cooling to room temperature, and filtering to remove insoluble impurities to obtain the single-component composition.
Comparative example 4
Adding 50g of semen Sojae Atricolor extract and 50g of glycerol into 250mL flask equipped with thermometer and stirrer, heating to 40 deg.C, stirring for 50min until all the components are dissolved, cooling to room temperature, and filtering to remove insoluble impurities to obtain single component composition.
Example 10 zone of inhibition test.
1. Experimental strains: escherichia coli ATCC8099, Staphylococcus aureus ATCC6538, Bacillus subtilis ATCC55614 and Candida albicans ATCC10231, and the source is Guangdong province microbial strain collection center.
2. Preparation of a culture medium:
nutrient broth culture medium: taking 18g of nutrient broth culture medium solid, heating and dissolving in 1000mL of purified water, and autoclaving at 121 ℃ for 15min for later use.
Improving a martin culture medium: taking 28.5g of improved Martin culture medium solid, heating and dissolving in 1000mL of purified water, and autoclaving at 121 ℃ for 15min for later use.
3. Preparation of bacterial suspension:
sterilizing test tubes and nutrient broth culture medium at 121 deg.C for 30min, respectively, adding 5mL nutrient broth culture silicon rubber plugs into 3 sterilized test tubes on a superclean bench, cooling to below 40 deg.C, inoculating appropriate amount of Escherichia coli, Staphylococcus aureus, and Bacillus subtilis, respectively placing into the test tubes, mixing, culturing in 37 deg.C incubator for 18-24h, and adjusting turbidity with McLeeb turbidimeter to make bacterial suspension reach 10 ℃5CFU/mL, spare.
Sterilizing test tubes and nutrient broth culture medium at 121 deg.C for 30min, respectively, adding 5mL nutrient broth culture silicon rubber plugs into 3 sterilized test tubes on a superclean bench, cooling to below 40 deg.C, placing appropriate amount of Candida albicans into the test tubes, mixing, culturing at 26.5 deg.C for 18-24 hr, and adjusting turbidity with McLeeb turbidimeter to obtain bacterial suspension of 105CFU/mL, spare.
4. Experimental samples: the plant extract multi-effect compositions prepared in examples 5-9 and the one-component compositions prepared in comparative examples 1-4 were used at a concentration of 2% with a 1% glycerol aqueous solution as a blank.
5. And (3) measuring the antibacterial activity by an oxford cup method: and (3) sucking 300 mu L of the bacterial suspension into the solid culture medium by using a pipette gun, and uniformly coating by using an applicator. And clamping the oxford cup by using a sterile forceps and putting the oxford cup on a culture medium coated with uniform bacterial liquid, so that the oxford cup is fully contacted with the culture medium without a gap. The position of the oxford cup is moderate. Each strain was subjected to 3 replicates. After 150 mul of sample liquid is added into each Oxford cup, the culture dish is carefully placed in an incubator, escherichia coli, staphylococcus aureus and bacillus subtilis are placed in the incubator at 37 ℃, candida albicans are placed in the incubator at 26.5 ℃, the culture is cultured for 18-24h, the size of the inhibition zone is observed, and the diameter of the inhibition zone is measured by a ruler.
6. Judging the bacteriostatic action: if the diameter of the inhibition zone is larger than 7mm, the patient is judged to have the inhibition effect. And judging that the diameter of the inhibition zone is less than or equal to 7mm as no inhibition. And if the inhibition results are obtained in all 3 repeated experiments, judging the product to be qualified. The results are shown in Table 1.
TABLE 1 statistics of zone of inhibition.
Figure BDA0002838776380000061
Figure BDA0002838776380000071
As can be seen from the comparison in the above table, under the same dosage, when the artemisia capillaris thunb extract, the flos caryophylli extract, the cinnamon extract and the black soybean extract are used alone, the diameter of the inhibition zone is smaller than that of the composition using at least three of the artemisia capillaris thunb extract, the flos caryophylli extract and the black soybean extract, which indicates that the three or four components have synergistic antibacterial effect.
Example 11DPPH radical scavenging capacity assay.
The antioxidant capacity can be reflected by the measurement of DPPH free radical scavenging capacity. The higher the DPPH free radical clearance rate, the stronger the antioxidant capacity, and vice versa.
The specific method comprises the following steps:
a certain amount of DPPH is weighed and prepared into 0.04mg/mL DPPH solution by using absolute ethyl alcohol. 2mL of solutions of samples (2, 4, 6, 8mg/mL) prepared in examples 5 to 9 and comparative examples 1 to 4, respectively, at different concentrations were added to 2mL of DPPH solution, mixed well, left at room temperature for 30min, and then centrifuged at 5000r/min for 10 min. The supernatant was collected and absorbance was measured at 517 nm. Vc was used as a positive control. The DPPH radical clearance rate of the sample is calculated by the following formula:
DPPH free radical clearance rate of 100% - (A1-A2)/A0 × 100%
A0: the light absorption value of 2mL of absolute ethyl alcohol and 2mL of DPPH solution;
a1: the light absorption value of 2mL of sample solution +2mL of DPPH solution;
a2: absorbance of 2mL sample solution +2mL absolute ethanol.
Table 2 test results for DPPH radical scavenging rate.
Numbering Test sample DPPH radical clearance rate
1 Comparative example 1 63.2%
2 Comparative example 2 51.6%
3 Comparative example 3 56.4%
4 Comparative example 4 57.9%
5 Example 5 82.2%
6 Example 6 80.3%
7 Example 7 84.4%
8 Example 8 78.5%
9 Example 9 88.6%
From the above table, under the condition of the same amount, the antioxidant effect of any three or more of the compositions of artemisia capillaris extract, flos caryophyllata extract, cinnamon extract and black soybean extract is good when any one of the above components is used alone, wherein the antioxidant effect of the composition formed by the four extracts is the best, which indicates that the three or four components have synergistic antioxidant effect.
Example 12 preservation challenge evaluation experiments.
1. Experimental strains: the bacteria used in the experiment are mixed bacteria of pseudomonas aeruginosa ATCC9027, escherichia coli ATCC8739 and staphylococcus aureus ATCC 6538; the fungi include Candida albicans ATCC10231 and Aspergillus niger ATCC16404, and are from Guangdong province microorganism culture collection center.
2. Preparing the toner: the plant-extract multi-effect compositions prepared in examples 5 to 9 and the one-component compositions prepared in comparative examples 1 to 4 (in the following table 3, the plant-extract multi-effect compositions prepared in examples 5 to 9 and the one-component compositions prepared in comparative examples 1 to 4 are collectively referred to as compositions) were added to the formulations of table 3, respectively, to prepare skin lotions, the formulations of which are shown in table 3.
3. The test method comprises the following steps: referring to CTFA challenge experiment requirements, namely adding a certain amount of mixed microbial suspension into cosmetics, wherein the added mixed microbial suspension amount is as follows: bacterium 3.0X 107CFU/g (CFU/mL) and fungi 1.0X 105CFU/g (CFU/mL), and separating and detecting the mixed sample at a specific time to observe the survival condition of the microorganism.
4. And (3) judging test results: results at 0 hours (i.e., immediate post inoculation sampling), 7 days, 14 days, 21 days, and 28 days required 99.9% reduction in bacteria and 90% reduction in fungi at day 7; and continuously drops to zero within 28 days to judge the antiseptic effect of the toner, and the specific judgment result refers to table 4.
TABLE 3 toner formulation.
Name (R) Mass fraction (%)
Composition comprising a metal oxide and a metal oxide 0.5
Hyaluronic acid sodium salt 0.08
Trehalose 2
Sodium lactate 2
Demin medicine 0.2
Glucan 2
Glycerol glucoside 2
Lijian bacterin 3
Deionized water Balance of
The preparation method comprises the following steps:
1. adding deionized water, adding sodium hyaluronate, trehalose and sodium lactate into a stirring pot while stirring, and heating to about 85-90 deg.C;
2. standing, maintaining the temperature for 20min for sterilization, slowly cooling to about 60 deg.C under stirring, and adding chlorphenamine maleate, dextran, and glycerol glucoside into the system;
3. continuously stirring and cooling to about 40 ℃, respectively adding the linjian bacterin and the composition into the system, continuously stirring for about 10 minutes, stopping stirring and cooling, and then inspecting to be discharged;
4. and sealing the storage barrel after discharging, and moving to a standing room for later use.
TABLE 4. results of microbiological preservation challenge test of the resulting toner.
Figure BDA0002838776380000091
As can be seen from Table 4, the toners containing the plant extract multi-effect compositions prepared in examples 5-9 all passed the preservative challenge test and had potent preservative efficacy. The toners containing the one-component compositions prepared in comparative examples 1-4 showed a decrease in total bacterial and fungal counts over time, indicating that they all had some preservative efficacy, but none passed the preservative challenge test, and in addition, the plant extract multi-effect compositions had a synergistic preservative effect.
Example 13 human skin patch test:
the purpose of the test is as follows: the safety of the emulsions containing the phytoextraction multi-effect compositions prepared in examples 5-9 was tested.
Preparation of the emulsion: the plant extract multi-effect compositions prepared in examples 5-9 were added to the emulsions prepared according to the formulations in table 5, respectively, the formulations being given in table 5.
TABLE 5 emulsion formulation.
Figure BDA0002838776380000092
Figure BDA0002838776380000101
The preparation method of the emulsion comprises the following steps:
1. oil phase: adding glyceryl stearate, isononyl isononanoate, isooctyl palmitate, caprylic capric triglyceride and polydimethylsiloxane into a jacketed dissolving pot, starting steam for heating, and heating to 70-75 deg.C under continuously stirring to melt or dissolve completely. Adding an oil phase into the plant extraction multi-effect composition before emulsification;
2. water phase: adding deionized water into jacket dissolving pot, adding C12-20 alkyl glucose, C16/18 alcohol, dextran, EDTA disodium, and triethanolamine, stirring, heating to 90-100 deg.C, maintaining for 20min for sterilization, and cooling to 70-80 deg.C;
3. preparing xanthan gum, carbomer 941, and dextran, dissolving in water, stirring at room temperature to swell uniformly and prevent agglomeration, homogenizing if necessary, and adding water phase before emulsification. In order to supplement the water volatilized during heating and emulsification, 3 to 5 percent of water is added according to the formula;
4. and adding the oil-phase and water-phase raw materials into an emulsifying pot through a filter in a certain sequence, and stirring and emulsifying for a certain time at the temperature of 70-80 ℃. After emulsification, cooling the emulsification system to be close to room temperature, continuing stirring for about 10min, stopping stirring, cooling, and then checking to be discharged;
5. and sealing the storage barrel after discharging, and moving to a standing room for later use.
The test method comprises the following steps: a48 h closed patch test was used. Respectively weighing 0.02mL of diluted aqueous solution of different emulsion products into a spot tester, and simultaneously setting a blank control group, wherein the control group is the diluent of the cosmetic. 50 healthy volunteers are selected, the age is 18-24 years, and no allergic history exists. After cleaning the inner forearm of the subject, 0.02mL of sample was applied to a piece of filter paper attached to the plaque tester. The patch tester is applied to the inner side of forearm of the subject with non-irritating adhesive tape, and then is applied to skin by pressing with fingers for 48 h. The examinee is ordered to keep the spot-pasting part dry within 48h, and violent exercise, scratching the spot-pasting part, long-time sunlight irradiation and the like are avoided. After 48h, the tester is removed and marked, after 30min, the pressure marks disappear under sufficient light for judgment, and the revisit observation is carried out within 72h and 96h respectively.
TABLE 6 grading Standard of adverse skin reactions.
Figure BDA0002838776380000111
TABLE 7 Patch test results.
Figure BDA0002838776380000112
Figure BDA0002838776380000121
As can be seen from table 7, it was found through experiments that none of the emulsions containing the plant extract multi-effect compositions prepared in examples 5 to 9 had severe adverse reactions, and the subjects had substantially negative reactions, and it was determined that the emulsions containing the plant extract multi-effect compositions prepared in examples 5 to 9 had no adverse reactions to human bodies.

Claims (8)

1. A plant extraction multi-effect composition is characterized in that: the composition consists of a plant-derived antibacterial and antioxidant component and a solvent, wherein the plant-derived antibacterial and antioxidant component is selected from at least three of the following substances: herba Artemisiae Scopariae extract, flos Caryophylli extract, cortex Cinnamomi extract, and semen Sojae Atricolor extract; the plant source antibacterial and antioxidant component comprises the following components in percentage by mass: 0.5-30% of artemisia capillaris extract, 0.5-50% of flos caryophyllata extract, 1-40% of cinnamon extract and 1-40% of black soybean extract, wherein the mass percentages are expressed by the mass of each component relative to the total mass of the plant extraction multi-effect composition; the solvent is selected from one or more than one of 1, 2-propylene glycol, 1, 3-propylene glycol, 1, 2-butylene glycol, 1, 3-butylene glycol, 1, 4-butylene glycol, 1, 2-pentanediol, 1, 5-pentanediol, isoprene glycol, 1, 2-hexanediol, 1, 6-hexanediol, methoxybutanol, ethanol, menthol, ethyl acetate, laurocapram, polyvinylpyrrolidone, water, glycerol, methyl propylene glycol and ethyl hexyl glycerol.
2. The plant extract pleiotropic composition of claim 1, wherein the plant-derived antimicrobial and antioxidant ingredients are selected from the group consisting of: 0.5-30% of artemisia capillaris extract, 0.5-30% of flos caryophyllata extract and 1-40% of cinnamon extract.
3. The plant extract pleiotropic composition of claim 1, wherein the plant-derived antimicrobial and antioxidant ingredients are selected from the group consisting of: 0.5-30% of artemisia capillaris extract, 0.5-30% of flos caryophyllata extract and 1-40% of black soybean extract.
4. The plant extract pleiotropic composition of claim 1, wherein the plant-derived antimicrobial and antioxidant ingredients are selected from the group consisting of: 0.5-30% of flos caryophyllata extract, 1-40% of cinnamon extract and 1-40% of black soybean extract.
5. The plant extract pleiotropic composition of claim 1, wherein the plant-derived antimicrobial and antioxidant ingredients are selected from the group consisting of: 0.5-30% of artemisia capillaris extract, 1-40% of cinnamon extract and 1-40% of black soybean extract.
6. Use of a phytoextraction multi-effect composition according to claim 1 in the preparation of a cosmetic product comprising the phytoextraction multi-effect composition according to claim 1, wherein the cosmetic product is selected from the group consisting of facial mask solutions, skin lotions, essences, stock solutions, facial cleansers, perfumes, make-up removers, foundation lotions, foundations, concealers, rouges, lipsticks, eye shadows, and blushes.
7. Use of a phytoextraction multi-effect composition according to claim 1 in the preparation of a cosmetic product comprising the phytoextraction multi-effect composition according to claim 1, wherein the cosmetic product is selected from the group consisting of an emulsion, a cream, and a lotion.
8. The use of the plant extract multi-effect composition according to claim 6 or 7 in the preparation of cosmetics, characterized in that the mass percentage of the plant extract multi-effect composition is 0.1-5%.
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