CN115463055A - 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 PDF

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CN115463055A
CN115463055A CN202211313485.0A CN202211313485A CN115463055A CN 115463055 A CN115463055 A CN 115463055A CN 202211313485 A CN202211313485 A CN 202211313485A CN 115463055 A CN115463055 A CN 115463055A
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volatile oil
celery seed
seed volatile
cream
oil
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吴颖
王双旦
唐文
张蓓婷
刘晴
宋新玮
谷翀
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Shanghai Institute of Technology
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
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    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005Antimicrobial preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61Q19/00Preparations for care of the skin
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    • A61K2800/78Enzyme modulators, e.g. Enzyme agonists
    • A61K2800/782Enzyme inhibitors; Enzyme antagonists
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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Abstract

The invention relates to an antioxidant and whitening cosmetic, in particular to a composition containing celery seed volatile oil, a face cream and a preparation method of the face cream, wherein the weight ratio of the celery seed volatile oil to a plant extract is 1:0.1-30 by mass ratio; the plant extract is one or more of calendula, dandelion, red peony root and lithospermum. Compared with the prior art, the invention provides a new formula containing the celery seed volatile oil for the anti-oxidation 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

Composition containing celery seed volatile oil, facial cream and preparation method of facial cream
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, various researches find that certain herbal plant extracts can achieve the effect of repairing or beautifying the skin through metabolism after acting on the skin.
Plant volatile oil is widely researched due to the excellent characteristics of no toxicity, many functional components, greenness, no pollution and the like. The celery seed volatile oil is a light yellow oil substance extracted from celery seed, can be used as both medicine and food, has unique fresh fragrance, and has effects of removing edema, promoting skin smoothness, increasing blood flow, lowering blood pressure, improving cerebral microcirculation, etc. The celery seed essential oil has the functions of oxidation resistance, tumor resistance, bacteriostasis and the like, and can be applied to the fields of food, beauty cosmetics, health products, medicines and the like.
At present, many researchers research on the anti-oxidation and whitening of the compounding of various Chinese herbal medicines, but the research is only simple superposition of some effects, deep excavation and research are not carried out, and the expected effect is difficult to achieve; even the compounding of different species in some formulas can generate antagonism, thereby reducing the efficacy performance of the compound, wasting raw materials and further increasing the product cost. Therefore, how to develop an efficient, safe and stable synergistic antioxidant and whitening skin care product is still a difficult point.
The invention provides a compound formula containing celery seed volatile oil, which has synergistic antioxidant and whitening effects.
Disclosure of Invention
The invention aims to solve at least one of the problems, provides a composition containing celery seed volatile oil, a cream and a preparation method of the cream, provides a new formula containing the celery seed volatile oil for an anti-oxidation 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.
The purpose of the invention is realized by the following technical scheme:
the invention discloses a composition containing celery seed volatile oil, which is prepared by mixing celery seed volatile oil and plant extract according to the weight ratio of 1:0.1-30 by mass ratio;
the plant extract is one or more of calendula, dandelion, red peony root and lithospermum.
Further preferably, the ratio of the celery seed volatile oil to the plant extract is 1:0.5-20 by mass ratio.
More preferably, the compounding ratio of the celery seed volatile oil to the calendula officinalis ethyl acetate phase can be 1:1 or 1:5 or 1:9; the compounding proportion of the celery seed volatile oil and the dandelion alcohol extract can be selected from 1:5; the compounding proportion of the celery seed volatile oil and the red paeony root alcohol extract can be selected from 1:1 or 1:5; the compounding proportion of the celery seed volatile oil and the lithospermum alcohol extract can be selected from 1:5.
after GC-MS detection, the celery seed volatile oil is found to have main components of limonene, beta-caryophyllene and 4-ethyl propiophenone, and accounts for 84.79% of the total components. The limonene has good effects of resisting oxidation, inhibiting bacteria, whitening and the like; the beta-caryophyllene can be used as flavoring agent, and has antiinflammatory, antibacterial, and antioxidant effects. In addition, the celery seed volatile oil also contains abundant flavonoid compounds, and the compounds have better effects of oxidation resistance, whitening, aging resistance and the like; also contains linoleic acid, palmitic acid, etc., and has effects of promoting percutaneous absorption, promoting skin microcirculation, and resisting inflammation.
The dandelion belongs to a plant used as both medicine and food, has wide distribution and rich resources, and has the functions of clearing heat, relieving exterior syndrome, promoting urination, resolving hard mass, relieving swelling, detoxifying, inhibiting bacteria in a broad spectrum and the like. At present, various compounds such as phenolic acids, flavonoids, triterpenes, coumarins, phytosterols, fatty acids and the like are separated from the extract of the plant, and researches show that the compounds such as the phenolic acids, the triterpenes, the flavonoids and the like have biological activities of delaying senility, eliminating free radicals, diminishing inflammation, inhibiting bacteria and the like.
Radix Paeoniae Rubra contains various chemical components such as monoterpene, phenolic acids, monoterpene glycosides, flavonoids, phenolic acids, proteins, etc. Modern pharmacological research shows that red peony root has multiple effects of anticoagulation, anti-tumor, antibiosis, antioxidation, anti-inflammation 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 also comprises various substances such as amino acid, fatty acid, coumarin, polysaccharide, volatile oil and the like; researches show that the calendula officinalis has the effects of resisting inflammation, resisting oxidation, inhibiting bacteria, resisting aging, accelerating wound healing and the like.
The lithospermum has multiple effects of cooling blood, promoting blood circulation, detoxifying and the like, and the main chemical components comprise alkannin, naphthoquinones, polysaccharides, fatty acids, flavonoids, phenolic acids and other substances; modern pharmacological research shows that the lithospermum has the effects of resisting inflammation, resisting bacteria, resisting tumors, stopping bleeding and the like. Meanwhile, shikonin contained in Lithospermum erythrorhizon has effects of resisting oxidation and inhibiting tyrosinase activity, and can also be used as food colorant.
The celery seed volatile oil and one or a mixture of the plant extract are compounded for use, and the synergistic effect generated between the celery seed volatile oil and the plant extract in a certain proportion range can realize the antioxidant and whitening effects of 1+1 >2.
Preferably, the celery seed volatile oil is prepared by a steam distillation method, 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 to an oil-water separator, adding petroleum ether, performing oil-water separation, collecting a petroleum ether layer, removing water through anhydrous sodium sulfate, and volatilizing to remove the petroleum ether to obtain the celery seed volatile oil.
Preferably, 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.
Preferably, the extracts of dandelion, red peony root and lithospermum in the plant extract are alcohol extracts, and are obtained by ethanol reflux extraction;
the calendula extract in the plant extract is an ethyl acetate extract phase, and is obtained by ethanol reflux extraction and sequential extraction of petroleum ether and ethyl acetate.
Preferably, the ethanol reflux extraction adopts 60-90% ethanol concentration, heating reflux temperature is 64-105 deg.C, and time is 1-3h.
The invention discloses a face cream containing the composition as described in any one of the above, which comprises the following components in percentage by weight:
Figure BDA0003908016980000031
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 a ratio of 1:1:1:1 or 1:1:2:2 by 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 moistening property, chemical stability and the like, and has certain ultraviolet resistance and absorption capacity; the laureth-7 has excellent skin tolerance and care effect; behenyl alcohol polyether-25 has unique skin feeling, long-acting moisture keeping, excellent dispersing capacity, etc. The combination of the four can fully exert the function of the emulsifier and the effect of the emulsifier.
In a third aspect, the invention discloses a method for preparing a cream as described above, comprising the steps of:
s1: mixing and stirring emulsifier, squalane, olive oil and castor oil uniformly under the condition of water bath 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 uniformly stirring 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: adjusting the stirring 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, stirring uniformly, stopping heating, adjusting the stirring speed and cooling to room temperature to obtain the face cream.
Preferably, the first and second electrodes are formed of a metal,
in the step S1, the heating temperature of the water bath is 75-85 ℃, and the stirring speed is 400-500r/min;
in the step S2, the heating temperature of the water bath is 75-85 ℃, and the stirring speed is 400-500r/min;
in the step S3, the stirring speed is 250-350r/min, the emulsifying temperature is 80-90 ℃, and the time is 3-5min;
in the step S4, the stirring speed is adjusted to be 200-300r/min, and the time is 10-15min;
in step S5, the stirring speed is adjusted to 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, water is used as a solvent, the method is green and environment-friendly, the pollution of an organic solvent is reduced, the components of the volatile oil can be reserved to a greater extent, and the safety is higher; simple operation, low cost and strong feasibility.
(2) The main active component of the facial cream is natural plant extract, and the facial cream is mild and non-irritant to skin. The celery seeds have the effects of promoting penetration, removing edema, improving skin smoothness and the like; calendula officinalis has whitening and antioxidant effects; herba Taraxaci has effects of resisting ultraviolet and skin allergy; radix Arnebiae has antiviral and anticancer effects; radix Paeoniae Rubra has effects of resisting radiation and delaying aging; these plant extracts are safe and non-toxic and have been included in the cosmetic application list. GC-MS component analysis and identification are carried out on the celery seed volatile oil, so 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, promoting blood circulation, inhibiting bacteria and the like. According to the invention, the celery seed volatile oil, the dandelion alcohol extract, the lithospermum alcohol extract, the red peony root alcohol extract and the calendula ethyl acetate are combined to study the effects of antioxidation, whitening and the like, and the composition shows a certain synergistic effect, and the effect is superior to that of any single substance.
According to the invention, the celery seed volatile oil composition is adopted as an effective substance, and the compound obtains better results in the aspects of biological activities such as synergistic whitening, antioxidation and the like through reasonable compatibility, and meanwhile, the raw material cost is reduced. Through measuring the oxidation resistance and the whitening performance of the celery seed volatile oil composition, the composition can generate a synergistic effect in a certain proportion range, and further enhance the oxidation resistance and the inhibition on the activity of tyrosinase, so that the generation of melanin is effectively reduced, the skin is effectively protected, and the skin aging is prevented; in addition, the celery seed volatile oil and each single substance also have certain bacteriostatic activity.
Detailed Description
The present invention will now be described in detail with reference to specific examples, but the present invention is by no means limited thereto.
In the following examples, unless otherwise specified, reagents used may be commercially available products which can be routinely obtained by those skilled in the art, and the methods used may be those conventional in the art.
1. Preparation method of alcohol extract of herba Taraxaci
Heating and refluxing herba Taraxaci and 75% ethanol at 105 deg.C for 2 hr, vacuum filtering, concentrating, and evaporating to remove ethanol to obtain herba Taraxaci ethanol extract.
2. Preparation of red peony root alcohol extract
Reflux extracting radix Paeoniae Rubra with 90% ethanol at 64 deg.C for 2 hr, vacuum filtering, concentrating, and evaporating to remove ethanol to obtain radix Paeoniae Rubra ethanol extract.
3. Preparation of alkanna tinctoria alcohol extract
Heating radix Arnebiae and 90% ethanol at 64 deg.C under reflux for 2 hr, vacuum filtering, concentrating, and evaporating to remove ethanol to obtain radix Arnebiae ethanol extract.
4. Preparation of calendula officinalis ethyl acetate phase
Heating and refluxing calendula officinalis and 75% ethanol at 105 deg.C for 2 hr, vacuum filtering, concentrating, and evaporating to remove ethanol to obtain calendula officinalis ethanol extract. Dissolving the obtained calendula alcohol extract with distilled water, sequentially extracting with petroleum ether and ethyl acetate in equal amount to obtain an ethyl acetate extract phase, and selecting the calendula ethyl acetate phase as a substance compounded with the celery seed volatile oil.
5. Preparation of celery seed volatile oil
Soaking semen Apii Graveolentis in deionized water for 3h, adding NaCl 3% of the solution, heating in oil bath at 135 deg.C for 5h, adding petroleum ether, collecting petroleum ether layer, adding anhydrous sodium sulfate to remove water, volatilizing petroleum ether to obtain yellow volatile oil, and storing at 4 deg.C.
(1) DPPH free radical scavenging experiment
DPPH + Mixing the solution with the extract or the volatile oil or the compound of celery seed uniformly, standing at room temperature in the dark for 40min, taking out, measuring the absorbance value at the wavelength of 517nm, and carrying out three experiments in parallel by taking BHT as a positive control. The clearance calculation formula is: clearance (ESC,%) = [1- (a) i -A j )/A c ]X 100%, wherein A i Is the sample solution + DPPH + Absorbance value of the solution; a. The j The absorbance value of the sample solution plus absolute ethyl alcohol is obtained; a. The c Is absolute ethyl alcohol + DPPH + Absorbance value of the solution. The results of DPPH radical scavenging by each single substance are shown in tables 1 and 2.
IC 50 The concentrations of (A) are as follows: mg/mL.
TABLE 1 DPPH radical scavenging ratio of the individual substances
Figure BDA0003908016980000061
Figure BDA0003908016980000071
TABLE 2 IC for DPPH radical scavenging by individual substances 50 Value of
Substance(s) IC 50 (mg/mL)
Celery seed volatile oil 9.58
Alcohol extract of dandelion 0.098
Radix Paeoniae Rubra alcohol extract 0.033
Alcoholic extract of radix Arnebiae 0.063
Calendula officinalis ethyl acetate phase 0.058
BHT 0.25
As can be seen from tables 1 and 2, the celery seed volatile oil has a certain scavenging effect except that the celery seed volatile oil has no obvious scavenging effect on DPPH free radicals; IC from each extract 50 The oxidation resistance is shown as follows from strong to weak: alcohol extract of red peony root>Calendula officinalis ethyl acetate phase>Alcoholic extract of radix Arnebiae>Alcohol extract of dandelion>BHT>Volatile oil of semen Apii Graveolentis.
The compound formula is tested for the clearance rate of DPPH free radicals, the concentration of the compound is 0.04mg/mL, and the result is shown in Table 3;
in the table, SE, i.e. the synergy factor, depends on the ratio between the actual clearance or inhibition (ESC) and the theoretical clearance or inhibition (TSC) obtained for the formulation, i.e.: SE = ESC/TSC;
the formula for calculating TSC is as follows: TSC (%) = (ESC) 1 +ESC 2 )-(ESC 1 ×ESC 2 )/100;
In the formula: ESC is the actual clearance or inhibition of the formulation, ESC 1 The ESC is the actual clearance rate or the actual inhibition rate/%, of the celery seed volatile oil 2 Represents the actual clearance or actual inhibition/%, respectively, of the plant extract;
when the synergistic coefficient is greater than 1, the compound has positive synergistic effect; when the synergistic coefficient =1, the compound shows additive effect; when the synergistic coefficient is less than 1, the effect is antagonistic.
TABLE 3 elimination of DPPH free radical by the formulation of the celery seed volatile oil
Figure BDA0003908016980000081
Figure BDA0003908016980000091
Note: at 0.04mg/mL, the actual clearance of the BHT on DPPH free radicals was 7.89%, which is lower than the clearance of the DPPH free radicals by the compound in Table 3, 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 the alcohol extract of dandelion, the alcohol extract of red peony root, the alcohol extract of lithospermum and the ethanol acetate of calendula has a certain synergistic effect (SE is basically more than 1) on eliminating DPPH free radicals.
In a compound system of the dandelion alcohol extract and the celery seed volatile oil, 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 single substance is 0.04mg/mL, the clearance rate of the compound to DPPH free radicals is better than that of BHT under the same concentration, except that 1: in addition, the clearance rate of the compound on DPPH free radicals is better than that of a single substance under the same concentration (see the actual clearance rate, namely ESC, of the single substance concentration of 0.04mg/mL in Table 1), and it is supposed that the dandelion alcohol extract plays a main role in the compound system, so that the clearance rate is increased along with the increase of the proportion of the dandelion alcohol extract.
In a compound system of the red paeony root alcohol extract and the celery seed volatile oil, when the mass ratio of the red paeony root alcohol extract is increased, the clearance rate is gradually increased, but the synergistic coefficient is gradually reduced, and an antagonistic effect is likely to appear, which indicates that the synergistic effect is enhanced by properly increasing the mass ratio of the red paeony root alcohol extract, but the ratio is too large, the synergistic effect is reduced, and the antagonistic effect is likely to appear, so that a better value exists when the red paeony root 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 the trend of increasing firstly and then decreasing, and when the lithospermum and the celery seed volatile oil are 13: when 1, the compound has no obvious synergistic effect; it is presumed that the synergistic effect is enhanced by properly increasing the mass of the alcohol extract of lithospermum, but the synergistic effect is rather reduced by an excessive mass ratio, so that when the alcohol extract of lithospermum is used as a compound, a better value needs to be paid attention to.
After the calendula acetic ether phase and the celery seed volatile oil are compounded, the synergistic coefficient is gradually reduced along with the mass ratio of the calendula acetic ether phase, but the actual clearance rate is gradually increased, and when the concentrations of the compound and the single substance are both 0.04mg/mL, the clearance rate of the compound on DPPH free radicals is superior to that of BHT and the respective single substance under the same concentration (see the actual clearance rate that the concentration of the single substance in the table 1 is 0.04mg/mL, namely ESC), and the compounded system is presumed to possibly play a main role in the calendula acetic ether phase.
It can be seen from tables 1 and 3 that the single ethanol acetate phase of calendula and the single ethanol extract of dandelion has a lower effect of scavenging DPPH free radicals than the ethanol extract of red peony root, and the synergistic effect of the single ethanol extract of calendula and the ethanol extract of dandelion is stronger than the synergistic effect of the single ethanol extract of red peony root and the ethanol extract of celery seed in terms of scavenging DPPH free radicals after being compounded with the volatile oil of celery seed.
Overall, after the selected plant extract and the celery seed volatile oil are compounded, positive synergistic effects can be achieved, and data results show that the compound of the dandelion alcohol extract, the red peony root alcohol extract, the lithospermum alcohol extract, the calendula ethyl acetate phase and the celery seed volatile oil has a synergistic effect in the aspect of removing DPPH free radicals.
(2) Tyrosinase inhibition assay
The reaction solution of the experimental group comprises PBS buffer solution, extract or celery seed volatile oil or compound thereof and tyrosinase solution, after standing for 10min at room temperature, adding L-DOPA, mixing the solutions uniformly, reacting for 15min at room temperature, and measuring the absorbance value at 475nm by using a visible spectrophotometer. Three experiments were performed in parallel with arbutin as a positive control. The inhibition rate calculation formula is as follows: inhibition (ESC,%) = { [ (A-B) - (C-D) ]/(A-B) } × 100%, where A is the absorbance value with tyrosinase and without extract; b is the absorbance value of the extract without tyrosinase; c is the absorbance value of the extract containing tyrosinase; d is the absorbance value with or without tyrosinase in the presence of the extract. The results of the tyrosinase activity test for each individual substance are shown in tables 4 and 5.
TABLE 4 inhibition of tyrosinase Activity by Individual substances
Figure BDA0003908016980000111
Figure BDA0003908016980000121
TABLE 5 IC for tyrosinase activity for each individual substance 50 Value of
Substance(s) IC 50 (mg/mL)
Celery seed volatile oil 0.87
Alcohol extract of dandelion 1.97
Alcohol extract of red peony root 0.78
Alcoholic extract of radix Arnebiae 0.68
Calendula officinalis ethyl acetate phase 1.43
Arbutin 2.16
As can be seen from tables 4 and 5, the extracts both have a good inhibitory effect, IC 50 The values are all lower than those of the positive control arbutin; IC from each extract 50 The values show that the tyrosinase activity is inhibited from strong to weak: radix Arnebiae alcohol extract>Radix Paeoniae Rubra alcohol extract>Celery seed volatile oil>Calendula officinalis ethyl acetate phase>Alcohol extract of dandelion>Arbutin.
The tyrosinase activity inhibition test was performed on the formulated formulations, and the concentrations of the formulations were all 0.4mg/mL, with the results shown in Table 6.
TABLE 6 inhibition of tyrosinase Activity by the Complex formulation of celery seed volatile oil
Figure BDA0003908016980000122
Figure BDA0003908016980000131
Note: at 0.4mg/mL, the actual inhibition rate of arbutin on tyrosinase activity is 16.93%, which is lower than the inhibition effect of the compound in Table 6 on tyrosinase activity, indicating that the inhibition effect of the compound with the same concentration on the tyrosinase activity is better than that of the positive control arbutin.
As can be seen from Table 6, the combination of the celery seed volatile oil and the dandelion alcohol extract, the red peony root alcohol extract, the lithospermum alcohol extract and the calendula officinalis ethyl acetate phase respectively has synergistic effect on the inhibition of tyrosinase activity.
In a compounding system of the dandelion alcohol extract and the celery seed volatile oil, the synergistic coefficients are 1.20, 1.08 and 0.96 in sequence along with the increase of the mass ratio of the dandelion alcohol extract, which indicates that the synergistic effect of the dandelion alcohol extract and the celery seed volatile oil is gradually weakened, and certain antagonism may exist after the ratio is increased to a certain ratio, so the proportioning range needs to be paid attention to when the compounding system is adopted.
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 composition has a good synergistic effect, the mass ratio of the red paeony root alcohol extract is increased, and the synergistic effect is reduced; as can be seen from Table 5, the red peony alcohol extract with better enzyme inhibiting effect is close to the celery seed volatile oil in the effect of inhibiting the tyrosinase activity, and after the red peony alcohol extract and the celery seed volatile oil are compounded, the mass ratio of any species is increased, and the synergistic effect of a compounding system can be reduced.
Similarly, in a compound system of the lithospermum alcohol extract with better enzyme inhibiting effect and the celery seed volatile oil, the mass ratio of the lithospermum alcohol extract is increased, the synergistic coefficients are 1.07, 1.08 and 1.06, the synergistic effect is not obvious, and the compound system is supposed to possibly play a main role in the celery seed volatile oil.
In a complex system of the calendula officinalis ethyl acetate phase and the celery seed volatile oil, the mass ratio of the calendula officinalis ethyl acetate phase is increased, and the synergistic effect is gradually reduced, which is probably related to that the activity of the calendula officinalis ethyl acetate phase is lower than that of the celery seed volatile oil.
According to data results, the compound of 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 has a certain synergistic effect on the aspect of inhibiting the tyrosinase activity on the whole.
(3) Experiment for inhibiting bacteria
The experiment adopts a paper diffusion method to determine the bacteriostatic activity of 5 single substances on common strains. And (3) adjusting 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 circular filter paper sheet is placed in the middle of the culture dish, a sample with the concentration of 25mg/mL, DMSO and a positive control streptomycin sulfate with the concentration of 1mg/mL are respectively dripped on the filter paper sheet, the culture dish is inverted and placed in an incubator at 37 ℃ for culture for 24 hours. After the culture dish is taken out, the diameters of the two perpendicular directions of the inhibition zone are measured by a vernier caliper by a cross method, each experiment is carried out in parallel for three times, and the average value (mm) is taken as a measurement result. A larger zone of inhibition indicates a stronger antibacterial activity. Evaluation standard of antibiotic zone of inhibition experiment result: the diameter of the inhibition zone is more than 15mm, the sensitivity is high, the sensitivity is moderate, the sensitivity is 10-15mm (excluding 10mm, including 15 mm), the sensitivity is low, and the insensitivity is expressed by the non-inhibition zone (6 mm) and the sensitivity is 6-10mm (excluding 6mm, including 10 mm). The test results are shown in Table 7.
TABLE 7 bacteriostatic Activity of Individual substances against common strains
Figure BDA0003908016980000141
Note: "-" indicates no bacteriostasis effect, i.e. the bacteriostasis zone 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 coliform bacteria and has a certain inhibition effect on staphylococcus aureus, the lithospermum alcohol extract has no inhibition effect on coliform bacteria and staphylococcus aureus, and other substances have inhibition effects on the coliform bacteria and the staphylococcus aureus but are lower than positive control streptomycin sulfate. These extracts are more sensitive to staphylococcus aureus than e.coli, except for the alcohol extract of red peony root.
The following examples are related to the creams:
example 1
A synergistic antioxidant and whitening cream containing a celery seed volatile oil composition mainly comprises the following components in percentage by weight: 0.6% of calendula officinalis ethyl acetate phase, 0.6% of celery seed volatile oil, 1% of alkyl glycoside, 7% of laureth-7: 1%, behenyl polyether-25: 1%, polydimethylsiloxane 1%, squalane 1.5%, olive oil 1%, castor oil 1%, glycerol 3%, polyethylene glycol 2%, 1,3-butanediol 1%, hydroxyethyl cellulose 1%, xanthan gum 0.5% and ultrapure water 83.8%. The preparation method comprises the following steps:
(1) According to the mass percentage, heating alkyl glycoside, laureth-7, beheneth-25, polydimethylsiloxane, squalane, olive oil and castor oil in water bath at 400r/min to 80 ℃, dissolving uniformly, and keeping the temperature for standby use, and marking as A;
(2) According to the mass percentage, ultrapure water, glycerol, polyethylene glycol and 1,3-butanediol are heated to 80 ℃ in a water bath under the condition of 450r/min, are uniformly dissolved, and are kept warm for standby, and are marked as B;
(3) Quickly pouring the substance A into the substance B, continuously stirring at the rotation speed of 300r/min, and emulsifying at 85 ℃ for 3min;
(4) Adjusting the rotating speed to 250r/min, continuously stirring for 10min, and adding hydroxyethyl cellulose and xanthan gum according to the mass percentage;
(5) Adding the celery seed volatile oil composition according to the mass percentage, stopping heating after uniformly stirring, 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 from the embodiment 1 is that the synergistic antioxidant 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, 7% of laureth-7: 0.5%, behenyl polyether-25: 1%, polydimethylsiloxane 1%, squalane 1.5%, olive oil 1%, castor oil 1%, glycerol 3%, polyethylene glycol 2%, 1,3-butanediol 1%, hydroxyethyl cellulose 1.5%, xanthan gum 0.8% and ultrapure water 83.2%.
Example 3
The difference from the embodiment 1 is that the synergistic antioxidant 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 7% of laureth-7: 1%, behenyl polyether-25: 2 percent of polydimethylsiloxane, 2 percent of squalane, 1.5 percent of olive oil, 2 percent of castor oil, 3 percent of glycerol, 2 percent of polyethylene glycol, 1,3-butanediol 1 percent, 1 percent of hydroxyethyl cellulose, 0.5 percent of xanthan gum and 80 percent of ultrapure water.
Example 4
The difference from the embodiment 1 is that the synergistic antioxidant 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 7% of laureth-7: 1%, behenyl polyether-25: 2%, polydimethylsiloxane 2%, squalane 1.5%, olive oil 1%, castor oil 1%, glycerol 4%, polyethylene glycol 3%, 1,3-butanediol 2%, hydroxyethyl cellulose 1%, xanthan gum 0.5% and ultrapure water 79.4%.
(4) Sensory evaluation and shelf life observation of the cream:
the creams of examples 1 to 4 were each evaluated by sensory evaluation. The test population is 15 women, the age is 20-50 years, the skin of the test subject is healthy, and no allergic history of the skin disease exists. The evaluation indexes are as follows:
1) Greasy feeling: whether the face cream is soft or not when being applied or not has granular feel;
2) Coating and spreading properties: whether the face cream is easy to push away in the smearing process;
3) Refreshing degree: whether the cream has greasy feeling after being smeared;
4) Moistening property: whether the face can feel moist after the face cream is applied;
5) Acceptance degree: whether the smell, color, touch and the like of the cream can be accepted during and after the use of the cream.
The evaluation criteria were scored from 0 to 5, with 0 being the worst and 5 being the best. The results are summarized in Table 8, where the evaluation scores are average scores.
TABLE 8 evaluation of skin feel for examples 1-4
Greasy feeling Spreadability Degree of freshness Moistening property Receptivity
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 is good in use experience, moist but not sticky, mild and non-irritant.
Table 9 partial physical and chemical properties test results of cream
Figure BDA0003908016980000161
Figure BDA0003908016980000171
Note: 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 moistening cream.
Table 9 several physicochemical properties common to the creams were tested, wherein the blank control was a formula supplemented with ultrapure water after removal of the extract and the celery seed volatile oil (i.e. the composition containing the celery seed volatile oil); the preparation procedure was identical to that provided in example 1.
As is clear from the analysis of tables 8 and 9 and the combination of tables 1 to 7, a cream having excellent safety and having whitening and antioxidant properties can be obtained by adding the relevant composition to the cream base formulation. The shelf life of the cream after the composition is added can be relatively prolonged, which is probably related to the composition containing effective components such as antioxidant and bacteriostatic components.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, 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 embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (10)

1. The composition containing the celery seed volatile oil is characterized in that the celery seed volatile oil and plant extract are mixed in a weight ratio of 1:0.1-30 by mass ratio;
the plant extract is one or more of calendula, dandelion, red peony root and lithospermum.
2. The composition containing the celery seed volatile oil according to claim 1, wherein the celery seed volatile oil is prepared by a steam distillation method, and the method comprises the following specific steps:
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 to an oil-water separator, adding petroleum ether, performing oil-water separation, collecting a petroleum ether layer, removing water through anhydrous sodium sulfate, and volatilizing to remove the petroleum ether to obtain the celery seed volatile oil.
3. The composition containing celery seed volatile oil according to claim 2, wherein celery seed is 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.
4. The composition containing the celery seed volatile oil according to claim 1, wherein the extracts of dandelion, red peony root and lithospermum erythrorhizon in the plant extract are alcohol extracts and are obtained by ethanol reflux extraction;
the calendula extract in the plant extract is an ethyl acetate extract phase, and is obtained by ethanol reflux extraction and sequential extraction of petroleum ether and ethyl acetate.
5. The composition containing celery seed volatile oil according to claim 4, wherein ethanol is adopted for reflux extraction, the concentration of ethanol is 60-90%, the heating reflux temperature is 64-105 ℃, and the time is 1-3h.
6. A cream comprising a composition as claimed in any one of claims 1 to 5, characterised in that it comprises, in weight percent:
Figure FDA0003908016970000011
Figure FDA0003908016970000021
7. a cream according to claim 6, wherein the emulsifier is selected from at least three of alkyl glycoside, laureth-7, beheneth-25 and polydimethylsiloxane.
8. A cream according to claim 7, wherein the emulsifier is selected from the group consisting of alkyl glycosides, laureth-7, beheneth-25 and polydimethylsiloxanes in a ratio of 1:1:1:1 or 1:1:2:2 in a mass ratio.
9. A method of preparing a cream as claimed in any one of claims 6 to 8, comprising the steps of:
s1: mixing and stirring emulsifier, squalane, olive oil and castor oil uniformly under the condition of water bath 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 uniformly stirring 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: adjusting the stirring 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, stirring uniformly, stopping heating, adjusting the stirring speed and cooling to room temperature to obtain the face cream.
10. The method for preparing a facial cream according to claim 9,
in the step S1, the heating temperature of the water bath is 75-85 ℃, and the stirring speed is 400-500r/min;
in the step S2, the heating temperature of the water bath is 75-85 ℃, and the stirring speed is 400-500r/min;
in the step S3, the stirring speed is 250-350r/min, the emulsifying temperature is 80-90 ℃, and the time is 3-5min;
in the step S4, the stirring speed is adjusted to 200-300r/min for 10-15min;
in step S5, the stirring speed is adjusted to 100-200r/min.
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