CN115463055B - Composition containing celery seed volatile oil, facial cream and preparation method of facial cream - Google Patents
Composition containing celery seed volatile oil, facial cream and preparation method of facial cream Download PDFInfo
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- CN115463055B CN115463055B CN202211313485.0A CN202211313485A CN115463055B CN 115463055 B CN115463055 B CN 115463055B CN 202211313485 A CN202211313485 A CN 202211313485A CN 115463055 B CN115463055 B CN 115463055B
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- volatile oil
- celery seed
- oil
- seed volatile
- stirring
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Classifications
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- A61K2800/74—Biological properties of particular ingredients
- A61K2800/78—Enzyme modulators, e.g. Enzyme agonists
- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
Abstract
The invention relates to an antioxidant and whitening cosmetic, in particular to a composition containing celery seed volatile oil, a facial cream and a preparation method of the facial cream, wherein the celery seed volatile oil and plant extract are mixed according to a ratio of 1:0.1 to 30 mass ratio; the plant extract is one or more of calendula, dandelion, red paeony root and lithospermum. Compared with the prior art, the invention provides a novel formula containing the celery seed volatile oil for the antioxidation and whitening cream and a corresponding preparation method, and has the advantages of high safety, obvious synergistic effect, convenient preparation, low cost and the like.
Description
Technical Field
The invention relates to an antioxidant and whitening cosmetic, in particular to a composition containing celery seed volatile oil, a facial cream and a preparation method of the facial cream.
Background
In recent years, many studies have found that, after some herbal extracts act on the skin, the effect of repairing or beautifying the skin can be achieved by metabolism.
The plant volatile oil is widely studied due to the excellent characteristics of no toxicity, multiple functional components, green and pollution-free properties and the like. For example, the celery seed volatile oil is a faint yellow oil substance extracted from celery seeds, can be used as both medicine and food, has unique fresh fragrance, and has the effects of removing edema, promoting skin smoothness, improving blood flow, lowering blood pressure, improving brain microcirculation and the like. The celery seed essential oil has the functions of resisting oxidation, resisting tumor, inhibiting bacteria and the like, and can be applied to the fields of foods, beauty cosmetics, health care products, medicines and the like.
At present, a plurality of researchers perform antioxidant and whitening researches on the compounding of various Chinese herbal medicines, but only simple superposition of some effects is achieved, deep excavation and research are not performed, and expected effects are difficult to achieve; even the compounding of different species in some formulas can generate antagonism, so that the efficacy performance of the compound is reduced, raw materials are wasted, and the product cost is further increased. Therefore, how to develop efficient, safe and stable synergistic antioxidant and whitening skin care products is still a difficult point.
The invention provides a compound formula containing celery seed volatile oil, which has synergistic antioxidation and whitening effects.
Disclosure of Invention
The invention aims to solve at least one of the problems, and provides a composition containing celery seed volatile oil, a facial cream and a preparation method of the facial cream, and provides a novel formula containing celery seed volatile oil for antioxidation and whitening facial cream and a corresponding preparation method.
The aim of the invention is achieved by the following technical scheme:
The invention discloses a composition containing celery seed volatile oil, which is prepared from celery seed volatile oil and plant extract in a ratio of 1:0.1 to 30 mass ratio;
The plant extract is one or more of calendula, dandelion, red paeony root and lithospermum.
Further preferably, the celery seed volatile oil and the plant extract are mixed according to the ratio of 1: and the mass ratio of 0.5-20.
Still further preferably, the compounding ratio of the celery seed volatile oil and the calendula ethyl acetate phase is selected from 1:1 or 1:5 or 1:9, a step of performing the process; the compounding ratio of the celery seed volatile oil and the dandelion alcohol extract is selected from 1:5, a step of; the compounding ratio of the celery seed volatile oil and the red paeony root alcohol extract is 1:1 or 1:5, a step of; the compounding ratio of the celery seed volatile oil and the lithospermum alcohol extract is selected from 1:5.
After GC-MS detection, the celery seed volatile oil is found to be mainly composed of limonene, beta-caryophyllene and 4-ethyl propiophenone, and accounts for 84.79% of the total components. The limonene has good effects of antioxidation, bacteriostasis, whitening and the like; beta-caryophyllene can be used as a flavoring agent, and has anti-inflammatory, antibacterial, and antioxidant effects. In addition, the celery seed volatile oil also contains rich flavonoid compounds, and the compounds have good effects of resisting oxidation, whitening, resisting aging and the like; also contains linoleic acid, palmitic acid, etc., and has effects of promoting transdermal absorption, promoting skin microcirculation, and relieving inflammation.
The dandelion belongs to a plant for both medicine and food, has wide distribution and rich resources, and has the functions of clearing heat and relieving exterior syndrome, promoting urination and resolving hard mass, detumescence and detoxification, broad-spectrum bacteriostasis and the like. Various compounds such as phenolic acid, flavonoid, triterpene, coumarin, phytosterol, fatty acid and the like are separated from the extract, and the biological activities such as delaying aging, scavenging free radicals, diminishing inflammation, inhibiting bacteria and the like are found by researching the compounds such as the phenolic acid, the triterpene, the flavonoid and the like.
The radix Paeoniae Rubra contains various chemical components such as monoterpenes, phenolic acids, monoterpene glycosides, flavonoids, phenolic acids, proteins, etc. Modern pharmacological researches show that the radix paeoniae rubrathe has multiple effects of anticoagulation, anti-tumor, antibacterial, antioxidation, anti-inflammatory and the like.
Calendula officinalis belongs to a plant used as both medicine and food, contains a large amount of carotenoid and flavonoid substances, and further comprises various substances such as amino acid, fatty acid, coumarin, polysaccharide, volatile oil and the like; researches show that calendula officinalis has the effects of resisting inflammation, resisting oxidation, inhibiting bacteria, resisting aging, accelerating wound healing and the like.
Radix Arnebiae has multiple effects of cooling blood, promoting blood circulation, and removing toxic substances, and comprises shikonin, naphthoquinone, polysaccharide, fatty acid, flavonoid, phenolic acid, etc.; modern pharmacological researches show that lithospermum has the effects of resisting inflammation, resisting bacteria, resisting tumor, stopping bleeding and the like. Meanwhile, shikonin contained in lithospermum has the functions of resisting oxidization, inhibiting tyrosinase activity and the like, and can also be used as a food colorant.
The celery seed volatile oil and one or a mixture of the plant extract extracts are compounded for use, and the synergistic effect generated between the celery seed volatile oil and the plant extract extracts within a certain proportion range can realize the antioxidation and whitening effects of 1+1> 2.
Preferably, the celery seed volatile oil is prepared by steam distillation, and the specific steps are as follows:
soaking celery seeds in water, adding sodium chloride into the solution, and then placing the solution in an oil bath for extraction;
Transferring the solution into an oil-water separator, adding petroleum ether, collecting a petroleum ether layer after oil-water separation, removing water through anhydrous sodium sulfate, and volatilizing to remove petroleum ether to obtain the celery seed volatile oil.
Preferably, celery seeds are soaked in water for 1-3 hours; the adding amount of sodium chloride is 1-5% of the mass of the solution; the temperature of the oil bath is 120-135 ℃; the extraction time is 2-8h.
Preferably, the extracts of dandelion, red paeony root and lithospermum in the plant extract are alcohol extracts and are obtained by reflux extraction of ethanol;
The calendula extract in the plant extract is ethyl acetate extract phase, calendula alcohol extract is obtained by ethanol reflux extraction, and petroleum ether and ethyl acetate are sequentially extracted to obtain the calendula extract.
Preferably, the ethanol concentration adopted by the ethanol reflux extraction is 60-90%, the heating reflux temperature is 64-105 ℃ and the time is 1-3h.
The second aspect of the invention discloses a face cream containing a composition as described in any of the preceding claims, comprising the following components in weight percent:
Preferably, the emulsifier is selected from at least three of alkyl glycoside, laureth-7, beheneth-25 and polydimethylsiloxane.
Preferably, the emulsifier is prepared from alkyl glycoside, laureth-7, beheneth-25 and polydimethylsiloxane in an amount of 1:1:1:1 or 1:1:2:2, and mixing the materials according to the mass ratio.
The alkyl glycoside has good compatibility, can be compounded with other surfactants to generate a synergistic effect, and has good thickening property and skin compatibility; the polydimethylsiloxane has good air permeability, skin moisturizing property, chemical stability and the like, and has certain ultraviolet absorption resistance; laureth-7 has excellent skin tolerance and care effects; the behenyl alcohol polyether-25 has unique skin feel, long-acting moisture retention, excellent dispersing capability and the like. The four are used together to fully exert the function of the emulsifier and the effect of the emulsifier.
In a third aspect, the invention discloses a method of preparing a cream as described above, comprising the steps of:
S1: mixing and stirring an emulsifier, squalane, olive oil and castor oil uniformly under the water bath condition according to the formula amount to obtain a mixture A;
s2: mixing ultrapure water, glycerol, polyethylene glycol and 1, 3-butanediol according to the formula amount under the water bath condition, and stirring uniformly to obtain a mixture B;
S3: adding the mixture A obtained in the step S1 into the mixture B obtained in the step S2 for emulsification and continuing stirring;
s4: regulating the stirring rotation speed, and adding hydroxyethyl cellulose and xanthan gum according to the formula amount;
S5: adding the composition containing the celery seed volatile oil according to the formula amount, uniformly stirring, stopping heating, regulating the stirring rotation speed, and cooling to room temperature to obtain the face cream.
Preferably, the method comprises the steps of,
In the step S1, the heating temperature of the water bath is 75-85 ℃, and the stirring rotating speed is 400-500r/min;
In the step S2, the heating temperature of the water bath is 75-85 ℃, and the stirring rotating speed is 400-500r/min;
In the step S3, the stirring speed is 250-350r/min, the emulsifying temperature is 80-90 ℃ and the emulsifying time is 3-5min;
In the step S4, the stirring rotation speed is regulated to be 200-300r/min, and the time is 10-15min;
In the step S5, the stirring rotation speed is regulated to be 100-200r/min.
Compared with the prior art, the invention has the following beneficial effects:
(1) The preparation method of the celery seed volatile oil is a steam distillation method, takes water as a solvent, is environment-friendly, reduces pollution of an organic solvent, can reserve components of the volatile oil to a greater extent, and has higher safety; simple operation, low cost and strong feasibility.
(2) The main active ingredient of the face cream is natural plant extract, and is mild and nonirritating to skin. The celery seed has the functions of promoting penetration, removing edema, improving skin smoothness and the like; calendula has effects of whitening skin and resisting oxidation; herba Taraxaci has effects of resisting ultraviolet and skin allergy; radix Arnebiae has antiviral and anticancer effects; radix Paeoniae Rubra has radioprotective and antiaging effects; these plant extracts are safe and nontoxic and are all listed in the catalogue of cosmetic use. GC-MS component analysis and identification are carried out on the celery seed volatile oil to obtain that the main components of the celery seed volatile oil are limonene, beta-caryophyllene and 4-ethyl propiophenone, and the components have the effects of resisting oxidation, whitening, activating blood, inhibiting bacteria and the like. According to the invention, the celery seed volatile oil, dandelion alcohol extract, lithospermum alcohol extract, red paeony alcohol extract and calendula ethyl acetate are combined to research the effects of antioxidation, whitening and the like, and the composition is found to show a certain synergistic effect, and the effect is superior to any single substance.
According to the invention, the celery seed volatile oil composition is used as an effective substance, and the compound achieves better results in the aspects of biological activities such as synergistic whitening and antioxidation through reasonable compatibility, and meanwhile, the raw material cost is reduced. By measuring the antioxidant and whitening properties of the celery seed volatile oil composition, the composition is found to generate a synergistic effect within a certain proportion range, so that the antioxidant capacity and the inhibition of tyrosinase activity are further enhanced, the generation of melanin is effectively reduced, the skin is more effectively protected, and the skin aging is prevented; in addition, the celery seed volatile oil and each single substance also have certain antibacterial activity.
Detailed Description
The invention is described in detail below in connection with specific examples, but in no way limits the invention.
Unless otherwise specified in the examples below, the reagents used may be commercially available products which can be conventionally purchased by those skilled in the art, and the methods used may be conventional means in the art.
1. Preparation of dandelion alcohol extract
Heating herba Taraxaci and 75% ethanol at 105deg.C under reflux for 2 hr, vacuum filtering, concentrating, and evaporating ethanol to obtain herba Taraxaci ethanol extract.
2. Preparation of radix Paeoniae Rubra alcohol extract
Reflux-heating radix Paeoniae Rubra and 90% ethanol at 64deg.C for 2 hr, vacuum filtering, concentrating, and evaporating ethanol to obtain radix Paeoniae Rubra ethanol extract.
3. Preparation of lithospermum alcohol extract
Reflux-heating radix Arnebiae and 90% ethanol at 64deg.C for 2 hr, vacuum filtering, concentrating, and evaporating ethanol to obtain radix Arnebiae ethanol extract.
4. Preparation of calendula ethyl acetate phase
Reflux-heating calendula and 75% ethanol at 105deg.C for 2 hr, vacuum filtering, concentrating, and evaporating ethanol to obtain calendula ethanol extract. Dissolving the calendula alcohol extract with distilled water, sequentially extracting with equal amount of petroleum ether and ethyl acetate to obtain ethyl acetate extract phase, and selecting calendula ethyl acetate phase as the substance compounded with celery seed volatile oil.
5. Preparation of celery seed volatile oil
Mixing and soaking celery seed with deionized water for 3h, adding NaCl accounting for 3% of the solution mass, heating in an oil bath at 135 ℃ for 5h, adding a certain amount of petroleum ether into an oil-water separator, collecting a petroleum ether layer, adding anhydrous sodium sulfate to remove water, volatilizing petroleum ether to obtain yellow volatile oil, namely celery seed volatile oil, and storing at 4 ℃.
(1) DPPH free radical scavenging experiments
Mixing DPPH + solution with extract or celery seed volatile oil or compound, standing at room temperature in dark for 40min, taking out, measuring absorbance value at 517nm wavelength, and performing three experiments in parallel with BHT as positive control. The clearance rate calculation formula is: clearance (ESC,%) = [1- (a i-Aj)/Ac ] ×100%, where a i is the absorbance value of the sample solution+dpph + solution, a j is the absorbance value of the sample solution+absolute ethanol, and a c is the absorbance value of the absolute ethanol+dpph + solution, and the single substance scavenging results are shown in tables 1 and 2.
The concentrations of IC 50 were all: mg/mL.
Table 1 scavenging of DPPH radical by individual substances
TABLE 2 IC 50 values for DPPH radical scavenging for individual substances
| Substance (B) | IC50(mg/mL) |
| Celery seed essential oil | 9.58 |
| Taraxacum mongolicum ethanol extract | 0.098 |
| Radix Paeoniae Rubra alcohol extract | 0.033 |
| Lithospermum alcohol extract | 0.063 |
| Calendula ethyl acetate phase | 0.058 |
| BHT | 0.25 |
As can be seen from tables 1 and 2, the extracts have certain scavenging effect except that the celery seed volatile oil has no obvious scavenging effect on DPPH free radicals; from the IC 50 value of each extract, the oxidation resistance was successively from strong to weak: radix Paeoniae Rubra alcohol extract > calendula ethyl acetate phase > radix Arnebiae alcohol extract > herba Taraxaci alcohol extract > BHT > herba Apii Graveolentis seed volatile oil.
The compound formula is tested for DPPH free radical clearance rate, the compound concentration is 0.04mg/mL, and the results are shown in Table 3;
in the table, SE, the co-factor, is the ratio between the actual clearance or actual inhibition (ESC) and the theoretical clearance or theoretical inhibition (TSC) depending on the formulation, i.e.: SE = ESC/TSC;
The calculation formula of TSC is as follows: TSC (%) = (ESC 1+ESC2)-(ESC1×ESC2)/100;
Wherein: ESC is the actual clearance or actual inhibition of the compound, ESC 1 is the actual clearance or actual inhibition/% > of the celery seed essential oil, ESC 2 represents the actual clearance or actual inhibition/% > of the plant extract respectively;
When the synergy coefficient is more than 1, the compound has positive synergy; when the synergy coefficient=1, the compound appears to be additive; when the synergy coefficient is <1, the antagonism effect is obtained.
TABLE 3 scavenging Rate of DPPH free radical by Complex formulation of celery seed volatile oil
Note that: at 0.04mg/mL, the actual clearance of BHT to DPPH free radical is 7.89%, which is lower than the clearance of the compound in Table 3 to DPPH free radical, indicating that the clearance of the compound at the same concentration is better than that of the positive control BHT.
As can be seen from table 3, the combination of the celery seed volatile oil with dandelion alcohol extract, red peony alcohol extract, lithospermum alcohol extract and calendula ethyl acetate phase respectively has a certain synergistic effect on scavenging DPPH free radicals (SE is basically more than 1).
In a dandelion alcohol extract and celery seed volatile oil compound system, when the mass ratio of the dandelion alcohol extract is increased, the clearance rate of DPPH free radicals is gradually increased, and the synergistic coefficient is gradually increased. When the concentration of the compound and the concentration of the single substance are both 0.04mg/mL, the clearance rate of the compound to DPPH free radical is better than that of BHT at the same concentration, and the clearance rate is divided by 1: in addition, the clearance rate of the compound on DPPH free radicals is superior to that of single substances at the same concentration (see the actual clearance rate of the single substances with the concentration of 0.04mg/mL in the table 1, namely ESC), and presumably, the dandelion alcohol extract plays a main role in a compound system, so that the clearance rate can be increased along with the increase of the proportion of the dandelion alcohol extract.
In the compound system of the red paeony alcohol extract and the celery seed volatile oil, when the mass ratio of the red paeony alcohol extract is increased, the clearance rate is gradually increased, but the synergy coefficient is gradually reduced, and the antagonism effect can be possibly generated, which indicates that increasing the mass ratio of the red paeony alcohol extract in a proper amount can enhance the synergy effect, but the ratio is too large, the synergy effect is reduced, and even the antagonism effect can be possibly generated, so that a better value exists when the red paeony alcohol extract is adopted as the compound.
After the lithospermum alcohol extract and the celery seed volatile oil are compounded, the mass ratio of the lithospermum alcohol extract is increased, the clearance rate and the synergistic coefficient show a trend of increasing firstly and then decreasing, and when the lithospermum and the celery seed volatile oil are 13:1, the compound has no obvious synergistic effect; it is presumed that properly increasing the quality of the shikonin extract enhances the synergistic effect, but the mass ratio is too large and the synergistic effect is rather lowered, so that when the shikonin extract is used as a compound, a preferable value needs to be paid attention to.
After the calendula officinalis ethyl acetate phase and the celery seed volatile oil are compounded, the synergy coefficient is gradually reduced along with the increase of the mass ratio of the calendula officinalis ethyl acetate phase, but the actual clearance rate is gradually increased, when the concentration of the compound and the concentration of the single substance are both 0.04mg/mL, the clearance rate of the compound to DPPH free radical is superior to that of BHT and the respective single substance at the same concentration (see the actual clearance rate, namely ESC, of the concentration of the single substance is 0.04mg/mL in the table 1), and the compound system is presumed to possibly play a main role in the calendula officinalis ethyl acetate phase.
From tables 1 and 3, it is known that the scavenging effect of single calendula ethyl acetate phase and dandelion alcohol extract on DPPH free radical is lower than that of red paeony alcohol extract, and the synergistic effect of the single calendula ethyl acetate phase and dandelion alcohol extract on DPPH free radical scavenging rate after being compounded with celery seed volatile oil is stronger than that of the compound of red paeony root and celery seed volatile oil, which also shows that the antioxidant activity of single substance is better, but the synergistic effect of single substance and celery seed volatile oil after being compounded has a certain difference, which is possibly related to the molecular structure, acting force and the like among different components.
In the whole, the selected plant extract and celery seed volatile oil can have positive synergistic effect after being compounded, and the data result intuitively shows that the compound of dandelion alcohol extract, red paeony root alcohol extract, lithospermum alcohol extract, calendula ethyl acetate and celery seed volatile oil has synergistic effect in the aspect of eliminating DPPH free radicals.
(2) Tyrosinase inhibition assay
The experimental group reaction solution comprises PBS buffer solution, extract or celery seed volatile oil or its compound and tyrosinase solution, standing at room temperature for 10min, adding L-DOPA, mixing the solutions uniformly, reacting at room temperature for 15min, and measuring absorbance value at 475nm with a visible spectrophotometer. The arbutin is used as a positive control group for three experiments in parallel. The inhibition rate calculation formula is: inhibition ratio (ESC,%) = { [ (a-B) - (C-D) ]/(a-B) } ×100%, wherein a is absorbance value with tyrosinase without extract; b is the absorbance value of tyrosinase-free and extract-free; c is absorbance value of tyrosinase with extract; d is the absorbance value of the extract without tyrosinase. The results of the tyrosinase activity test for each individual material are shown in tables 4 and 5.
TABLE 4 inhibition of tyrosinase activity by individual substances
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TABLE 5 IC 50 values for tyrosinase activity for individual substances
| Substance (B) | IC50(mg/mL) |
| Celery seed essential oil | 0.87 |
| Taraxacum mongolicum ethanol extract | 1.97 |
| Radix Paeoniae Rubra alcohol extract | 0.78 |
| Lithospermum alcohol extract | 0.68 |
| Calendula ethyl acetate phase | 1.43 |
| Arbutin | 2.16 |
As can be seen from tables 4 and 5, the extracts have good inhibition effect, and the IC 50 values are lower than the positive control arbutin; from the IC 50 values of the respective extracts, the inhibition of tyrosinase activity was from strong to weak: radix Arnebiae alcohol extract > radix Paeoniae Rubra alcohol extract > herba Apii Graveolentis seed volatile oil > calendula officinalis ethyl acetate phase > herba Taraxaci alcohol extract > arbutin.
The inhibition test of tyrosinase activity was performed on the formulated formulation, the concentration of the compound was 0.4mg/mL, and the results are shown in Table 6.
TABLE 6 inhibition of tyrosinase activity by formulated formulation of celery seed essential oil
Note that: at 0.4mg/mL, the actual inhibition rate of the arbutin to the tyrosinase activity is 16.93 percent, which is lower than the inhibition effect of the compound in Table 6 to the tyrosinase activity, and the inhibition effect of the compound with the same concentration is superior to that of the positive control arbutin.
Table 6 shows that the compound of the celery seed volatile oil and dandelion alcohol extract, red peony root alcohol extract, lithospermum alcohol extract and calendula ethyl acetate phase respectively has synergistic effect on inhibiting tyrosinase activity.
In the dandelion alcohol extract and celery seed volatile oil compound system, as the mass ratio of the dandelion alcohol extract is increased, the synergistic coefficient is sequentially 1.20, 1.08 and 0.96, which shows that the synergistic effect of the dandelion alcohol extract and the celery seed volatile oil is gradually weakened, and a certain antagonism can exist after the dandelion alcohol extract and the celery seed volatile oil are increased to a certain proportion, so that the compound system needs to pay attention to the proportion range.
In a compound system of the red paeony root alcohol extract and the celery seed volatile oil, the compound mass ratio is 1:1, the preparation method has a good synergistic effect, increases the mass ratio of the red paeony root alcohol extract, and reduces the synergistic effect; from table 5, it can be seen that the radix paeoniae rubra alcohol extract with better enzyme inhibition effect is similar to the inhibition effect of the celery seed volatile oil on tyrosinase activity, and after the radix paeoniae rubra alcohol extract and the celery seed volatile oil are compounded, the mass ratio of any species is increased, so that the synergistic effect of a compounding system is probably reduced.
In the complex system of the lithospermum alcohol extract with better enzyme inhibition effect and the celery seed volatile oil, the mass ratio of the lithospermum alcohol extract is increased, the synergistic coefficient is 1.07, 1.08 and 1.06, the synergistic effect is not obvious, and the complex system is presumed to be possible to play a main role in the celery seed volatile oil.
In the calendula officinalis ethyl acetate and celery seed volatile oil compound system, the mass ratio of the calendula officinalis ethyl acetate phase is increased, and the synergistic effect is gradually reduced, which is possibly related to that the activity of the calendula officinalis ethyl acetate phase is lower than that of the celery seed volatile oil.
According to the data result, the dandelion alcohol extract, the red paeony root alcohol extract, the lithospermum alcohol extract, the calendula officinalis ethyl acetate phase and the celery seed volatile oil compound have a certain synergistic effect on inhibiting tyrosinase activity.
(3) Bacteriostasis experiment
The experiment adopts a paper sheet diffusion method to measure the antibacterial activity of 5 single substances on common strains. And (3) regulating the concentration of the bacterial suspension by using sterilized normal saline, and uniformly coating the prepared bacterial suspension on the surface of a culture medium flat plate. A sterilized 6mm round filter paper sheet is placed in the middle of a culture dish, a sample with the concentration of 25mg/mL, DMSO and positive control streptomycin sulfate with the concentration of 1mg/mL are respectively dripped on the filter paper sheet, the culture dish is inverted, and the culture dish is placed in a culture box at 37 ℃ for culture for 24 hours. And taking out the culture dish, measuring the diameters of the bacteriostasis ring in two vertical directions by using a vernier caliper by adopting a crisscross method, and taking an average value (mm) as a measurement result in three times of each experiment. The larger the inhibition zone, the stronger the antibacterial activity. Evaluation criteria of antibiotic inhibition zone experimental results: the diameter of the inhibition zone is larger than 15mm and is highly sensitive, 10-15mm (excluding 10mm and including 15 mm) is moderately sensitive, 6-10mm (excluding 6mm and including 10 mm) is lowly sensitive, and no inhibition zone (6 mm) indicates insensitivity. The test results are shown in Table 7.
Table 7 bacteriostatic Activity of individual substances against common species
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Note that: "-" indicates no bacteriostasis effect, i.e. the bacteriostasis circle is less than or equal to 6mm.
As can be seen from table 7, the celery seed volatile oil has no obvious inhibition effect on escherichia coli, has a certain inhibition effect on staphylococcus aureus, the lithospermum alcohol extract has no inhibition effect on escherichia coli and staphylococcus aureus, and other substances have inhibition effect on escherichia coli and staphylococcus aureus, but are lower than positive control streptomycin sulfate. In addition to the red peony alcohol extract, these extracts are more sensitive to staphylococcus aureus than escherichia coli.
The following examples are related to creams:
Example 1
A synergistic antioxidation and whitening cream containing celery seed volatile oil composition mainly comprises the following components in percentage by weight: 0.6% of calendula ethyl acetate phase, 0.6% of celery seed volatile oil, 1% of alkyl glycoside and laureth-7: 1%, behenpolyether-25: 1% of polydimethylsiloxane, 1.5% of squalane, 1% of olive oil, 1% of castor oil, 3% of glycerin, 2% of polyethylene glycol, 1, 3-butanediol, 1% of hydroxyethyl cellulose, 0.5% of xanthan gum and 83.8% of ultrapure water. The preparation method comprises the following steps:
(1) According to the mass percentage, alkyl glycoside, laureth-7, behenpolyether-25, polydimethylsiloxane, squalane, olive oil and castor oil are heated to 80 ℃ in a water bath under the condition of 400r/min, and are dissolved uniformly, and the mixture is kept warm for standby, and is marked as A;
(2) Heating ultrapure water, glycerol, polyethylene glycol and 1, 3-butanediol to 80 ℃ in a water bath under the condition of 450r/min according to the mass percentage, dissolving uniformly, preserving heat for standby, and marking as B;
(3) Pouring the substance A into the substance B rapidly, continuously stirring at a rotating speed of 300r/min, and emulsifying for 3min at 85 ℃;
(4) Adjusting the rotating speed to 250r/min, continuously stirring for 10min, and adding hydroxyethyl cellulose and xanthan gum according to mass percent;
(5) Adding the celery seed volatile oil composition according to the mass percentage, stopping heating after stirring uniformly, adjusting the rotating speed to 150r/min, and cooling to room temperature to obtain the antioxidant whitening cream containing the celery seed volatile oil composition.
Example 2
The difference with the embodiment 1 is that the synergistic antioxidation and whitening cream containing the celery seed volatile oil composition mainly comprises the following components in percentage by weight: 1% of dandelion alcohol extract, 1% of celery seed volatile oil, 0.5% of alkyl glycoside and 7% of laureth: 0.5%, behenol polyether-25: 1% of polydimethylsiloxane, 1.5% of squalane, 1% of olive oil, 1% of castor oil, 3% of glycerin, 2% of polyethylene glycol, 1, 3-butanediol, 1.5% of hydroxyethyl cellulose, 0.8% of xanthan gum and 83.2% of ultrapure water.
Example 3
The difference with the embodiment 1 is that the synergistic antioxidation and whitening cream containing the celery seed volatile oil composition mainly comprises the following components in percentage by weight: 0.5% of lithospermum alcohol extract, 0.5% of celery seed volatile oil, 1% of alkyl glycoside and laureth-7: 1%, behenpolyether-25: 2% of polydimethylsiloxane, 2% of squalane, 1.5% of olive oil, 2% of castor oil, 3% of glycerin, 2% of polyethylene glycol, 1, 3-butanediol, 1% of hydroxyethyl cellulose, 0.5% of xanthan gum and 80% of ultrapure water.
Example 4
The difference with the embodiment 1 is that the synergistic antioxidation and whitening cream containing the celery seed volatile oil composition mainly comprises the following components in percentage by weight: 0.3% of red paeony root alcohol extract, 0.3% of celery seed volatile oil, 1% of alkyl glycoside and laureth-7: 1%, behenpolyether-25: 2% of polydimethylsiloxane, 1.5% of squalane, 1% of olive oil, 1% of castor oil, 4% of glycerin, 3% of polyethylene glycol, 2% of 1, 3-butanediol, 1% of hydroxyethyl cellulose, 0.5% of xanthan gum and 79.4% of ultrapure water.
(4) Sensory evaluation and shelf life observation of the creams:
the creams of examples 1-4 were evaluated separately using a sensory evaluation method. The population of subjects was 15 females, aged between 20 and 50 years, with healthy skin and no history of dermatological allergies. The evaluation index is as follows:
1) Fine feel: whether the face cream is soft or soft when being smeared or not, and whether the face cream has granular feel or not;
2) Spreadability: whether the face cream is easy to push away in the smearing process;
3) Freshness degree: whether the cream has greasy feeling after being smeared;
4) Moistening property: after the face cream is smeared, whether the face can feel moist or not;
5) Acceptance degree: the odor, color, touch, etc. of the cream can be accepted at the time of and after use.
The evaluation criteria were scored from 0 to 5 points, with 0 being the worst and 5 being the best. The results are summarized in Table 8, where the evaluation scores are averaged.
TABLE 8 evaluation of skin feel for examples 1-4
| Fine and smooth feeling | Spreadability of coating | Fresh and cool degree | Moistening property | Acceptance degree | |
| Example 1 | 4.7 | 4.7 | 4.9 | 4.6 | 4.8 |
| Example 2 | 4.8 | 4.8 | 4.8 | 4.7 | 4.6 |
| Example 3 | 4.6 | 4.8 | 4.7 | 4.9 | 4.7 |
| Example 4 | 4.9 | 4.6 | 4.9 | 4.8 | 4.8 |
Therefore, the face cream formula provided by the invention has good use experience, is moist but not sticky, is mild and has no stimulation.
Surface 9 results of determination of partial physicochemical Properties of the creams
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Note that: the color appearance, fragrance, stability, cold resistance, heat resistance and shelf life of the prepared cream are detected according to the current industry standard QB/T1857-2013 skin-care cream.
Table 9 several physical and chemical properties common to creams were tested, wherein the blank was a formulation supplemented with ultrapure water after removal of the extract and celery seed volatile oil (i.e. the composition containing celery seed volatile oil); the preparation procedure was as provided in example 1.
By analyzing tables 8 and 9 and further combining tables 1 to 7, it is known that the addition of the relevant composition on the basis of the base formulation of the cream can provide a cream having good safety and whitening and antioxidative properties. The shelf life of the cream after adding the composition is relatively prolonged, which may be related to the composition containing the functional components of antioxidation, bacteriostasis, etc.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (5)
1. A composition containing celery seed volatile oil, which is characterized in that the ratio of celery seed volatile oil to plant extract is 1:0.1 to 30 mass ratio;
The plant extract is one or more of calendula, dandelion, red paeony root and lithospermum;
The celery seed volatile oil is prepared by steam distillation, and the specific steps are as follows: soaking celery seeds in water, adding sodium chloride into the solution, and then placing the solution in an oil bath for extraction; transferring the solution into an oil-water separator, adding petroleum ether, collecting a petroleum ether layer after oil-water separation, removing water through anhydrous sodium sulfate, and volatilizing to remove petroleum ether to obtain celery seed volatile oil; wherein, the celery seeds are soaked in water for 1-3h; the adding amount of sodium chloride is 1-5% of the mass of the solution; the temperature of the oil bath is 120-135 ℃; the extraction time is 2-8h
The extracts of dandelion, red paeony root and lithospermum in the plant extract are alcohol extracts and are obtained by reflux extraction of ethanol; the calendula extract in the plant extract is ethyl acetate extract phase, and is obtained by extracting calendula alcohol extract through ethanol reflux, and then sequentially extracting with petroleum ether and ethyl acetate; wherein the ethanol concentration adopted by the ethanol reflux extraction is 60-90%, the heating reflux temperature is 64-105 ℃ and the time is 1-3h.
2. A cream comprising the composition of claim 1, comprising the following components in weight percent:
0.1-7% of a composition containing celery seed volatile oil;
2.5-10% of emulsifying agent;
0.5-3% of squalane;
0.5-3% of olive oil;
0.5-3% of castor oil;
glycerol 1-6%;
polyethylene glycol 1-6%;
1-3% of 1, 3-butanediol;
0.1-2% of hydroxyethyl cellulose;
0.1-1% of xanthan gum;
ultrapure water balance;
The emulsifier is at least three selected from alkyl glycoside, laureth-7, beheneth-25 and polydimethylsiloxane.
3. A cream according to claim 2, wherein the emulsifier is selected from the group consisting of alkyl glycosides, laureth-7, behenpolyether-25 and dimethicone at 1:1:1:1 or 1:1:2:2, and mixing the materials according to the mass ratio.
4. A method of preparing a cream as claimed in any one of claims 2 to 3, comprising the steps of:
S1: mixing and stirring an emulsifier, squalane, olive oil and castor oil uniformly under the water bath condition according to the formula amount to obtain a mixture A;
s2: mixing ultrapure water, glycerol, polyethylene glycol and 1, 3-butanediol according to the formula amount under the water bath condition, and stirring uniformly to obtain a mixture B;
S3: adding the mixture A obtained in the step S1 into the mixture B obtained in the step S2 for emulsification and continuing stirring;
s4: regulating the stirring rotation speed, and adding hydroxyethyl cellulose and xanthan gum according to the formula amount;
S5: adding the composition containing the celery seed volatile oil according to the formula amount, uniformly stirring, stopping heating, regulating the stirring rotation speed, and cooling to room temperature to obtain the face cream.
5. A method of preparing a facial cream according to claim 4,
In the step S1, the heating temperature of the water bath is 75-85 ℃, and the stirring rotating speed is 400-500r/min;
In the step S2, the heating temperature of the water bath is 75-85 ℃, and the stirring rotating speed is 400-500r/min;
In the step S3, the stirring speed is 250-350 r/min, the emulsifying temperature is 80-90 ℃ and the emulsifying time is 3-5min;
In the step S4, the stirring rotation speed is regulated to be 200-300r/min, and the time is 10-15min;
In the step S5, the stirring rotation speed is regulated to be 100-200 r/min.
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