CN110664725B - Preparation method of emulsion containing nanometer propolis extract and emulsion prepared thereby - Google Patents
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Abstract
The invention discloses a preparation method of an effective repair emulsion containing a nano propolis extract. The method can furthest retain the effective components of the propolis, and the obtained functional repairing emulsion has good effects of repairing damaged skin, shaping smooth and fine skin and the like.
Description
Technical Field
The invention belongs to the field of cosmetics, and particularly relates to a preparation method of an effective repairing emulsion containing a nano propolis extract and a repairing emulsion prepared by the preparation method.
Background
With the development of science in recent years, many animal and plant active ingredients with skin beautifying and protecting functions in the nature are discovered by human beings and widely applied to the fields of cosmetics and skin care products. Continuously developing new functional skin care products to achieve better skin beautifying and protecting effects has become an important research subject in the field at present.
Propolis is a colloidal substance obtained by collecting resin from plant buds, bark, etc. by bee, mixing with glandular secretion of bee such as lingual gland and ceriferous gland, and processing and converting by bee. Modern researches have proved that propolis has good broad-spectrum antibacterial, antiinflammatory, antiviral, analgesic, antioxidant, tissue regeneration promoting, and immunity enhancing effects. The usage of propolis for beauty treatment is divided into oral administration and external application. The oral administration of propolis can enhance immunity, refresh human body, prevent fatigue, resist oxidation, prevent chloasma and prevent vascular aging; the propolis is externally applied, so that chloasma can be prevented, skin grease is removed, the effects of resisting bacteria, diminishing inflammation, removing acne, promoting wound healing, preventing wound scars, relieving pain and the like are achieved.
The propolis contains terpenes, flavonoids, caffeic acid phenethyl ester and other active substances, and has pharmacological effects of resisting bacteria, diminishing inflammation, relieving pain and softening blood vessels, wherein the content of caffeic acid in the propolis is about 300mg/100g, and the caffeic acid has good pain relieving effect. The flavonoid compound as the marker component of the propolis endows the propolis with good antioxidant function, senile plaque is generated by human aging and excessive free radicals acting on human body, and the flavonoid compound in the propolis can remove the free radicals, so that the formation of the senile plaque can be blocked. When organism tissues, particularly skin tissues, are damaged at a certain depth, inflammatory reaction occurs on the wound surface, leukocytes, macrophages, mast cells and the like infiltrate first, various cytokines are released, fibroblasts and myofibroblasts are proliferated in a large amount and synthesize a large amount of collagen and matrix, the metabolism and arrangement of the collagen are abnormal, the abnormal matrix is deposited, and scars are finally formed under the influence of microcirculation and free radical factors. The propolis can effectively kill bacteria on the surface of a wound, prevent the wound from being infected and inflamed, block the contact with air and prevent the wound tissue from being oxidized, thereby preventing the formation or the enlargement of a wound scar.
Propolis is difficult to dissolve in water, so that a special process is needed to make propolis hydrophilic, and the absorptivity of the body to propolis is increased, so that the above-mentioned beautifying effect can be exerted. When the propolis is externally applied, the research on improving the transdermal absorption efficiency of the propolis is needed, and how to improve the absorption efficiency of the propolis is an important content for developing propolis beauty products. In addition, a large amount of unsaturated substances in the propolis are easy to oxidize, so that the color of a propolis product is deepened, and a propolis alcohol solution is unstable, so that a black substance of poly caffeic acids is easily formed after long-time storage, and the appearance of the product is influenced. Therefore, the above two disadvantages have been the problems which plague the propolis cosmetics, and there is a need for research and improvement thereof.
How to create an effective skin care product containing nano propolis extract and a preparation method thereof, which has high safety, no anaphylaxis, multiple skin care effects and can assist in repairing damaged skin barriers, is one of the important research subjects in the field.
Disclosure of Invention
In view of the disadvantages of the prior art, according to one aspect of the present invention, it is an object of the present invention to provide a method for preparing an effective repair emulsion containing nano propolis extract, the method comprising the steps of:
1) freezing raw propolis at-10 to-20 ℃ for 4 hours, then crushing the raw propolis by using a ball mill, adding crushed raw propolis powder into an extraction tank, wherein cation exchange resin is filled in the extraction tank, then adding absolute ethyl alcohol according to the volume ratio of the propolis to the ethyl alcohol of 1:6, stirring the mixture at 20 ℃ for 10 hours, then filtering the mixture by using a filter with a filter screen of 600 to 700 meshes, and concentrating the filtrate in a vacuum concentration tank to remove an ethanol solvent to obtain pretreated propolis powder;
2) adding the pretreated propolis into an extractor provided with an ultrasonic generator, adding 95% ethanol solution and petroleum ether by mass percentage, stirring and extracting for 30 minutes at 40 ℃, cooling and filtering, repeating for 3 times, combining the extract liquor, and concentrating under reduced pressure to obtain a propolis extract, wherein the weight ratio of the pretreated propolis to the 95% ethanol solution to the petroleum ether is 1:3.75:1.25, the ultrasonic frequency is 40kHz, and the power is 100W;
3) dissolving the extract obtained in the step 2) by using 80% by mass of ethanol to prepare 1% by mass of propolis ethanol solution;
4) preparing a beta-cyclodextrin water solution with the mass percent concentration of 5%;
5) adding 2 times volume of the propolis ethanol solution obtained in the step 3) into the beta-cyclodextrin water solution obtained in the step 4) under stirring, and homogenizing by using a high-pressure homogenizer, wherein the pressure of the high-pressure homogenizer is kept at 35MPa, and the homogenizing time is 30min, so as to obtain the nano propolis extract.
6) Directly freeze-drying the nano propolis extract obtained in the step 5) at-35 ℃ to obtain nano propolis extract solid particles.
7) Sequentially adding the components of the emollient into an oil pan, stirring and heating to 85-90 ℃ until the raw materials are completely and uniformly dissolved to form a first mixture A.
8) Adding the chelating agent into water for dissolving, then adding the skin conditioner, adding the humectant after the chelating agent is completely dissolved, stirring and heating to 85-90 ℃ until the raw materials are completely dissolved uniformly to form a second mixture B.
9) Starting vacuum, pumping 3/4 amount of the second mixture B in the step 8) into an emulsifying pot, pumping the first mixture A in the step 7) into the emulsifying pot, stirring for 5min, pumping the rest 1/4 amount of the second mixture B in the step 8) into the emulsifying pot, and stirring for 5 min; keeping the negative pressure of-0.03 to-0.07 MPa, starting a homogenizing switch, and homogenizing for 5 min.
10) Adding an emulsifier into the emulsifying pot in the step 9), starting vacuum, continuing stirring for 3-5min, keeping negative pressure of-0.03 to-0.07 MPa, starting a homogenizing switch, and homogenizing for 5-10 min;
11) cooling to 40-45 deg.C, stirring for 5-10min, adding the nanometer propolis extract solid particles obtained in step 6), stirring for 3-5min, adding the plant extract, stirring for 3-5min while maintaining negative pressure of-0.03 to-0.07 Mpa, starting a homogenizing switch, homogenizing for 30min, and adding deionized water to obtain the effective repairing emulsion containing nanometer propolis extract.
Based on 100 parts by weight of the functional repairing emulsion, the functional repairing emulsion comprises 70-86 parts by weight of deionized water, 0.5-3 parts by weight of nano propolis extract, 0.02-0.05 part by weight of skin conditioner, 3-15 parts by weight of humectant, 2-10 parts by weight of emollient, 0.05-0.2 part by weight of plant extract, 0.01-0.05 part by weight of chelating agent and 1-5 parts by weight of emulsifier.
Preferably, the skin conditioner consists of sodium hyaluronate and soluble collagen, wherein the weight parts of the sodium hyaluronate are 0.01-0.02, and the weight parts of the soluble collagen are 0.01-0.03.
Preferably, the humectant consists of propylene glycol, butanediol and isoprene glycol, wherein 3-5 parts by weight of propylene glycol, 2-4 parts by weight of butanediol and 2-4 parts by weight of isoprene glycol are contained.
Preferably, the emollient is composed of isononyl isononanoate, C13-16 isoparaffin, caprylic/capric triglyceride, polydimethylsiloxane, mineral oil and C10-13 isoparaffin, wherein 2-3 parts by weight of isononyl isononanoate, 2-4 parts by weight of C13-16 isoparaffin, 1-3 parts by weight of caprylic/capric triglyceride, 0.5-2 parts by weight of polydimethylsiloxane, 0.2-0.5 part by weight of mineral oil and 0.1-0.2 part by weight of C10-13 isoparaffin.
Preferably, the plant extract is composed of glycyrrhiza glabra root extract, aloe vera leaf extract, centella asiatica extract, snow lotus herb extract and peony root extract, wherein glycyrrhiza glabra root extract is 0.01-0.03 parts by weight, aloe vera leaf extract is 0.01-0.03 parts by weight, centella asiatica extract is 0.01-0.03 parts by weight, snow lotus herb extract is 0.01-0.03 parts by weight and peony root extract is 0.01-0.03 parts by weight.
Preferably, the chelating agent is disodium EDTA.
Preferably, the emulsifier is composed of wax stearyl alcohol, glyceryl stearate, PEG-100 stearate, PEG-40 sorbitan stearate, potassium wax alcohol phosphate and polysorbate-80, wherein wax stearyl alcohol 0.5-2 parts by weight, glyceryl stearate 0.5-1.5 parts by weight, PEG-100 stearate 0.5-0.8 parts by weight, PEG-40 sorbitan stearate 0.5-0.8 parts by weight, potassium wax alcohol phosphate 0.2-0.5 parts by weight and polysorbate-800.01-0.03 parts by weight.
Further preferably, based on 100 parts by weight of the functional repairing emulsion, the functional repairing emulsion comprises 84.77 parts by weight of deionized water, 2.6 parts by weight of nano propolis extract, 0.04 part by weight of skin conditioner, 5.2 parts by weight of humectant, 6.12 parts by weight of emollient, 0.06 part by weight of plant extract, 0.01 part by weight of chelating agent and 1.2 parts by weight of emulsifier.
Advantageous effects
The invention relates to an effective repair emulsion containing a nano propolis extract, wherein the nano propolis extract in the components has stronger water solubility, is easier to be absorbed by organisms, contains rich bioactive substances, combines with plant component extracts with anti-inflammation and whitening effects, has the effect of repairing skin, can supplement nutrition and moisture lost by skin, helps pore contraction, effectively repairs damaged skin, and shapes smooth and fine skin, and is an effective skin care product suitable for various skin types. The repair emulsion takes the nano propolis extract as a repair agent, and the best repair effect is achieved through the synergistic effect; the glycyrrhiza glabra extract can penetrate into the skin and keep high activity, and effectively inhibit the activity of various enzymes (such as tyrosinase) in the melanin generation process; the aloe vera leaf extract can make skin tender and elastic, and has antiseptic effect; the centella extract can tighten the connecting part of the epidermis and the dermis, so that the skin becomes soft and elastic; can also promote the formation of collagen in the dermis layer and regenerate fibrin; the saussurea involucrate extract can effectively protect the skin from being damaged by ultraviolet rays; the aging of skin tissue is delayed by peony extract. The repairing emulsion disclosed by the invention is excellent in storage stability, high in skin permeability and good in skin elasticity repairing.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
Compared with the traditional propolis, the nano propolis extract prepared by the preparation method of the invention has relatively active chemical properties and stronger water solubility, so that the nano propolis extract is relatively easy to be absorbed by organisms. On one hand, the active ingredients in the propolis are effectively prevented from losing through ultrasonic-assisted two-phase extraction, on the other hand, the active ingredients in the propolis are further prevented from being damaged in the subsequent process steps through compounding with beta-cyclodextrin, and the propolis is easier to absorb through the use of a freeze drying technology. In addition, the surface structure of the nanometer propolis extract particle is changed, and the nanometer propolis extract particle has the surface interface effect of nanometer particles, and enhances various biological effects of the nanometer propolis extract particle, such as the functions of accelerating organism tissue regeneration, resisting bacteria and tumors, improving organism immunity, resisting oxidation and the like. The nano technology is introduced in the preparation of the propolis to change the propolis into nano particles, so that the physicochemical properties and corresponding effects of the propolis are changed, a new generation of nano propolis extract product is created, and the value of the propolis can be greatly improved.
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
Example 1
1) Freezing raw propolis at-10 to-20 ℃ for 4 hours, then crushing the raw propolis by using a ball mill, adding crushed raw propolis powder into an extraction tank, wherein cation exchange resin is filled in the extraction tank, then adding absolute ethyl alcohol according to the volume ratio of the propolis to the ethyl alcohol of 1:6, stirring the mixture at 20 ℃ for 10 hours, then filtering the mixture by using a filter with a filter screen of 600 to 700 meshes, and concentrating the filtrate in a vacuum concentration tank to remove an ethanol solvent to obtain pretreated propolis powder.
2) Adding the pretreated propolis into an extractor provided with an ultrasonic generator, adding 95% ethanol solution and petroleum ether by mass percentage, stirring and extracting for 30 minutes at 40 ℃, cooling and filtering, repeating for 3 times, combining the extract liquor, and concentrating under reduced pressure to obtain the propolis extract, wherein the weight ratio of the pretreated propolis to the 95% ethanol solution to the petroleum ether is 1:3.75:1.25, the ultrasonic frequency is 40kHz, and the power is 100W.
3) Dissolving the extract obtained in the step 2) by using 80% by mass of ethanol to prepare 1% by mass of propolis ethanol solution.
4) Preparing a beta-cyclodextrin water solution with the mass percent concentration of 5%.
5) Adding 2 times volume of the propolis ethanol solution obtained in the step 3) into the beta-cyclodextrin water solution obtained in the step 4) under stirring, and homogenizing by using a high-pressure homogenizer, wherein the pressure of the high-pressure homogenizer is kept at 35MPa, and the homogenizing time is 30min, so as to obtain the nano propolis extract.
6) Directly freeze-drying the nano propolis extract obtained in the step 5) at-35 ℃ to obtain nano propolis extract solid particles.
7) Sequentially adding various components of the emollient with the formula ratio into an oil pan, stirring and heating to 85-90 ℃ until the raw materials are completely and uniformly dissolved to form a first mixture A.
8) Adding the chelating agent with the formula amount into water to dissolve, then adding the skin conditioning agent with the formula amount, adding the humectant with the formula amount after the chelating agent with the formula amount is completely dissolved, stirring and heating to 85-90 ℃ until the raw materials are completely dissolved uniformly to form a second mixture B.
9) Starting vacuum, pumping 3/4 amount of the second mixture B in the step 8) into an emulsifying pot, pumping the first mixture A in the step 7) into the emulsifying pot, stirring for 5min, pumping the rest 1/4 amount of the second mixture B in the step 8) into the emulsifying pot, and stirring for 5 min; keeping the negative pressure of-0.03 to-0.07 MPa, starting a homogenizing switch, and homogenizing for 5 min.
10) Adding the emulsifier with the formula amount into the emulsifying pot in the step 9), starting vacuum, continuing stirring for 3-5min, keeping the negative pressure of-0.03 to-0.07 MPa, starting a homogenizing switch, and homogenizing for 5-10 min;
11) cooling to 40-45 deg.C, stirring for 5-10min, adding nanometer propolis extract solid particles obtained in step 6), stirring for 3-5min, adding plant extract, stirring for 3-5min while maintaining negative pressure of-0.03-0.07 Mpa, starting homogenizing switch, homogenizing for 30min, and adding deionized water to obtain the final product.
12) Sampling, discharging after inspection and filling.
13) And aging for 1-2 days, filling and warehousing.
The functional repairing emulsion comprises, based on 100 parts by weight of the functional repairing emulsion, 84.77 parts by weight of deionized water, 2.6 parts by weight of nano propolis extract, 0.04 part by weight of skin conditioner, 5.2 parts by weight of humectant, 6.12 parts by weight of emollient, 0.06 part by weight of plant extract, 0.01 part by weight of chelating agent and 1.2 parts by weight of emulsifier.
The skin conditioner consists of sodium hyaluronate and soluble collagen, wherein the weight parts of the sodium hyaluronate and the soluble collagen are 0.02.
The humectant consists of propylene glycol, butanediol and isoprene glycol, wherein the propylene glycol accounts for 2.5 parts by weight, the butanediol accounts for 1.2 parts by weight, and the isoprene glycol accounts for 2 parts by weight.
The emollient is composed of isononyl isononanoate, C13-16 isoparaffin, caprylic/capric triglyceride, polydimethylsiloxane, mineral oil and C10-13 isoparaffin, wherein 1.5 parts by weight of isononyl isononanoate, 1.5 parts by weight of C13-16 isoparaffin, 1.5 parts by weight of caprylic/capric triglyceride, 0.9 part by weight of polydimethylsiloxane, 0.5 part by weight of mineral oil and 0.22 part by weight of C10-13 isoparaffin.
The plant extracts comprise glycyrrhiza glabra root extract, aloe barbadensis leaf extract, centella asiatica extract, snow lotus herb extract and peony root extract, wherein the glycyrrhiza glabra root extract is 0.01 weight part, the aloe barbadensis leaf extract is 0.01 weight part, the snow lotus herb extract is 0.01 weight part and the peony root extract is 0.02 weight part.
The chelating agent is EDTA disodium salt 0.01 weight portion.
The emulsifier is composed of wax stearyl alcohol, glycerol stearate, PEG-100 stearate, PEG-40 sorbitan stearate, potassium wax alcohol phosphate and polysorbate-80, wherein wax stearyl alcohol 0.2 part by weight, glycerol stearate 0.2 part by weight, PEG-100 stearate 0.2 part by weight, PEG-40 sorbitan stearate 0.2 part by weight, potassium wax alcohol phosphate 0.2 part by weight and polysorbate-800.2 part by weight.
Example 2
The formula of the effective repair emulsion containing the nano propolis extract in the embodiment is as follows:
the functional repairing emulsion comprises 80.44 parts by weight of deionized water, 3 parts by weight of nano propolis extract, 0.04 part by weight of skin conditioner, 6 parts by weight of humectant, 8 parts by weight of emollient, 0.1 part by weight of plant extract, 0.02 part by weight of chelating agent and 2.4 parts by weight of emulsifier based on 100 parts by weight of the functional repairing emulsion.
Wherein the skin conditioning agent, humectant, emollient, plant extract and emulsifier are adjusted in the proportions listed in example 1.
The effective repair emulsion containing nano propolis extract was prepared in the same manner as in example 1, except that the formulation of the effective repair emulsion containing nano propolis extract was adjusted as above.
Comparative example 1
An efficacious repair emulsion containing propolis was prepared according to the same formulation and preparation method as in example 1, except that steps 1) to 6) were not performed, that is, commercially available propolis was directly used as a raw material without any treatment of propolis.
Comparative example 2
An efficacious repair emulsion containing propolis was prepared according to the same formulation and preparation method as in example 1, except that the step 2) was not performed, that is, propolis was not treated by ultrasonic-assisted two-phase extraction.
Comparative example 3
An efficacious repair emulsion containing propolis was prepared according to the same formulation and preparation method as in example 1, except that the steps 4) and 5) were not performed, that is, the aqueous solution of β -cyclodextrin was not used.
Test example 1: measurement of particle size of propolis extract
Taking a proper amount of the nano propolis extract prepared in the step 5) of the examples 1 and 2, and dispersing the proper amount of the nano propolis extract by using a 0.3% poloxamer 188 solution to ensure that the final concentration of the nano propolis extract is 0.1 mg/ml. Vortex shaking for 10min, and determining particle size with Zeta potential meter. The nano-propolis extract prepared in example 1 has a particle size of about 220.1nm, and the nano-propolis extract prepared in example 2 has a particle size of about 231.4 nm.
Test example 2: nanometer propolis extract antioxidant research
2.1 test materials
Nano propolis extract prepared in step 5) of example 1, commercially available propolis, tween-80, SDS, Na2HPO4O-benzenetriol, FeSO4·7H2O, salicylic acid, hydrochloric acid, hydrogen peroxide, 95% ethanol, Tris, sodium nitrite, aluminum nitrate and sodium hydroxide in percentage by mass, and the above reagents are all commercially available domestic analytical purifiers unless otherwise specified.
2.2 test apparatus
A vacuum freeze dryer; CU420 type constant temperature water bath; an electronic balance of type FA 1640; 85-1 type constant temperature magnetic stirrer; model TDL-60B centrifuge; 723 visible spectrophotometer; 202-1A type digital display electric heating constant temperature drying oven.
2.3 test procedure
2.3.1 preparation of reagents.
10mmol/L HCl; 50mmol/L Tris-HCl buffer solution with pH 8.2; 3mmol/L pyrogallol solution.
2.3.2 para superoxide anion radical (O)2 ˉ) Measurement of clearance.
By using systems in which the oxidizing process is carried out with superoxide anion radicals (O)2 ˉ) Generation of (A) O2 ˉThe interaction with certain compounds produces a colored substance with a specific absorption, which is measured using a spectrophotometer. If the test substance can remove O2 ˉIf so, the absorbance changes, and the test object can be indirectly judged to be O2 ˉThe inhibitory action of (1). The pyrogallol is quickly autooxidized under the alkaline condition, and O is generated in the autooxidation process2 ˉ，O2 ˉAnd the autoxidation rate of the pyrogallol is accelerated, a colored intermediate substance is generated, the accumulation of the colored intermediate product has a good linear relation with time within 30-45 s, the accumulation is generally maintained for about 4min, and then the accumulation is slowed down. The colored intermediate product has a strong light absorption at 322 nm. Due to autoxidationIs dependent on O2 ˉConcentration of (2), elimination of O2 ˉInhibiting the autoxidation reaction and preventing the accumulation of intermediate products, thereby evaluating the inhibition of O by the test substance2 ˉThe ability of the cell to perform.
Preparing the nano propolis extract prepared in the step 5) of the example 1 and a commercially available propolis sample into 2.4% solution by mass percent, respectively, and measuring the obtained superoxide anion radical (O) by taking 0.1ml and 0.2ml of the solution2 ˉ) The clearance of (D) is shown in Table 1.
Table 1: various sample solutions to superoxide anion radical (O)2 ˉ) Inhibition rate of
As can be seen from Table 1, both the nano-propolis extract prepared according to step 5) of example 1 and the commercially available propolis samples were able to scavenge superoxide anion (O) within 180s2 ˉ) However, the removing effect of the nano propolis extract in example 1 is better than that of the commercially available propolis sample, which shows that the superoxide anion removing activity of the propolis is enhanced after the propolis is treated by the method of the invention.
2.3.3 measurement of the auto-oxidation rate of pyrogallol.
Taking 4.5ml of 50mmol/L Tris-HCl buffer solution (pH value is 8.2), uniformly mixing 4.2ml of distilled water in a 25ml test tube, then preserving heat in a water bath at 37 ℃ for 20min, immediately adding 0.5ml of pyrogallol preheated at 37 ℃, quickly shaking up, pouring into a cuvette, measuring absorbance at intervals of 30s at 325nm, calculating the increase of absorbance per minute in a linear range, preparing a blank tube by using 10mmol/L HCl solution as a control, and recording the result. According to the steps, 0.1ml of sample liquid with different concentrations is added before the pyrogallol is added, and the distilled water is reduced correspondingly. A blank tube was also prepared with 10mmol/L HCl solution as a control, absorbance was measured, and the results were recorded, and each sample was repeated 3 times and averaged. The inhibition rate was calculated according to the formula: inhibition ratio (%) (. DELTA.A)1/△t-△A2/△t)/△A1/. DELTA.t.times.100%; in the formula: delta A1V. delta. t is the reaction rate during the autoxidation of pyrogallol, delta. A2And/. DELTA.t is the reaction rate of pyrogallol autoxidation after the sample liquid is added.
The absorbance values of the pyrogallol autoxidation rate measured every 30s at 0, 30, 60, 90, 120, 150 and 180s are respectively 0.260, 0.608, 0.784, 0.856, 0.902, 0.924 and 0.940, and the pyrogallol autoxidation rate delta A1/△t＝37.78×10-4。
Test example 3: stability test
After the propolis-containing efficacy repair emulsions prepared in examples 1 and 2 and comparative examples 1 to 3 were stored at 50 ℃, 25 ℃, and-5 ℃ for 2 months, respectively, their appearances were observed with the naked eye. Further, the presence or absence of crystal precipitation was confirmed by observation with an optical microscope (400 times). As a result, the results are shown in table 2, in which no emulsion separation or crystal precipitation was observed at any temperature and the one excellent in stability is indicated by "o", the one showing no emulsion separation or crystal precipitation and the one showing no instability at any temperature is indicated by "x":
table 2: stability test
| Detecting items | Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Stability at 50 deg.C | ○ | ○ | × | ○ | ○ |
| Stability at 25 ℃ | ○ | ○ | × | × | ○ |
| Stability at-5 deg.C | ○ | ○ | × | × | × |
As can be seen from the data in Table 2, the propolis-containing effective repair emulsion prepared according to the method of the present invention has very good stability even when stored at-5 ℃ for 2 months, and no emulsion separation or crystallization phenomenon is observed.
Test example 4: skin elasticity test
50 35 healthy women of age 35 were randomly selected as test subjects, and were randomly divided into 5 groups, and the propolis-containing efficacy-restoring emulsions of examples 1 and 2 and comparative examples 1 to 3 were used, respectively. The test instrument is a revisometer RV600 (elastic fiber tissue test probe) of the skin elasticity tester MPA580 of CK company, germany, and the average value is taken five times.
And (3) testing conditions are as follows: (1) an indoor environment; (2) no strong sunlight or direct light; (3) the ambient temperature is 20 +/-2 ℃, and the ambient humidity is 40-60%.
Test area: the right zygomatic part.
The testing steps are as follows: the blank values (R2, R5, R7) were measured 30min after the test area was cleansed, and then the subjects were prescribed to adhere to the samples every morning and evening, and the skin elasticity index R2, R5, R7 values of the test area after 4 weeks (the negative pressure was constant at 450mbar during the test).
Specification of indexes: the closer the skin elasticity indexes R2, R5, R7 are to 1, the better the elasticity of the skin. Wherein R2 ═ Ua/Uf; r5 ═ Ur/Ue; r7 ═ Ur/Uf. Uf is the maximum skin stretch, and Ue is the skin stretch at 0.1s after a constant negative pressure is applied to the skin, and the elastic portion stretch is located. Ur is the value of elastic part Ur, namely the value of recovery and viscoelastic part, or moulding part, of skin after negative pressure is removed for 0.1 s. Ua is the recovery value of the skin from the elimination of the negative pressure to the next continuous test of the skin surface plus the negative pressure.
The test results are shown in table 3 below.
Table 3 skin elasticity test
As shown in table 3, the propolis-containing efficacious repair emulsion cosmetics produced according to examples 1 and 2 of the present invention are excellent in storage stability; after 4 weeks of coating, the propolis-containing effective repair emulsion cosmetics produced according to examples 1 and 2 of the present invention all obtained better elasticity retention, while the propolis-containing effective repair emulsion obtained without the preparation method of the present invention was not ideal enough in effect, indicating that the propolis-containing effective repair emulsion according to the present invention has high skin penetration and high skin elasticity improvement.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (8)
1. A preparation method of an effective repairing emulsion containing nano propolis extract comprises the following steps:
1) freezing raw propolis at-10 to-20 ℃ for 4 hours, then crushing the raw propolis by using a ball mill, adding crushed raw propolis powder into an extraction tank, wherein cation exchange resin is filled in the extraction tank, then adding absolute ethyl alcohol according to the volume ratio of the propolis to the ethyl alcohol of 1:6, stirring the mixture at 20 ℃ for 10 hours, then filtering the mixture by using a filter with a filter screen of 600 to 700 meshes, and concentrating the filtrate in a vacuum concentration tank to remove an ethanol solvent to obtain pretreated propolis powder;
2) adding the pretreated propolis into an extractor provided with an ultrasonic generator, adding 95% ethanol solution and petroleum ether by mass percentage, stirring and extracting for 30 minutes at 40 ℃, cooling and filtering, repeating for 3 times, combining the extract liquor, and concentrating under reduced pressure to obtain a propolis extract, wherein the weight ratio of the pretreated propolis to the 95% ethanol solution to the petroleum ether is 1:3.75:1.25, the ultrasonic frequency is 40kHz, and the power is 100W;
3) dissolving the extract obtained in the step 2) by using 80% by mass of ethanol to prepare 1% by mass of propolis ethanol solution;
4) preparing a beta-cyclodextrin water solution with the mass percent concentration of 5%;
5) adding 2 times of the volume of the propolis ethanol solution obtained in the step 3) into the beta-cyclodextrin aqueous solution obtained in the step 4) under stirring, and then homogenizing by using a high-pressure homogenizer, wherein the pressure of the high-pressure homogenizer is kept at 35MPa, and the homogenizing time is 30min, so as to obtain a nano propolis extract;
6) directly freeze-drying the nano propolis extract obtained in the step 5) at-35 ℃ to obtain nano propolis extract solid particles;
7) sequentially adding various components of the emollient into an oil pan, stirring and heating to 85-90 ℃ until the raw materials are completely and uniformly dissolved to form a first mixture A;
8) adding a chelating agent into water for dissolving, then adding a skin conditioner, adding a humectant after the chelating agent is completely dissolved, stirring and heating to 85-90 ℃ until the raw materials are completely dissolved uniformly to form a second mixture B;
9) starting vacuum, pumping 3/4 amount of the second mixture B in the step 8) into an emulsifying pot, pumping the first mixture A in the step 7) into the emulsifying pot, stirring for 5min, pumping the rest 1/4 amount of the second mixture B in the step 8) into the emulsifying pot, and stirring for 5 min; keeping the negative pressure of-0.03 to-0.07 MPa, starting a homogenizing switch, and homogenizing for 5 min;
10) adding an emulsifier into the emulsifying pot in the step 9), starting vacuum, continuing stirring for 3-5min, keeping negative pressure of-0.03 to-0.07 MPa, starting a homogenizing switch, and homogenizing for 5-10 min;
11) cooling to 40-45 deg.C, stirring for 5-10min, adding the nanometer propolis extract solid particles obtained in step 6), stirring for 3-5min, adding the plant extract, stirring for 3-5min while maintaining negative pressure of-0.03 to-0.07 Mpa, starting a homogenizing switch, homogenizing for 30min, and adding deionized water to obtain the effective repairing emulsion containing nanometer propolis extract;
based on 100 parts by weight of the functional repairing emulsion, the functional repairing emulsion comprises 70-86 parts by weight of deionized water, 0.5-3 parts by weight of nano propolis extract, 0.02-0.05 part by weight of skin conditioner, 3-15 parts by weight of humectant, 2-10 parts by weight of emollient, 0.05-0.2 part by weight of plant extract, 0.01-0.05 part by weight of chelating agent and 1-5 parts by weight of emulsifier.
2. The method according to claim 1, wherein the skin conditioner comprises sodium hyaluronate and soluble collagen, and the amount of the sodium hyaluronate is 0.01 to 0.02 parts by weight and the amount of the soluble collagen is 0.01 to 0.03 parts by weight.
3. The method according to claim 1, wherein the humectant is composed of propylene glycol, butylene glycol, and isoprene glycol, and wherein propylene glycol is 3 to 5 parts by weight, butylene glycol is 2 to 4 parts by weight, and isoprene glycol is 2 to 4 parts by weight.
4. The method of claim 1, wherein the emollient is composed of isononyl isononanoate, C13-16 isoparaffin, caprylic/capric triglyceride, polydimethylsiloxane, mineral oil, and C10-13 isoparaffin, wherein isononyl isononanoate 2-3 parts by weight, C13-16 isoparaffin 2-4 parts by weight, caprylic/capric triglyceride 1-3 parts by weight, polydimethylsiloxane 0.5-2 parts by weight, mineral oil 0.2-0.5 part by weight, and C10-13 isoparaffin 0.1-0.2 part by weight.
5. The method of claim 1, wherein the plant extract is composed of glycyrrhiza glabra root extract, aloe barbadensis leaf extract, centella asiatica extract, snow lotus extract and peony root extract, wherein glycyrrhiza glabra root extract is 0.01-0.03 parts by weight, aloe barbadensis leaf extract is 0.01-0.03 parts by weight, snow lotus extract is 0.01-0.03 parts by weight, and peony root extract is 0.01-0.03 parts by weight.
6. The method of claim 1, wherein the chelating agent is disodium EDTA.
7. The method according to claim 1, wherein the emulsifier is composed of parts by weight of wax stearyl alcohol, glyceryl stearate, PEG-100 stearate, PEG-40 sorbitan stearate, parts by weight of potassium wax alcohol phosphate, and polysorbate-80, wherein parts by weight of wax stearyl alcohol, 0.5 to 1.5 parts by weight of glyceryl stearate, 0.5 to 0.8 parts by weight of PEG-100 stearate, 0.5 to 0.8 parts by weight of PEG-40 sorbitan stearate, 0.2 to 0.5 parts by weight of parts by weight of potassium wax alcohol phosphate, and polysorbate-800.01 to 0.03 parts by weight.
8. The method of claim 1, wherein the effective repair emulsion comprises 84.77 parts by weight of deionized water, 2.6 parts by weight of nano propolis extract, 0.04 parts by weight of skin conditioner, 5.2 parts by weight of humectant, 6.12 parts by weight of emollient, 0.06 parts by weight of plant extract, 0.01 parts by weight of chelating agent and 1.2 parts by weight of emulsifier, based on 100 parts by weight of the effective repair emulsion.
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