CN117017880A - Plant energized essence and preparation method thereof - Google Patents
Plant energized essence and preparation method thereof Download PDFInfo
- Publication number
- CN117017880A CN117017880A CN202310837474.0A CN202310837474A CN117017880A CN 117017880 A CN117017880 A CN 117017880A CN 202310837474 A CN202310837474 A CN 202310837474A CN 117017880 A CN117017880 A CN 117017880A
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- extract
- essence
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- tremella
- plant
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Classifications
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- A61K8/8147—Homopolymers or copolymers of acids; Metal or ammonium salts thereof, e.g. crotonic acid, (meth)acrylic acid; Compositions of derivatives of such polymers
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- A61K8/9728—Fungi, e.g. yeasts
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- A61K8/9783—Angiosperms [Magnoliophyta]
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Abstract
The invention discloses a preparation process and quality evaluation of plant essence, wherein the formula of the essence is optimized by adopting single factor and orthogonal experiments, the use amount of bletilla striata extract, dittany bark extract and tremella extract is screened by taking the clearance of hydroxyl radicals as an index; and then the viscosity is used as an index to screen the dosage of auxiliary materials such as carbomer resin 940, sodium hyaluronate and the like. The essence has 3 functions of moisturizing, resisting oxidation and whitening, and can improve skin state with safety and no irritation.
Description
Technical Field
The invention relates to the technical field of natural cosmetics, in particular to essence of natural plant cosmetics, a preparation process thereof and quality evaluation.
Background
The market of skin care products has been developed until today, and the most important of the skin care products is the unification of the appearance and the effect of the products. Nowadays, with rapid progress in the skin care product industry, the update speed of skin care products is gradually increased, and more raw materials are applied to the field of skin care products. However, the selection of skin care raw materials is increasingly prone to natural products. The main reason is that the natural product has the special properties of low irritation, safety and no pollution, accords with the high-quality, healthy and environment-friendly skin care concept pursued by people at present, and is increasingly applied to skin care products at present. The development of traditional Chinese medicine has been thousands of years in China, and traditional Chinese medicine skin care is related to the development of traditional Chinese medicine in more than 2000, and according to relevant data, the ancient people in China use natural plant Chinese herbal medicines for skin care, thereby providing help and reference for more widely researching plant skin care products.
The Bletilla striata (Bletilla striata) is a traditional Chinese herbal medicine in the genus of Bletillae of the family of Orchidaceae, and the Bletilla striata gum in the Bletilla striata is a substance which can be used as a suspending agent and an emulsifying agent, has good effect of scavenging free radicals, and can be used for whitening and lightening spots, delaying skin aging, nourishing skin and the like.
Cortex Dictamni (Cortex Dictamni) is a dry root bark of Dictamni Radicis belonging to Rutaceae, and has antiinflammatory, antibacterial, and antioxidant effects. The cortex dictamni extract can be used for treating various skin diseases in clinic, and can be used for resisting candida albicans in vitro, and the cortex dictamni is often used for treating the skin diseases in ancient times by being matched with different traditional Chinese medicines.
Tremella (Tremella fuciformis) is also called tremella, tremella auriculata, and polysaccharide thereof has effects of resisting oxidization, improving skin and the like, and tremella polysaccharide is also called "plant hyaluronic acid".
The bletilla striata herbal hand cream, the dittany bark antibacterial cream and the tremella pearl nourishing cream have mild effects, small side effects and are deeply favored by consumers by pure natural plant traditional Chinese medicine essence. Because natural plant polysaccharide has viscosity, the skin care product has a moisturizing effect, and natural plants are often added into the skin care product in the form of plant polysaccharide.
Lin Min (Chinese medicinal composition, anti-inflammatory acne-removing essence and application [ P ]. Fujian province: CN115813982A, 2023-03-21), developing an anti-inflammatory acne-removing essence by taking patchouli, coptis chinensis, burdock and pseudo-ginseng as raw materials, wherein the essence comprises 0.1-10% of the Chinese medicinal composition, 0.1-2% of sodium hyaluronate and the balance of cosmetic matrix; the four components of the patchouli fermented product, the coptis extract, the burdock extract and the pseudo-ginseng extract are used for synergistic effect, so that acnes can be effectively removed, skin inflammation can be eliminated, damaged skin can be repaired, and the skin is smooth and elastic.
Luo Jia (an oil-controlling and moisturizing essence and its preparation method [ P ]. Sichuan province: CN115778842A, 2023-03-14). The oil-controlling and moisturizing essence is prepared from radix Glycyrrhizae, radix Scutellariae, lavender, and herba Menthae by: sodium hyaluronate, butylene glycol, propylene glycol, glycerin, ethanol, carbomer, tridecyl alcohol polyether, nicotinamide, plant extract, sodium hydroxide, and the balance water; the essence can be used for moisturizing and controlling the oil of the skin, can prevent impurities from entering the skin from pores to damage the skin, and can not influence the skin under the condition of controlling the oil and moisturizing.
Ouchun Feng (Ouchun Feng, hengfang, chen Yurong. A whitening and skin-brightening essence and its preparation method [ P ]. Guangdong province: CN115671001A, 2023-02-03) uses radix Paeoniae, radix Sophorae Flavescentis and herba Salvia officinalis as raw materials, and discloses a whitening and skin-brightening essence. The composition comprises the following components: solubilizer, humectant, nicotinamide, p-hydroxyacetophenone, skin conditioner, 1, 2-hexanediol, radix Paeoniae extract, radix Sophorae Flavescentis extract, herba Salvia officinalis extract, tranexamic acid, pH regulator, antioxidant, 1, 3-butanediol, and water. The paeonia lactiflora extract, the sophorae flavescentis extract and the sage extract have synergistic effect in whitening, and the essence also has excellent effects of resisting oxidation, resisting aging, nourishing, repairing and improving skin elasticity.
The energized cosmetics are regarded as names, endow the cosmetics with the functionality, and the common skin care products mainly comprise moisturizing, anti-aging, whitening and the like, wherein the moisturizing is the basic requirement of the skin care products. The essence in the current market can effectively remove acnes, preserve moisture and control oil, resist oxidation, resist aging and the like, but has single function.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides the essence which is easy to be absorbed by human skin, simultaneously endows the cosmetics with 3 functions of moisturizing, antioxidation and whitening, is safe and non-irritating, and has good market prospect. After 30 days of use, skin spots, pigments, acne and the like are obviously reduced, and skin moisture is increased; p >0.01 of pores and acnes has no significant difference, P <0.05 of spots, roughness, wrinkles and pigments has significant difference, and water P <0.01 has very significant difference; the results show that the essence can be used for supplementing water and improving the skin state.
According to a first aspect of the present invention, there is provided a plant-energized essence comprising carbomer resin 940, sodium hyaluronate, glycerin, 1, 2-propanediol, triethanolamine, bletilla striata extract, dittany bark extract, tremella extract and water; the triethanolamine is used to adjust the pH of the system to a skin acceptable range.
Preferably, the bletilla striata extracting solution is prepared by pulverizing 40g of bletilla striata, soaking in distilled water for 0.5h, extracting at 80deg.C for three times, wherein the ratio of the first time to the second time is 1:10 (g/mL), and the extracting time is l.5h; the second feed-liquid ratio is 1:6 (g/mL), and the extraction time is 1h; the third time of the liquid-to-solid ratio is 1:6 (g/mL), the extraction time is 0.5h, 3 layers of gauze are used for filtering, the three filtrates are combined, the mixture is heated and concentrated in a water bath to 500mL, the mixture is centrifuged at 4800rpm for 10min, the supernatant is taken out and placed in a refrigerator for standby, and the polysaccharide content in the bletilla striata extract is 65.78+/-3.7%.
Preferably, the preparation method of the cortex dictamni extract comprises the steps of crushing 50g of cortex dictamni, heating and extracting at a feed liquid ratio of 1:25 (g/mL) and 100 ℃ for 2 hours, filtering with 3 layers of gauze, centrifuging at 4800rpm for 10 minutes, taking the supernatant, and placing in a refrigerator for later use, wherein the polysaccharide content in the cortex dictamni extract is 6.47+/-1.1%.
Preferably, the tremella extract is prepared by crushing 40g tremella, extracting twice at 80 ℃, wherein the ratio of the first time to the second time is 1:25 (g/mL), and the extraction time is 1h; the second time of the extraction is carried out for 1h with the feed liquid ratio of 1:10 (g/mL). Filtering with 3 layers of gauze, mixing the filtrates, heating in water bath, concentrating to 400mL, centrifuging at 4800r/min for 10min, collecting the supernatant, and placing in refrigerator until the polysaccharide content in Tremella extract is 43.60+ -2.2%.
Preferably, the total weight ratio of the bletilla striata extract, the dittany bark extract and the tremella extract is 30% +/-5% according to the weight percentage.
Preferably, the weight percentages of carbomer resin 940, sodium hyaluronate 0.04+ -0.01%, glycerin 7+ -0.9%, 1, 2-propanediol 3+ -1.0%, triethanolamine appropriate amount, rhizoma Bletillae extract 7.47+ -1.2%, cortex Dictamni Radicis extract 3.74+ -1.0%, tremella extract 18.79+ -2.3% and ultrapure water are up to 100%.
According to a second aspect of the present invention, the present invention provides a method for preparing a plant-energized essence, comprising the steps of:
adding 1, 2-propylene glycol, carbomer resin 940, sodium hyaluronate and glycerol into ultrapure water with the temperature of 80-85 ℃, stirring until the components are completely dissolved, and keeping for 20min. Cooling to 40-45 ℃, adding triethanolamine, stirring to be transparent, finally adding the bletilla striata extract, the dittany bark extract and the tremella extract, stirring to be uniform without insoluble substances, and packaging to obtain the compound essence.
The application of the plant energizing essence is used for improving the skin state of a human body and moisturizing the skin.
Preferably, the improvement of the skin state of the human body means improvement of any one or more of skin spots, pigments, acne, pores, roughness and wrinkles. Further preferred is an improvement in skin problems of any one or more of skin stains, pigments, acne, roughness and wrinkles.
The essence is light yellow slightly viscous liquid, has light Chinese herbal medicine fragrance, and accords with the fragrance specified by Chinese cosmetic execution standard (GB/T21171-2018).
The pH value of the essence is 6.0+/-0.02, and the essence accords with the skin value of a human body. Viscosity: 400+/-10.8 mPas, and moderate viscosity; and (3) centrifuging: centrifuging at different rotation speeds, wherein the essence has no phenomena of water drops, layering and the like; heat resistance: the temperature is 40+/-1 ℃ and the reaction time is 24 hours, and no obvious difference exists between the reaction time and the experiment time; the cold resistance is 15+/-1 ℃, and the temperature is kept for 24 hours without obvious difference from the temperature before the experiment; cold and hot alternation test: the essence does not become thin, discolored, layered and precipitated and changes the state of the essence; combustion test: the phenomenon of outward splashing does not occur during combustion, and a small amount of black smoke occurs, which indicates that the less the content of grease components is, the smaller the grease water distribution coefficient is, the lower the hydrophobicity is, and the skin absorption effect is favorably influenced. The essence has good stability.
The total number of bacterial colonies of the essence disclosed by the invention shows that pseudomonas aeruginosa, staphylococcus aureus and escherichia coli are not detected, the total number of mould and saccharomycetes is less than or equal to 10, the total number of bacterial colonies is less than 20, and the detection result of the microbial index meets the requirements of cosmetic industry standards (GB/T7918-1987).
The moisture retention rate of the essence is 99.38+/-3.7%, and the moisture retention effect of the essence is best. The three plant polysaccharides can achieve the effects of antioxidation and anti-aging through the activity clearance rate of hydroxyl radicals of 65+/-2.7 percent. The inhibition rate of tyrosinase of the essence is 33.07 +/-1.6%, and the result shows that the essence can remarkably inhibit the activity of tyrosinase and has the whitening effect.
Compared with the prior art, the invention has the remarkable advantages that:
(1) According to the invention, the bletilla striata, the dittany bark and the tremella are added into the essence as three independent units, and the effects of moisturizing, antioxidation and whitening are achieved through the transdermal absorption effect of the essence.
(2) The polysaccharide components can be retained to the maximum extent by adopting a method of low feed liquid proportion and multiple hot water soaking, and the polysaccharide structure is retained from being damaged to a greater extent by hot water extraction.
(3) The essence is compared with the commercial essence from the aspects of moisturizing, antioxidation and whitening, and the result is that the essence has better moisturizing, antioxidation and whitening effects than the commercial essence.
Drawings
FIG. 1 is a comparison of the ability of different extract additions to scavenge hydroxyl radicals.
FIG. 2 effect curve.
Fig. 3 is a process flow diagram for preparing the essence.
FIG. 4 shows the relationship between moisture absorption rate and time change of each sample.
FIG. 5 shows the relationship between the moisture retention rate and the time change of each sample.
Figure 6 vitamin C hydroxyl radical scavenging profile.
Figure 7 vitamin C dose response curve.
FIG. 8A graph of the tyrosinase inhibition activity by arbutin.
FIG. 9 arbutin dose-response curve.
Fig. 10 is a comparison data analysis before and after 30 days of product use.
Fig. 11 is a graph of statistical differences.
Detailed Description
Example 1: determination of polysaccharide content
The phenol-sulfuric acid process is used. The absorbance at 490nm was measured using 1mL of a 5% phenol solution and 3.5mL of 98% concentrated sulfuric acid as a blank, and the absorbance A was plotted on the ordinate with the glucose concentration C as the abscissa.
Standard curve y=28.163x+0.04, r 2 ＝0.9991。
Example 2: preparation of plant extract
Preparation of rhizoma Bletillae extractive solution comprises pulverizing 40g rhizoma Bletillae, soaking in distilled water for 0.5 hr, extracting at 80deg.C for three times, wherein the ratio of the first material to the liquid is 1:10 (g/mL), and the extraction time is l.5 hr; the second feed-liquid ratio is 1:6 (g/mL), and the extraction time is 1h; the third time of the liquid-to-solid ratio is 1:6 (g/mL), the extraction time is 0.5h, 3 layers of gauze are used for filtering, the three filtrates are combined, the mixture is heated and concentrated in a water bath to 500mL, the mixture is centrifuged at 4800rpm for 10min, and the supernatant is taken and placed in a refrigerator for standby. The polysaccharide content in the rhizoma bletilla extract is 65.78+ -3.7%.
The preparation method of cortex Dictamni Radicis extractive solution comprises pulverizing 50g cortex Dictamni Radicis, heating at 100deg.C for 2 hr at a feed-liquid ratio of 1:25 (g/mL), filtering with 3 layers of gauze, centrifuging at 4800rpm for 10min, collecting the supernatant, and placing in refrigerator. The polysaccharide content in the cortex Dictamni Radicis extract is 6.47+ -1.1%.
The tremella extract is prepared by pulverizing 40g tremella, extracting at 80deg.C twice, wherein the first time of extraction is 1:25 (g/mL) for 1 hr; the second time of the extraction is carried out for 1h with the feed liquid ratio of 1:10 (g/mL). Filtering with 3 layers of gauze, mixing the filtrates, heating in water bath, concentrating to 400mL, centrifuging at 4800r/min for 10min, collecting the supernatant, and placing in refrigerator. The polysaccharide content in the tremella extract is 43.60+/-2.2%.
The polysaccharide obtained by the hot water extraction method has higher content, can be directly added and prepared, saves the cost and is beneficial to industrial production.
Example 3 method for evaluating functionality
(1) Moisture retention test
And measuring the moisture absorption rate, namely weighing 10g of a sample to be measured, placing the sample into a dryer with the temperature of 20+/-2 ℃ and the humidity of 81%, weighing the sample every 2 hours by using a balance, and calculating the moisture absorption rate.
Moisture absorption (%) = (m) 2 －m 1 )÷m 1 ×100％
And (3) measuring the moisture retention rate, namely weighing 10g of a sample to be measured, and placing the sample into a weighing bottle which is dried to constant weight. The weighing flask was placed in a desiccator containing silica gel (humidity 40%), and weighed with a balance at 2h intervals, and the moisture retention was calculated.
Moisture retention (%) =m 2 ÷m 1 ×100％
In the formula, m 1 The mass of the sample before drying; m is m 2 The mass of the sample after drying.
(2) Antioxidant experiment
Salicylic acid-ferrous sulfate process: (1) A is that 1 0.8mL 9mmol/L FeSO is taken 4 Mixing the solution with 0.60mL9mmol/L salicylic acid-ethanol solution, and fixing the volume to 10.0mL with distilled water; (2) A is that 2 0.80mL 9mmol/L FeSO is taken 4 Solution, 0.60mL9mmol/L salicylic acid-ethanol solution, 1.0mL 1% H 2 O 2 And mixing plant extracts with different concentrations, and then fixing the volume to 10.0mL by distilled water. (3) A is that 3 0.80mL 9mmol/L FeSO is taken 4 The solution, 0.60mL9mmol/L salicylic acid-ethanol solution and plant extracts with different concentrations are uniformly mixed, and distilled water is used for constant volume to 10.0mL.
A after constant volume is taken respectively 1 、A 2 、A 3 1mL of the solution, and the absorbance was measured at a wavelength of 510 nm. Distilled water is used as a reference substance, and the clearance rate in the sample is calculated by adopting the following formula:
(3) Tyrosinase inhibition rate
Phosphate Buffer Solution (PBS), weighing 7.16g of sodium dihydrogen phosphate, and fixing the volume to 100mL with distilled water to obtain solution A; weighing 3.12g of disodium hydrogen phosphate, and fixing the volume to 100mL by using distilled water to obtain a solution B; taking 51mL of solution A and 49mL of solution B, and mixing to obtain the phosphate buffer solution.
L-tyrosine solution 50.0 mg L-tyrosine is precisely weighed into a 50mL volumetric flask and dissolved in phosphate buffer. 1.0mg of tyrosinase was weighed precisely, dissolved in phosphate buffer and fixed to a volume of 10mL, and stored at 4℃for further use.
Table 1 reaction solution preparation scheme
The tyrosinase inhibition rate is used as an index: four solutions were added according to Table 1, each set was set up for 3 parallel runs, water-bath at 37℃for 10min, then tyrosinase solution was added,stirring well, and heating in water bath at 37deg.C for 20min; taking out from the water bath, adding 200 mu L of each reaction solution into a 96-well plate, measuring absorbance at 475nm, and marking as A 1 、A 2 、A 3 、A 4 . Preparing 1mg/mL arbutin solution by using arbutin as a control, respectively diluting the arbutin solution into 0.8mg/mL, 0.6mg/mL, 0.4mg/mL and 0.2mg/mL of arbutin solution, measuring absorbance at 475nm by using an enzyme-labeled instrument, calculating tyrosinase inhibition rate, drawing a standard curve, drawing a dose-response curve graph, and calculating IC (integrated circuit) 50 。
In which A is 1 Absorbance values containing only substrate and tyrosinase system;
A 2 absorbance values containing only substrate;
A 3 absorbance values of the substrate, tyrosinase, inhibitor system only;
A 4 absorbance values for substrate, inhibitor system only.
Example 4: essence plant extract and auxiliary material single factor experiment
The embodiment provides a method for optimizing plant extract and auxiliary materials by single factors, which comprises the following steps:
(1) Single factor experiment of plant extract
The salicylic acid-ferrous sulfate method in example 3 (2) was used to determine the ability of the different concentrations of bletilla striata extract, dittany bark extract and tremella fuciformis extract to scavenge hydroxyl radicals, and three experiments were repeated.
The factors of 1mL of dittany bark extract and 1mL of tremella extract are fixed, the investigation variables of the bletilla striata extract are 0.5mL, 1mL, 1.5mL, 2mL and 2.5mL, and when the adding amount of the bletilla striata extract is 1.5mL, the clearance of the plant extract to OH is up to 94.50%.
The fixed factors are 1mL of bletilla striata extract and 1mL of tremella extract, the investigation variables of the dittany bark extract are 0.5mL, 1mL, 1.5mL, 2mL and 2.5mL, and when the addition amount of the dittany bark extract is 1.0mL, the clearance of the plant extract to OH is up to 84.20%.
The fixed factors are 1mL of bletilla striata extract and 1mL of dittany bark extract, the investigation variables of tremella extract are 0.5mL, 1mL, 1.5mL, 2mL and 2.5mL, and when the addition amount of tremella extract is 3.0mL, the clearance of the plant extract to OH is up to 95.59%.
According to the antioxidation result in fig. 1, the dosage of the bletilla striata extract in the essence is 1.5mL, the dosage of the dittany bark extract in the essence is 1.0mL, and the dosage of the tremella extract in the essence is 3.0mL.
In summary, the dosage of the cortex dictamni extract is 1.0mL, the dosage of the bletilla striata extract is 1.5mL, the dosage of the tremella extract is 3.0mL, the ratio is 30%, the ratio is 2:3:6, and all the extracts are added according to the actual required amount in proportion.
(2) Adjuvant single factor experiment
The viscosity of the liquid product was measured according to the method of national standard surfactant and detergent rotational viscometer (GB/T15357), and the amounts of carbomer resin 940 and sodium hyaluronate were selected using the viscosity as an index (viscosity of essence at 400.+ -. 10.8 Pa.s): the fixed factors of 1.5mL of bletilla striata extract, 1.0mL of dittany bark extract, 3.0mL of tremella extract, 10g of glycerin, 3g of 1, 2-propylene glycol, the study variables of 0.1g, 0.2g, 0.3g, 0.4g and 0.5g (0.04 g of sodium hyaluronate) of carbomer resin 940, and the study variables of 0.02g, 0.03g, 0.04g, 0.05g and 0.06g (0.3 g of carbomer resin 940) of sodium hyaluronate are respectively complemented with water to 100g in 2 experiments.
The amounts of glycerol and 1, 2-propanediol used were selected using the moisture retention rate of example 3- (1) as an index.
The fixed factors of 1.5mL of bletilla striata extract, 1.0mL of dittany bark extract and 3.0mL of tremella extract, 940.3 g of carbomer resin and 0.04g of sodium hyaluronate, the research variables of 5g, 7g, 9g, 11g and 13g (3 g of 1, 2-propanediol), the research variables of 1, 2-propanediol and 1g, 2g, 3g, 4g and 5g (10 g of glycerol) are respectively supplemented with water to 100g in 2 experiments.
Results of adjuvant usage: the viscosity affects the sensory evaluation of the essence, reduces the use feeling, and is preferably added with 0.3+ -0.02 g of carbomer resin 940 and 0.04+ -0.01 g of sodium hyaluronate in combination with the viscosity of the essence in life. When the adding amount of the glycerol is 7+/-0.9 g, the lost water is the lowest, and the moisture retention rate is the highest; however, since the added amount of glycerin is large, which leads to an increase in the viscosity of the concentrate and a decrease in the sensory score, the added amount of glycerin is preferably 7g; when the addition amount of 1, 2-propylene glycol is 3+/-1.0 g, the lost water is the lowest; 1. the moisture retention rate was highest when the amount of 2-propanediol added was 3.+ -. 1.0 g.
(3) Orthogonal experiments
The dosage is further optimized by selecting seven factors of sodium hyaluronate, carbomer resin 940, glycerol, 1, 2-propylene glycol, rhizoma Bletillae extract, cortex Dictamni Radicis extract and Tremella extract, wherein three levels (see Table 2) are selected according to L18 (3) 7 ) The orthogonal table (see table 3) is tested, viscosity, pH, moisture retention, tyrosinase inhibition rate and hydroxyl radical removal rate are used as indexes, comprehensive evaluation is carried out by using a comprehensive evaluation method, the queuing evaluation method described in the literature is adopted, corresponding evaluation values are given by sequencing, and are used as unit indexes for data analysis and processing, and the optimal combination is selected. (orthogonal experiment reduced by 10 times, finally make up to 10g with water)
TABLE 2 orthogonality factor and level table
Note that: 1.5mL = 1.02g of bletilla striata extract, 1.0mL = 0.68g of dittany bark, 3.0mL = 2.05g of tremella extract.
TABLE 3 orthogonal experiment schedules
The method for measuring the viscosity and the moisture retention rate is as above; the pH was measured according to GB/T13531.1-2008.
According to the invention, firstly, the addition amounts of the bletilla striata extract, the dittany bark extract and the tremella extract are inspected through a single factor experiment, and secondly, the addition amounts of the plant extract and the auxiliary materials are further optimized through an orthogonal experiment.
The viscosity, the moisture retention rate, the hydroxyl radical removal rate and the tyrosinase inhibition rate are used as indexes, a queuing scoring method is adopted for comprehensive scoring, the viscosity score is shown in table 4, the moisture retention rate score is shown in table 5, the hydroxyl radical removal rate score is shown in table 6 and the tyrosinase inhibition rate score is shown in table 7. Visual analysis and analysis of variance of experimental data results are shown in table 8.
Table 4 essence viscosity score data sheet
Table 5 essence moisture retention score data sheet
Table 6 essence hydroxyl radical clearance score data sheet
TABLE 7 essence tyrosinase inhibition score data sheet
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Table 8 visual analysis table for orthogonal experimental results
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According to visual analysis table 8, the degree of influence of each factor on the experiment was determined. If seven factors of bletilla striata extract, dittany bark extract, tremella extract, carbomer resin 940, sodium hyaluronate, glycerol and 1, 2-propanediol are respectively marked as A, B, C, D, E, F, G, the arrangement sequence of main and secondary factors is B > C > F > A > D > E > G. In the experiment, the optimal level combination of each factor is determined according to the experimental index value to select the optimal test scheme. At the same time, the comprehensive effect curve (figure 2) is synthesized to obtain a correct comprehensive analysis result, a comprehensive visual analysis table and an effect curve graph to obtain a preferred scheme B 1 C 1 F 2 A 1 D 2 E 2 G 1 Namely 0.68g of bletilla striata extract, 0.34g of dittany bark extract, 1.71g of tremella extract, 940.03 g of carbomer resin, 0.004g of sodium hyaluronate, 0.7g of glycerol, and 0.03g of 1, 2-propanediol. The weight percentages of the bletilla striata extract, the dittany bark extract, the tremella extract, the carbomer resin 940.3 g, the sodium hyaluronate 0.04g, the glycerol 7g, the 1, 2-propylene glycol 0.3g are 6.8g, 3.4g, 17.1 g.
Calculated by the formula proportion of 100%, the total amount ratio of the bletilla striata extract, the dittany bark extract and the tremella extract to the essence is 30%, and the ratio of the bletilla striata extract to the dittany bark extract to the tremella extract is 2:3:6 in sequence. According to the orthogonal test result, the proportion of the total addition of the three components of 27.3 percent and 30 percent is calculated to obtain 7.47 percent of bletilla striata extract, 3.74 percent of dittany bark extract and 18.79 percent of tremella extract. The final specific formulation is shown in Table 9.
Table 9 final formulation of Compound plant essence
Note that: the dosage of the triethanolamine is based on the pH=6.0+/-0.02 of the final compound plant essence system, and meets the requirements of human bodies.
Example 5: preparation method of essence
Carbomer resin 940 0.3+ -0.02%, sodium hyaluronate 0.04+ -0.01%, glycerol 7+ -0.9%, 1, 2-propylene glycol 3+ -1.0%, rhizoma Bletillae extract 7.47+ -1.2%, cortex Dictamni Radicis extract 3.74+ -1.0%, tremella extract 18.79+ -2.3%, and ultrapure water to 100%.
Adding 1, 2-propylene glycol, carbomer resin 940, sodium hyaluronate and glycerol into ultrapure water with the temperature of 80-85 ℃, stirring until the components are completely dissolved, and keeping for 20min. Cooling to 40-45deg.C, adding triethanolamine, stirring to transparency, adding rhizoma Bletillae extractive solution, cortex Dictamni Radicis extractive solution and Tremella extractive solution, stirring to uniformity without insoluble substances, and packaging to obtain compound essence (figure 3); and used for the tests of examples 6-10.
Example 6: functional evaluation results
(1) Moisture retention test
The moisture absorption and retention effects of glycerin, 1, 2-propanediol, tremella extract and bletilla extract, essence samples (prepared in example 5) and control (meii water-run essence-threg make-up net preparation 2019003654) were compared as determined in example 3 (1).
The results show that: when the time is 6h, the moisture retention capacity is that essence, control group, glycerin, tremella extract, bletilla striata extract, 1, 2-propylene glycol. The moisturizing rate of the experimental group (essence sample) is 99.38+/-3.7%, the moisturizing rate of the control group is 89.37+/-2.9%, and the moisturizing effect of the experimental group is the best, and the results are shown in figures 4 and 5.
(2) Antioxidant experiment
The salicylic acid-ferrous sulfate method of example 3 (2) was used to determine the ability of the essence sample to scavenge hydroxyl radicals.
The results show that: the essence sample prepared in example 5 has a hydroxyl radical activity clearance of 65+/-2.7%, can achieve the effects of antioxidation and anti-aging, and has a hydroxyl radical clearance of 30.14+/-2.6% for the essence of the control group. The essence sample has better antioxidation effect.
Fig. 6 is a graph of the hydroxyl radical scavenging rate of vitamin C. The regression equation of vitamin C is y=95.765x+3.919, and the linear coefficient is R 2 =0.9975. IC for scavenging vitamin C hydroxyl radical is obtained from vitamin C dose-response curve chart (figure 7) 50 Is 0.5744mg/mL.
(3) Whitening experiment
The whitening effect of the essence sample and the control group essence was measured as in (3) of example 3, and the results showed that: the tyrosinase inhibition rate of the essence sample prepared in example 5 was 33.07 + -1.6%, and the tyrosinase inhibition rate of the control group was 30.72+ -1.3%.
FIG. 8 is a graph showing the inhibition of tyrosinase activity by arbutin. The regression equation of arbutin is y=53.806x+22.35, and the linear coefficient R 2 = 0.9951. IC for inhibiting tyrosinase activity by arbutin is obtained from arbutin dose-response curve chart 9 50 Is 0.5837mg/mL.
The tyrosinase inhibition rate is an important index for evaluating the activity of the whitening agent, and the higher the inhibition rate is, the stronger the tyrosinase activity inhibition capability is, and the better the whitening effect is. Therefore, the essence can obviously inhibit tyrosinase activity and has the whitening effect.
Example 7 sensory evaluation
50 healthy people with correct discrimination ability and 20-50 years old are selected as volunteers, and 4cm of the arms of the volunteers are selected 2 In (2) were applied evenly to the arm and the volunteer looped with the other hand until the sample was completely absorbed and sensory scored during application. All take excellent (90 points), good (80 points) and lattice (60 points) as scoring standards, applyThe questionnaire method performed statistics on volunteer scores.
And counting the situations of people with different skin types in the using process and after the use of the woody product by adopting a questionnaire investigation mode, and summarizing to obtain the conclusion shown in the table 10 below.
Table 10 sensory evaluation results
EXAMPLE 8 evaluation of physicochemical Properties
The character is that whether the color and the luster of the product are comfortable and beautiful or not is judged by observing the color and the luster of the essence, whether the product is uniform or not has layering phenomenon or not is checked by smell sense. The results show that: the light yellow liquid with a slight viscous shape has the fragrance of Chinese herbal medicines, and meets the prescribed fragrance.
pH value measurement according to the method for detecting pH value of national standard cosmetic general test method (GB/T13531.1-2008), the pH value of the essence sample is measured at room temperature of 25 ℃. The pH meter was calibrated according to the instructions of the instrument, the electrodes were inserted into the serum, read, and the data recorded. The experiments were performed in triplicate. The results show that: 6.0+/-0.02, and accords with the skin value of a human body.
Viscosity the method for measuring liquid products according to the national standard surfactant and detergent rotational viscometer (GB/T15357) was carried out using a rotational viscometer. Standing the essence at room temperature for 24 hours to remove bubbles, pouring the essence into a beaker, regulating the temperature of the essence to 23 ℃ by a constant-temperature water bath, selecting a proper rotor, immersing the rotor into a solution to be tested, preventing the essence from generating bubbles, and recording data in three times in parallel when the reading of a rotary viscometer is stable. The results show that: 400+/-10.8 mPa.s, and the essence has moderate viscosity and is favorable for skin absorption.
Centrifugal test, namely taking 5g of essence according to an experimental method described in national standard skin care emulsion (GBT 29665-2013) of the people's republic of China, respectively centrifuging for 30min at 2000r/min, 3000r/min, 4000r/min and 5000r/min, and observing whether the essence has layering, water-oil separation and other phenomena. The results show that: centrifugal force at different rotation speeds, the essence has no phenomena of water drops, layering and the like.
According to the experimental method described in national standard skin care emulsion (GBT 29665-2013) of the people's republic of China, 2g of each of the two essences is taken, one of the two essences is placed in a constant temperature incubator at 40+/-1 ℃ for 24 hours and then taken out, after the temperature is cooled to room temperature, the two essences are compared with the other one, and whether the essences are thinned, discolored, layered, precipitated and the like is observed to judge the heat resistance of the essences. The results show that: the temperature is 40+/-1 ℃ and the temperature is placed for 24 hours, and no obvious difference exists between the temperature and the temperature before the experiment.
According to the experimental method described in national standard skin care emulsion (GBT 29665-2013) of the people's republic of China, 2g of each of the two essences is taken, one sample is placed in a refrigerator at the temperature of minus 15+/-1 ℃ for 24 hours and taken out, after cooling to room temperature, the cooled sample is compared with the other essence, and whether the essences are thinned, discolored, layered, precipitated and the like is observed to judge the cold resistance of the essences. The results show that: -15+ -1deg.C, standing for 24h, no obvious difference from the experiment.
According to the experimental method described in the determination of the storage stability of the water-in-oil emulsion of the surfactant (GB/T16497-2007) national standard of the people's republic of China, 2g of essence is taken, placed in a constant temperature incubator at 40+/-1 ℃ for 24 hours, then placed at room temperature for 24 hours, and finally placed in a refrigerator at-15+/-1 ℃ for 24 hours, and whether layering, precipitation and color change of the essence occur or not is observed. The results show that: the essence still keeps its own state.
Burning test, namely putting 2g of essence into a crucible, putting an asbestos net on an electromagnetic oven, heating, observing the state of the essence, and smelling whether the essence has smell change. The results show that: the phenomenon of outward splashing does not occur during combustion, and a small amount of black smoke occurs, which indicates that the less the content of grease components is, the smaller the grease water distribution coefficient is, the lower the hydrophobicity is, and the skin absorption effect is favorably influenced.
EXAMPLE 9 evaluation of health index
1g of essence is added into 99mL of sterilized normal saline by a disinfection straw, mixed to prepare a detection solution of 1:100, cultured for 24 hours under specific conditions, and then the total number of colonies of 0.5mL of detection samples is measured, and the total number of bacteria, the total number of moulds and yeasts, the heat-resistant coliform bacteria, staphylococcus aureus and pseudomonas aeruginosa in the essence are measured according to the standard detection method of cosmetic microorganisms in 2015 edition of cosmetic safety technical Specification, and the results are shown in Table 11.
TABLE 11 microbial indicator evaluation results
Example 10 human body experiment measurement
Selecting 60 volunteers with healthy skin, dividing into 6 groups, and measuring 4cm in arm 2 2g of essence is weighed and evenly smeared on the inner side of an arm, the moisture and oil content of skin before smearing is measured by a skin moisture and oil tester, and then the moisture and oil contents of skin after smearing the essence for 5, 10, 15, 30 and 60 minutes are measured and compared, so that the moisture retention condition of the essence can be known. As can be seen from fig. 4 and 5, the moisture absorption rates of the glycerin, 1, 2-propanediol, tremella and bletilla striata extracts are gradually increased, the moisture retention rate is gradually reduced, the moisture retention rate of a single component is increased with time, the moisture retention effect is reduced, the essences of the experimental group and the control group are increased with time, and the moisture retention effect is remarkable.
However, the moisture absorption rate and the moisture retention rate of the essence and the control group are gradually increased, and the decrease speed of the moisture retention rate reflects the quality of the moisture retention performance of the substance. When the time is 6h, the moisture retention capacity is that essence, control group, glycerin, tremella extract, bletilla striata extract, 1, 2-propylene glycol. The moisture retention rate of the essence is 99.38+/-3.7%, the moisture retention rate of the control group is 89.37+/-2.9%, and the moisture retention effect of the essence is best.
In combination with the above method, the skin water oil condition was measured using a skin water oil tester, as shown in table 12. The results show that the essence can reduce skin oil content and improve skin moisture, and has the effects of moisturizing and regulating skin water-oil balance.
Table 12 skin water oil test results
Example 11 Instrument evaluation
Selecting 30 subjects without allergy history, weighing 2g of essence, smearing the essence on a skin fixed position, detecting the skin condition before the face is used by the product by using a magic mirror instrument, recording, uniformly smearing the 2g of essence on the face of a volunteer until the face is absorbed, detecting the face condition of the volunteer after the volunteer uses the product for one month again, and comparing the skin conditions before and after the use to know the action effect of the essence on the skin of the human body.
In combination with the above experimental method, before using the product, the data analysis of the color spots, pigments, wrinkles, acne moisture and the like on the face of the subject were measured by using a magic mirror instrument, and then after 30 days according to the use of the product, the data analysis of the color spots, pigments, wrinkles, acne, moisture and the like on the face were measured by combining the magic mirror instrument, as shown in fig. 10.
The data of the subjects before and after using the product, such as shown in fig. 10, are measured by combining a magic mirror instrument, and after using the essence for 30 days, skin color spots, pigments, acne and the like are obviously reduced, and skin moisture is increased. P >0.01 for pores and comedones has no significant difference, P <0.05 for stains, roughness, wrinkles and pigments has significant difference, and P <0.01 for moisture has significant difference. The results show that the essence can be used for supplementing water and improving the skin state. The result is that the bletilla striata polysaccharide is a polysaccharide with viscosity, so that a layer of film with good flexibility can be formed on the surface of the skin to prevent the skin from losing moisture; the tremella polysaccharide can improve skin conductivity and harm caused by toxic and harmful substances entering into skin, prevent skin moisture evaporation, increase skin epidermis moisture content, improve skin roughness, remove facial freckle, and has effects of promoting cell proliferation, dividing and reducing aging cell number. The sodium hyaluronate taken in from the outside can be decomposed into oligosaccharide by bacteria in the cecum, and can be absorbed by the large intestine, and can be introduced into the whole body from blood or lymph, so that the secretion of hyaluronic acid by cells in dermis layers can be promoted, and the relative stability of skin water content can be maintained. The sodium hyaluronate can improve the living environment of skin cells, induce proliferation and differentiation of cells, permeate the skin, help metabolism, accelerate cell renewal, improve skin immunity and achieve the effects of maintaining beauty and keeping young. Since tremella polysaccharide and hyaluronic acid are very similar in structure and can improve skin condition, it is presumed that tremella polysaccharide may have the same percutaneous absorption effect as hyaluronic acid. Experimental results show that the moisturizing and moisturizing effects can be achieved by compounding different plant extracts according to a certain proportion, and the moisturizing and moisturizing effects can be achieved, and the skin quality can be improved.
The statistical differences in moisture retention, oxidation resistance and whitening of the serum and the control serum are shown in figure 11. The moisture retention rate is 0.01< P <0.05, and the moisture retention rate has obvious difference; the P value of the hydroxyl radical clearance rate is less than 0.01, the remarkable difference exists, and the tyrosinase inhibition rate has no remarkable difference.
The bletilla striata in the essence studied in the example 5 is used as a core component, has the functions of absorbing water and combining water, and the bletilla striata polysaccharide can form a layer of film on the surface of the skin, so that the moisture loss is prevented, and the moisturizing effect is realized; the bletilla striata polysaccharide and the dittany bark both have the functions of removing hydroxyl radicals and inhibiting tyrosinase activity; the tremella polysaccharide and the sodium hyaluronate can be absorbed transdermally, the tremella polysaccharide has the functions of moisturizing, scavenging hydroxyl free radicals, inhibiting tyrosinase activity and the like, and the three plant polysaccharides are taken as independent units, and after being compounded with a skin care product matrix, stronger energizing effect is generated, and compared with a control group, the essence has better energizing effect.
Example 12 skin irritation test
Selecting 30 healthy people 18-40 years old with correct discrimination as volunteers, and selecting 5cm area behind the volunteer ear and at the arm 2 Is rubbed with alcohol while keeping the test area dry and clean and avoiding contact with other skin preparations (e.g., other skin care cosmetics or pharmaceutical preparations). The essence is uniformly smeared on the tested part for 2 times a day, and the thickness is about 1 mm. In the experimental process, the experimental part of the subject needs to be kept dry and clean for 2h,4h and 8h respectively,after 16h,32h and 48h, observing the smeared part of the skin to observe abnormal phenomena such as erythema, edema, allergy and the like.
The natural plants have safety, the extraction method is a hot water extraction method, no organic solvent is added, the auxiliary materials for preparing the essence are components such as glycerin, 1, 2-propylene glycol, sodium hyaluronate and the like which are commonly added in skin care products, no chemical preservative is added, and the evaluation grade is 0, wherein the irritation evaluation result shows that allergic phenomena such as erythema, edema and the like do not appear after the volunteer smears the essence.
The foregoing examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the foregoing examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principles of the present invention should be made therein and are intended to be equivalent substitutes within the scope of the present invention.
Claims (10)
1. A plant energized essence comprises carbomer resin 940, sodium hyaluronate, glycerol, 1, 2-propylene glycol, triethanolamine, rhizoma Bletillae water extract, cortex Dictamni Radicis water extract, tremella water extract and water; the triethanolamine is used for regulating the pH of the system to the acceptable range of skin;
the polysaccharide content in the bletilla striata water extract is 65.78+/-3.7%; the polysaccharide content in the water extract of the cortex dictamni is 6.47+/-1.1 percent; the polysaccharide content in the tremella water extract is 43.60+/-2.2%.
2. The plant energized essence according to claim 1, wherein the aqueous extract of bletilla striata is prepared by pulverizing 40g of bletilla striata, soaking in distilled water for 0.5h, extracting at 80deg.C for three times, the ratio of the first time to the second time being 1:10 (g/mL), and extracting for l.5h; the second feed-liquid ratio is 1:6 (g/mL), and the extraction time is 1h; the third time of the liquid-to-solid ratio is 1:6 (g/mL), the extraction time is 0.5h, 3 layers of gauze are used for filtering, the three filtrates are combined, the mixture is heated and concentrated in a water bath to 500mL, the mixture is centrifuged at 4800rpm for 10min, the supernatant is taken out and placed in a refrigerator for standby, and the polysaccharide content in the bletilla striata extract is 65.78+/-3.7%.
3. The plant energized essence according to claim 1, wherein the water extract of dittany bark is prepared by pulverizing 50g of dittany bark, heating and extracting at 100deg.C for 2h at a ratio of 1:25 (g/mL), filtering with 3 layers of gauze, centrifuging at 4800rpm for 10min, collecting the supernatant, and placing in a refrigerator for use, wherein the polysaccharide content in the water extract of dittany bark is 6.47+ -1.1%.
4. The plant energized essence according to claim 1, wherein the tremella water extract is prepared by pulverizing 40g tremella, extracting twice at 80deg.C, wherein the ratio of the first time to the second time is 1:25 (g/mL), and the extraction time is 1h; the second time of the extraction is carried out for 1h with the feed liquid ratio of 1:10 (g/mL). Filtering with 3 layers of gauze, mixing the filtrates, heating in water bath, concentrating to 400mL, centrifuging at 4800r/min for 10min, collecting the supernatant, and placing in refrigerator until the polysaccharide content in the tremella water extract is 43.60+ -2.2%.
5. The plant energized essence according to claim 1, wherein the total amount of the bletilla striata extract, the dittany bark extract and the tremella extract is 30% ± 5% by weight.
6. The plant energized essence according to claim 1, wherein the weight percentage is calculated according to the weight percentage, 0.3+/-0.02% carbomer resin 940, 0.04+/-0.01% sodium hyaluronate, 7+/-0.9% glycerin, 3+/-1.0% 1, 2-propylene glycol, a proper amount of triethanolamine, 7.47+/-1.2% bletilla striata extract, 3.74+/-1.0% dittany bark extract, 18.79+/-2.3% tremella extract and ultrapure water are complemented to 100%.
7. A method for preparing the plant energized essence according to claim 1, comprising the following steps:
adding 1, 2-propylene glycol, carbomer resin 940, sodium hyaluronate and glycerol into hot ultrapure water, and stirring until completely dissolved; cooling, adding triethanolamine, stirring to transparency, adding rhizoma Bletillae extractive solution, cortex Dictamni Radicis extractive solution and Tremella extractive solution, stirring to uniformity without insoluble substances, and packaging to obtain compound essence.
8. Use of the plant energizing essence of claim 1 for improving the skin condition and moisturizing the skin of a human.
9. The use according to claim 8, wherein the improvement of human skin state is an improvement of skin problems of any one or more of skin stains, pigments, acne, pores, roughness and wrinkles.
10. The use according to claim 8, wherein the improvement of human skin state is an improvement of skin problems of any one or more of skin stains, pigments, acne, roughness and wrinkles.
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