CN112957284B

CN112957284B - Repair essence containing peony seed oil nano-liposomes and preparation method thereof

Info

Publication number: CN112957284B
Application number: CN202110378135.1A
Authority: CN
Inventors: 常大伟; 张天宝
Original assignee: Guangzhou Dongzhimeng Cosmetics Co ltd
Current assignee: Guangzhou Dongzhimeng Cosmetics Co ltd
Priority date: 2021-04-08
Filing date: 2021-04-08
Publication date: 2023-06-23
Anticipated expiration: 2041-04-08
Also published as: CN112957284A

Abstract

The invention relates to the technical field of fine chemical engineering, in particular to a repair essence containing peony seed oil nano-liposomes and a preparation method thereof, wherein the skin care essence comprises polyalcohol, a thickener, p-hydroxyacetophenone, 1, 2-hexanediol, sodium hyaluronate and peony seed oil nano-liposomes; no preservative is added, and the liposome embedding technology is applied to the functional components which are not easy to permeate the skin horny layer, so that the transdermal absorptivity of the functional components is increased, and the skin care effect is greatly improved. After the essence containing the peony seed oil nano-liposome is used, the skin cutin barrier is better repaired, the transepidermal water loss rate is reduced, namely the skin water retention capacity is improved, the skin self-moisturizing performance is improved, and the skin health degree is improved; the skin pigmentation is improved, and the skin pigmentation has more remarkable improvement effect on the skin with the problems of color deposition such as color spots, acne marks and the like; the skin has increased collagen density, i.e. increased collagen content, and is younger.

Description

Repair essence containing peony seed oil nano-liposomes and preparation method thereof

Technical Field

The invention relates to the technical field of fine chemical engineering, in particular to repair essence containing peony seed oil nano-liposomes and a preparation method thereof.

Background

The peony seed oil is an effective vegetable oil extracted from peony seeds, and contains rich unsaturated fatty acids (especially alpha-linolenic acid), VA, VE, nicotinic acid, carotene, minerals and various amino acids, wherein the content of the unsaturated fatty acids is 2-5 times that of other seed oils, so that the peony seed oil has good health care value and skin care value. The peony seed oil can promote normal metabolism of skin epidermal cells, promote microcirculation of skin capillaries, activate peripheral nerves, inhibit skin dullness and aging caused by lipid peroxidation, slow down the whole skin aging process, and has comprehensive skin care effects of resisting oxidation, maintaining skin moisture, improving facial pigmentation, relieving wrinkles, increasing skin elasticity and the like.

The peony seed oil can be used as an oil phase raw material and added into an O/W emulsion or cream system or directly added into an oil skin care product. The skin care product of the pure oiling agent, namely skin care essential oil, has poor absorptivity, is easy to be oiled after being used on the face, has residual greasy feel on the hands, and therefore, the acceptance of consumers is generally low. Meanwhile, the effective components in the peony seed oil are difficult to exert the maximum value due to poor permeability and absorption. When the peony seed oil is used as an oil phase raw material to be added into the O/W emulsion, the unsaturated fatty acid in the peony seed oil is destroyed in the heating process and the skin care value is reduced because the oil phase needs to be heated to 75-85 ℃ before emulsification and simultaneously kept for 10min or more.

At present, no related research on directly adding the peony seed oil into a water-based skin care product or O/W emulsion under a low-temperature condition is performed after certain pretreatment, so that a mode of adding the peony seed oil into the water-based skin care product is searched, and the skin care value of the peony seed oil can be exerted to the greatest extent.

Disclosure of Invention

The invention aims to provide repair essence containing peony seed oil nano-liposomes and a preparation method thereof, which solve the problem that the peony seed oil is not added into water-based skin care products in the prior art.

The invention is realized by the following technical scheme:

the repair essence containing the peony seed oil nano liposome comprises the following components in percentage by mass:

further, the thickener is acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, ammonium acryloyldimethyl taurate/VP copolymer or polyacrylate cross-linked polymer-6;

when the thickener is acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, the repair essence also comprises an alkaline neutralizer.

Further, the alkaline neutralizer is sodium hydroxide or triethanolamine, and when sodium hydroxide is adopted, the mass ratio of the sodium hydroxide to acrylic acid (esters) or C10-30 alkanol acrylate crosslinked polymer is 0.4:1;

when triethanolamine is adopted, the mass ratio of the triethanolamine to the acrylic acid (ester) or the C10-30 alkanol acrylate cross-linked polymer is 1:1.

Further, the polyalcohol is one or more of glycerol, 1, 3-butanediol and 1, 2-pentanediol.

Further, the particle size of the peony seed oil nano liposome is 212-332 nm, and the encapsulation rate of the nano liposome is 79-96%.

The invention also discloses a preparation method of the repair essence containing the peony seed oil nano-liposome, which comprises the following steps:

s1, adding a thickening agent into water, soaking the thickening agent in the water, and standing for 1-2 h to obtain a mixed solution A;

uniformly dispersing sodium hyaluronate, adding the sodium hyaluronate into water, stirring and heating until the sodium hyaluronate is completely dissolved to obtain a mixed solution B; heating the mixed solution B to 60 ℃, adding p-hydroxyacetophenone and 1, 2-hexanediol, stirring and heating until the mixed solution B is completely dissolved, and obtaining a mixed solution C;

s2, adding the mixed solution C into the mixed solution A, stirring and heating to 75-80 ℃, continuously stirring until the mixed solution is completely dissolved, and preserving heat for 20-30 min to obtain a mixed solution D;

s3, cooling the mixed solution D to 42-45 ℃, adding the peony seed oil nanoliposome, and stirring until the mixture is uniformly dispersed to obtain a mixed solution E;

and S4, continuously cooling the mixed solution E to below 35 ℃ to obtain the repair essence containing the peony seed oil nano-liposome.

Further, the thickener is one of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, ammonium acryloyldimethyl taurate/VP copolymer or polyacrylate cross-linked polymer-6;

when the thickener is acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, in the step S3, after the mixed solution D is cooled to 42-45 ℃, adding an alkaline neutralizer, stirring to form uniform gel, then adding peony seed oil nanoliposome, and stirring until the mixture is uniformly dispersed.

Further, in S4, the preparation method of the peony seed oil nanoliposome specifically includes the following steps:

(1) Weighing 24 parts of surfactant, 2.4-12 parts of sterol and 2.4-12 parts of peony seed oil according to parts by weight;

(2) Mixing and stirring a surfactant and sterol to obtain an oil phase I, and then cooling to room temperature;

(3) Adding peony seed oil into the oil phase I, mixing to obtain an oil phase II, heating, stirring, and cooling to room temperature;

(4) Mixing glycerol and distilled water, and preheating to obtain a water phase;

(5) Adding the water phase into the oil phase II, mixing and stirring, and then incubating to obtain a mixed solution; homogenizing the mixed solution for 1-4 minutes to obtain primary emulsion, and cooling to 0-4 ℃;

(6) And performing ultrasonic dispersion on the colostrum to obtain the peony seed oil nanoliposome.

Further, the mass ratio of the surfactant to the sterol to the peony seed oil is 6:1:1.

Further, homogenizing at a rotational speed of 10000-20000 r/min.

Compared with the prior art, the invention has the following beneficial technical effects:

the invention discloses a repair essence containing peony seed oil nano-liposomes, which comprises polyalcohol, a thickening agent, p-hydroxyacetophenone, 1, 2-hexanediol, sodium hyaluronate and peony seed oil nano-liposomes; the liposome embedding technology is applied to the functional components which are not easy to permeate the skin horny layer, so that the transdermal absorptivity of the functional components is increased, the low-temperature addition of the active components is realized, the activity of the components is prevented from being reduced along with heating, and the skin care effect is greatly improved. The selected thickener has high safety to skin, strong ion resistance, enhances the physicochemical stability of the formula and is not easy to cause skin sensitization.

The complete peony seed oil nano-liposome has a certain targeting effect on skin, can penetrate through a cutin barrier to enter the deep layer of the skin, and meanwhile, because of the amphiphilicity of the liposome, the liposome-embedded components have higher osmotic absorptivity than water-based or oil-based components, that is, the peony seed oil nano-liposome can realize higher transdermal absorptivity than the peony seed oil in essential oil or emulsion, and the liposome has better affinity with a bilayer on the surface of a cell, even fuses with the lipid of the cutin layer, so that the lipid structure of the cutin layer is changed, a granular structure with gaps is formed, holes, cracks and folds are formed, and the functional components can enter the deep layer of the skin through the holes and the cracks. Therefore, the peony seed oil nanoliposome is beneficial to the transdermal absorption of other functional components while maintaining the self-high transdermal absorption rate.

Therefore, the peony seed oil nanoliposome is added into the water-based essence, so that the skin care effect of the peony seed oil can be maximally realized, and the absorption of other nutrient components in the water-based essence can be promoted. Besides being easier to penetrate through the stratum corneum penetration barrier, the peony seed oil nanoliposome can also penetrate through skin accessory structures such as hair follicles, sebaceous glands and the like to be absorbed by the skin, and the absorption rate of the peony seed oil nanoliposome penetrating through the hair follicles is 5-8 times that of a common water-based product. After verification, the essence containing the peony seed oil nanoliposome is used, the skin cutin barrier is better repaired, the transepidermal water loss rate is reduced, namely, the skin water retention capacity is improved, the skin self-moisturizing performance is improved, and the skin health degree is improved; the skin pigmentation is improved, and the skin pigmentation has more remarkable improvement effect on the skin with the problems of color deposition such as color spots, acne marks and the like; the skin has increased collagen density, i.e. increased collagen content, and is younger.

The invention also discloses a preparation method of the repair essence containing the peony seed oil nano-liposome, wherein the hyaluronic acid is pre-dispersed by using the polyalcohol and then added into cold water, so that the aggregation of the hyaluronic acid can be avoided, and the hyaluronic acid is difficult to dissolve; the most rapid dissolution of the p-hydroxyacetophenone can be realized by adding the p-hydroxyacetophenone at 60 ℃; the thickener and other water phase components are respectively pretreated, so that other components except the thickener can be fully dissolved, and the thickener can be ensured to form uniform gel; the low-temperature addition of the peony seed oil is realized, and the peony seed oil nanoliposome is added into the water-based essence, so that the percutaneous absorption of the peony seed oil and the skin care effect of the peony seed oil can be maximally realized, and the absorption of other nutrient components in the water-based essence can be promoted.

Furthermore, the invention also discloses a preparation method of the peony seed oil nanoliposome, which adopts a hot melting method to prepare the nanoliposome without using an organic solvent, so that the toxicity of the residual organic solvent to cells is avoided; the liposome is prepared by adopting a method of heating up and cooling down for multiple times, so that the oxidation of grease caused by continuous heating can be avoided, and the encapsulation rate of the obtained liposome is higher than that of the liposome prepared by an unmodified continuous heating hot melting method; the invention prepares the nano liposome by adopting a method combining homogenization and ultrasonic technology on the basis of a hot melting method, can play a role in fully dispersing the liposome, and effectively reduces the particle size of the liposome. The hot-melt method is a method for preparing liposome without using an organic solvent, and is based on the principle that the temperature is heated to above the phase transition temperature of the surfactant, so that the permeability and fluidity of a bilayer membrane of the surfactant such as lecithin and the like are increased, and thus the encapsulated substance can be incorporated into a lipid bilayer, then the addition of an aqueous phase allows the surfactant to self-assemble in the aqueous phase to form spherical liposome vesicles, and then the liposome is stabilized by magnetic stirring, and the purpose of dispersing the liposome to reduce the particle size is achieved. The hot-melting method is a method without using an organic solvent, so the prepared liposome has no toxicity to cells, but the liposome prepared by the hot-melting method only has low encapsulation efficiency (about 77.8%), which is probably due to the fact that the phospholipid bilayer is not fully developed, so that the doping efficiency of the encapsulated substance is low, grease is easily oxidized at high temperature in the heating process, and the adverse effect is caused to the liposome. Meanwhile, the liposome vesicles are dispersed in a stirring mode by adopting a hot melting method, and the dispersing mode is mild but has limited effect on reducing the particle size of the liposome vesicles, so that the prepared liposome has larger particle size (about 864.9 nm), and the prepared liposome cannot effectively penetrate through the stratum corneum of the skin, so that transdermal administration is not facilitated. The liposome prepared by the hot melting method has poor particle size uniformity, a high polydispersity index (about 0.47) and a small charge number (about-22.4 mV), so that the liposome is easy to have the phenomena of vesicle fusion, agglomeration, sedimentation and the like in the storage process, the stability of the product is poor, and finally, the hot melting method, the homogenization technology and the ultrasonic technology are combined to be used, so that the obtained nano liposome has higher encapsulation efficiency, smaller particle size, high particle size uniformity and high vesicle charge number, the particle size of the liposome is further reduced, the encapsulation efficiency of the liposome is improved, and the stability and popularization of the product are improved.

Drawings

FIG. 1 is a graph showing the particle size distribution of peony seed oil liposomes;

FIG. 2 shows Zeta potential of peony seed oil nanoliposomes;

FIG. 3 is a TEM image of peony seed oil nanoliposomes, FIG. 3 (a) represents a liposome image at 100000 magnification; FIG. 3 (b) represents a liposome image at 200000 magnification;

fig. 4 is a schematic diagram of patch positions.

Detailed Description

The invention will now be described in further detail with reference to specific examples, which are intended to illustrate, but not to limit, the invention.

The invention discloses repair essence containing peony seed oil nano-liposomes, which comprises the following components in percentage by mass:

specifically, the thickener is one of acrylic acid (esters)/C10-30 alkanol acrylate cross-linked polymer, ammonium acryloyldimethyl taurate/VP copolymer or polyacrylate cross-linked polymer-6.

When the thickener is acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, the phase B also comprises an alkaline neutralizer. The alkaline neutralizer is sodium hydroxide or triethanolamine, the mass ratio of sodium hydroxide to acrylic acid (esters) and C10-30 alkanol acrylate cross-linked polymer is 0.4:1, and the mass ratio of the triethanolamine to acrylic acid (esters) and C10-30 alkanol acrylate cross-linked polymer is 1:1.

The polyalcohol is one or more of glycerol, 1, 3-butanediol and 1, 2-pentanediol.

The preparation method of the peony seed oil nano liposome comprises the following steps:

(5) Adding the water phase into the oil phase II, mixing and stirring, and then incubating to obtain a mixed solution; homogenizing the mixed solution at a rotating speed of 10000-20000r/min for 1-4 minutes to obtain colostrum, and cooling to 0-4 ℃;

The particle size of the prepared peony seed oil nano liposome is 212-332 nm, and the encapsulation rate of the nano liposome is 79-96%.

The mass ratio of the surfactant to the sterol to the peony seed oil is 6:1:1.

Specifically, the surfactant is selected from one or more of soybean lecithin, egg yolk lecithin, dipalmitoyl phosphatidylcholine, dioleoyl lecithin, palmitoyl lysolecithin, myristoyl lysolecithin, stearoyl lysolecithin, dimyristoyl lecithin, 1-palmitoyl-2-oleoyl lecithin, dicaretitoyl lecithin, dicetyl phosphatidyl, stearoyl, phosphatidic acid, dipalmitoyl choline, distearoyl choline, phosphatidylcholine, dimyristoyl phosphatidylcholine, distearoyl phosphatidylcholine and the like.

The sterol is selected from one or more of cholesterol, sitosterol, stigmasterol, campesterol and ergosterol.

An example of preparing peony seed oil nanoliposomes is given below.

1. Preparation of peony seed lipidosome:

(1) Taking 0.3g of egg yolk lecithin and 0.05g of cholesterol, placing the egg yolk lecithin and the cholesterol on a constant temperature magnetic stirrer, mixing the egg yolk lecithin and the cholesterol at the speed of 600r/min for 20min at the temperature of 50 ℃ and stirring the mixture uniformly to obtain an oil phase I, and cooling the oil phase I to the room temperature.

(2) Taking 0.06g of peony seed oil, adding the oil phase I, heating to 50 ℃, mixing for 20min to obtain the oil phase II, and cooling to room temperature.

(3) 3ml of glycerol was taken and added to 150ml of distilled water, which was preheated to 50℃to give a water phase.

(4) Adding the water phase into the oil phase II, mixing at 50deg.C and 600r/min for 10min, and incubating for 30min. Homogenizing the mixed solution at 10000r/min for 2min to obtain colostrum.

(5) And (3) performing ultrasonic treatment on the colostrum through a probe for 6min in a mode of 1s/2s with 400W power to obtain the peony seed oil nano liposome dispersion liquid.

2. Determination of peony seed oil liposome particle size, PDI, zeta potential and encapsulation efficiency

Diluting the prepared peony seed oil nano liposome dispersion liquid with deionized water for 10 times to prevent particles from aggregating to influence a measurement result, then filling a sample into a specific sample cell, and measuring the particle size distribution, the polydispersity coefficient and the Zeta potential of the sample by adopting a An Dongpa Litesizer TM500 type nano particle size and Zeta potential analyzer.

The encapsulation efficiency determination method adopts an organic solvent extraction method: 5mL of peony seed oil plastid is removed to a centrifuge tube, 10mL of normal hexane is added to extract free oil, and the mixed solution is centrifuged at 4000rpm/min for 20min. The supernatant was measured for absorbance A at 234nm, absorbance A0 was measured for blank liposomes after extraction by the same method, and ΔA (a-A0) was calculated. The free oil content was calculated by standard curve and the total oil content was calculated by initial addition of oil content.

EE% = (total oil content-free oil content)/total oil content

The results are shown in Table 1, FIG. 1 and FIG. 2, and the obtained peony seed oil liposome has a particle size of 275.6.+ -. 0.45, a PDI value of 0.203 and below 0.3, which indicates that the particle size uniformity is good. The Zeta potential is-28.4+/-0.45 mV, and the absolute value is close to 30mV, which indicates that the surface of the liposome has more charge, and the liposome particles can repel each other, so that higher physical stability is maintained.

TABLE 1 particle size (nm), polydispersity index PDI, zeta potential (mV), encapsulation efficiency (%)

The invention combines the hot melting method, the homogenization technology and the ultrasonic technology, the obtained nano liposome has higher encapsulation efficiency, smaller particle size, high uniformity of particle size and high vesicle charge number, the particle size of the liposome is further reduced, the encapsulation efficiency of the liposome is improved, and the transdermal absorption rate can be increased.

3. Morphological characterization of peony seed oil liposome

Pretreating peony seed lipidosome by adopting a phosphotungstic acid negative staining method, taking a proper amount of sample, dripping the sample on a copper net for 4min, sucking the redundant sample at the edge by using filter paper, staining by using 1% phosphotungstic acid solution for 2min, sucking the redundant solution at the edge by using filter paper, naturally airing, and observing the morphological structure of the lipidosome by using a transmission electron microscope, wherein the accelerating voltage is 80kV. The results are shown in FIG. 3.

As is clear from the TEM images, as shown in fig. 3 (a) and 3 (b), the peony seed oil liposome was spherical, and a clear liposome-specific fingerprint structure was observed in the inside, and the particle size was about 270nm, which was consistent with the particle size measurement results in table 1.

s1, adding 0.05-3 parts of thickener into 42-49 parts of water, soaking the thickener in water, and standing for 1-2 hours to obtain a mixed solution A;

uniformly dispersing 0.01-2 parts of sodium hyaluronate with 1-5 polyalcohols, adding the dispersed sodium hyaluronate into 42-49 parts of water, stirring and heating until the sodium hyaluronate is completely dissolved to obtain a mixed solution B; heating the mixed solution B to 60 ℃, adding 0.5-1 part of p-hydroxyacetophenone and 0.5-1 part of 1, 2-hexanediol, stirring and heating until the mixed solution B is completely dissolved, and obtaining a mixed solution C;

s3, cooling the mixed solution D to 42-45 ℃, adding 0.5-5 parts of peony seed oil nanoliposome, and stirring until the mixture is uniformly dispersed to obtain a mixed solution E;

The thickener is one of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, ammonium acryloyldimethyl taurate/VP copolymer or polyacrylate cross-linked polymer-6;

when the thickener is acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, in the step S3, after the mixed solution D is cooled to 42-45 ℃, adding an alkaline neutralizer, stirring to form uniform gel, then adding 0.5-5 parts of peony seed oil nano-liposome and 0-1 part of daily essence, and stirring until the mixture is uniformly dispersed.

When the thickener is acrylamide dimethyl taurate/VP copolymer or polyacrylate crosslinked polymer-6, 0.5-5 parts of peony seed oil nanoliposome and 0-1 part of daily essence are added in sequence, and stirred until the mixture is uniformly dispersed.

Example 1

the preparation method specifically comprises the following steps of:

s1, adding 0.2 part of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer into 47 parts of water, soaking an ammonium acryloyldimethyl taurate/VP copolymer in water, and standing for 1h to obtain a mixed solution A;

uniformly dispersing 0.08 part of sodium hyaluronate with 3 parts of glycerol, adding the mixture into 47 parts of water, stirring and heating until the mixture is completely dissolved to obtain a mixed solution B; heating the mixed solution B to 60 ℃, adding 0.6 part of p-hydroxyacetophenone and 0.6 part of 1, 2-hexanediol, stirring and heating until the mixed solution B is completely dissolved to obtain a mixed solution C;

s2, adding the mixed solution C into the mixed solution A, stirring and heating to 75 ℃, continuously stirring until the mixed solution is completely dissolved, and preserving heat for 20min to obtain a mixed solution D;

s3, cooling the mixed solution D to 42 ℃, adding 1 part of peony seed oil nanoliposome, and stirring until the mixture is uniformly dispersed to obtain a mixed solution E;

Example 2

the preparation method specifically comprises the following steps of:

s1, adding 0.3 part of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer into 46.8 parts of water, soaking an ammonium acryloyldimethyl taurate/VP copolymer in water, and standing for 2 hours to obtain a mixed solution A;

uniformly dispersing 0.05 part of sodium hyaluronate with 2 parts of glycerol and 2 parts of 1, 3-butanediol, adding into 47 parts of water, stirring and heating until the sodium hyaluronate is completely dissolved to obtain a mixed solution B; heating the mixed solution B to 60 ℃, adding 0.55 part of p-hydroxyacetophenone and 0.55 part of 1, 2-hexanediol, stirring and heating until the mixture is completely dissolved to obtain a mixed solution C;

s2, adding the mixed solution C into the mixed solution A, stirring and heating to 80 ℃, continuously stirring until the mixed solution is completely dissolved, and preserving the temperature for 30min to obtain a mixed solution D;

s3, cooling the mixed solution D to 45 ℃, adding 1 part of peony seed oil nanoliposome, and stirring until the mixture is uniformly dispersed to obtain a mixed solution E;

Examples 3 and 4 refer to table 2 and the preparation process of example 2.

Example 5

the preparation method specifically comprises the following steps of:

s1, adding 1 part of ammonium acryloyldimethyl taurate/VP copolymer into 45.2 parts of water, soaking the ammonium acryloyldimethyl taurate/VP copolymer in water, and standing for 1h to obtain a mixed solution A;

uniformly dispersing 0.1 part of sodium hyaluronate with 4 parts of glycerin, adding the mixture into 45.2 parts of water, stirring and heating the mixture until the mixture is completely dissolved to obtain a mixed solution B; heating the mixed solution B to 60 ℃, adding 0.6 part of p-hydroxyacetophenone and 0.6 part of 1, 2-hexanediol, stirring and heating until the mixed solution B is completely dissolved to obtain a mixed solution C;

s3, cooling the mixed solution D to 42 ℃, adding 3 parts of peony seed oil nanoliposome and 0.3 part of daily essence, and stirring until the mixture is uniformly dispersed to obtain a mixed solution E;

Example 6 see the ingredients of table 2 and the preparation process of example 5.

Example 7

the preparation method specifically comprises the following steps of:

s1, adding 0.8 part of ammonium acryloyldimethyl taurate/VP copolymer into 46.4 parts of water, soaking the ammonium acryloyldimethyl taurate/VP copolymer in water, and standing for 1h to obtain a mixed solution A;

uniformly dispersing 0.05 part of sodium hyaluronate with 2 parts of glycerol and 1 part of 1, 3-butanediol, adding into 46.4 parts of water, stirring and heating until the sodium hyaluronate is completely dissolved to obtain a mixed solution B; heating the mixed solution B to 60 ℃, adding 0.6 part of p-hydroxyacetophenone and 0.6 part of 1, 2-hexanediol, stirring and heating until the mixed solution B is completely dissolved to obtain a mixed solution C;

s3, cooling the mixed solution D to 42 ℃, adding 2 parts of peony seed oil nanoliposomes, and stirring until the mixture is uniformly dispersed to obtain a mixed solution E;

Examples 8-9 see the components of table 3 and the preparation process of example 7.

Example 10

the preparation method specifically comprises the following steps of:

s1, adding 2.5 parts of polyacrylate crosslinked polymer-6 into 46.83 parts of water, soaking an ammonium acryloyldimethyl taurate/VP copolymer in water, and standing for 1h to obtain a mixed solution A;

uniformly dispersing 0.05 part of sodium hyaluronate with 2 parts of glycerol and 2 parts of 1, 3-butanediol, adding into 45 parts of water, stirring and heating until the sodium hyaluronate is completely dissolved to obtain a mixed solution B; heating the mixed solution B to 60 ℃, adding 0.5 part of p-hydroxyacetophenone and 0.5 part of 1, 2-hexanediol, stirring and heating until the mixed solution B is completely dissolved to obtain a mixed solution C;

s3, cooling the mixed solution D to 42 ℃, adding 0.5 part of peony seed oil nanoliposome, and stirring until the mixture is uniformly dispersed to obtain a mixed solution E;

Examples 11 to 12 see the components of table 3 and the preparation process of example 10.

TABLE 2

TABLE 3 Table 3

Product safety and efficacy evaluation

1. Safety test:

1) Human body sealing patch test:

(1) Number of test persons: 30 people

(2) Sample numbers are shown in table 4:

TABLE 4 Table 4

Sample numbering	0	1	2	3
					Formulation of	Purified water	Example 2	Example 5	Example 12

The formula selection basis is as follows: under the condition of different thickening agents, the preparation of the embodiment with higher addition amount of the peony free nanoliposome is selected for testing, and purified water is used as a negative control.

(3) The operation method comprises the following steps:

(1) the left forearm flexor side of the subject was marked with a 3cm x 3cm area and sterilized with 75% alcohol, keeping the marked area dry;

(2) spot tester cell numbers 0-2, and the test substances were placed in spot tester cells No. 0, 1,2, and 3, respectively, in an amount of 0.020-0.025 g, as shown in fig. 4, to ask the subject to feel, and the test period was prohibited from bathing.

(3) After 24 hours, the spot tester of the test object is removed, and after the indentation disappears, the skin reaction is observed.

(4) Judgment standard

TABLE 5 skin adverse reaction grading criteria

If more than 2 skin adverse reactions occur in 1 of 30 people or more than 2 people (including 2 people) and 1 skin adverse reaction occurs in 2 people, the sample is at risk of sensitization to the subject, and the patch test is not passed.

(5) Verification result

TABLE 6 human skin patch test results

The test proves that no skin adverse reaction (+/-) occurs in 30 volunteers, and the human body patch tests of the test No. 1, the test No. 2 and the test No. 3 are all passed according to the judging standard, so that the human body patch has no sensitization risk.

2) General human body trial

(1) The service time is as follows: 9/11/2020-9/13/2020

(2) Reporting time: 2020, 9 and 14 days

(3) Volunteer population: 48 people

(4) Volunteer information, see table 7:

TABLE 7

(5) Test formulation

Example 7

(6) Verification results and analysis

(1) Safety evaluation

Question \selectionItems	Without any means for	In general	Obvious and obvious	Severe severity of
					Redness	48(100％)	0(0％)	0(0％)	0(0％)
Heating up	48(100％)	0(0％)	0(0％)	0(0％)
					Itching of the skin	48(100％)	0(0％)	0(0％)	0(0％)
Stimulation(s)	48(100％)	0(0％)	0(0％)	0(0％)
					Pimple (pimple)	48(100％)	0(0％)	0(0％)	0(0％)

Among 48 persons verified at this time, no skin adverse reaction occurred. And according to the judgment standard, the security verification passes.

(2) Experience assessment

Question/option	Is very satisfactory	Satisfactory satisfaction	In general	Dissatisfaction with
					Skin feel	12(25％)	35(72.92％)	1(2.08％)	0(0％)
Comfort level	14(29.17％)	32(66.67％)	2(4.17％)	0(0％)
					Absorption effect	13(27.08％)	33(68.75％)	2(4.17％)	0(0％)
Moisturizing effect	12(25％)	33(68.75％)	3(6.25％)	0(0％)

In terms of experience, among 48 people who are authenticated this time, 1) for "skin feel", 47 people indicate "satisfactory" or "very satisfactory"; 1 person indicates "general";

2) For "comfort", 46 means "satisfactory" or "very satisfactory"; 2 represents "general";

3) For "absorbent effect", 46 means "satisfactory" or "very satisfactory"; 2 people represent "general";

4) For "moisturizing effect", 45 means "satisfactory" or "very satisfactory"; 3 persons mean "general".

The satisfaction of the test sample in the aspects of skin feel, comfort level, absorption effect and moisturizing effect is 98%, 96% and 94% respectively, and the overall satisfaction is higher, so that the use experience of the test sample is good.

(3) Overall evaluation of the product

Of the 48 volunteers tested this time, 47 selected "satisfactory" or "very satisfactory", and 1 indicated "general", with a satisfaction of 98%.

2. Efficacy testing

(1) 10 volunteers were selected for efficacy testing with the following test formulation:

(2) Volunteer basic information:

sequence number	Sex (sex)	Skin type	History of allergy
				Volunteer
1	Man's body	Resistance to miscibility	Never before
				Volunteer 2	Female	Sensitivity to mixing	Frequent allergies
Volunteer 3	Female	Resistance to miscibility	Never before
				Volunteer 4	Female	Oily tolerance	Very few
Volunteer
	5	Female	Sensitivity to mixing	Never before
Volunteer 6					Female	Sensitivity to mixing	Very few
	Volunteer
7		Female	Sensitivity to mixing	Allergy to specific environments or substances only
	Volunteer 8				Man's body	Sensitivity to mixing	Never before
Volunteer 9		Female	Oily tolerance	Very few
	Volunteer 10				Female	Sensitivity to mixing	Allergy to specific environments or substances only

(3) The using method comprises the following steps:

volunteers were subjected to half-face control tests, with the left face using the test group product, the right face using the control group product, and continued for 28 days, and the skin of the left and right faces of the volunteers were examined on

days

0, 7, 14, and 28, respectively. The volunteers avoid sun exposure, stay up and have light diet during the test period, and do not take health care products with the effects of whitening, anti-aging and the like, and the skin care products use matrix skin care products (do not contain effective components of whitening, anti-aging, repairing and the like).

(4) The detection indexes comprise: the skin moisture loss rate, the skin melanin content and the skin collagen density are measured by using a German CK skin multifunctional tester (CK-MPA 10), wherein the test is performed by fixing points, taking 3 points from one cheek, and the result is the average value of 3 points.

(5) The detection results are as follows:

1) Transepidermal water loss (TEWL) test probe is a moisture loss test probe in g/hm ² : before measurement, the tester cleans the face with warm water, and sits for 30 minutes in an environment with humidity of 40-60% at 20+ -1deg.C.

The transepidermal water loss (TEWL), which is the amount of water lost through the epidermis, is one of the important indicators for evaluating the barrier function of skin. When the skin's keratinous barrier is incomplete, moisture can flow through the keratinous layer, a so-called "lock-in" in daily life. In the brick wall structure of the stratum corneum, the stratum corneum barrier can be repaired by supplementing intercellular lipids, and the transepidermal water loss rate can be reduced.

The experimental results show that after 10 volunteers use the samples of the test group, the reduction rate of the TEWL value of the left cheek is 4.7% -21.4%, the total effective rate is 100%, the reduction rate of the TEWL value of the right cheek of the control group is-5.3% -8.0%, and the total effective rate is 80%. And for each subject, the improvement of the cheek TEWL value on the left side is better than that on the right side, and the average height is 9.6 percent, which indicates that compared with a control group, after the essence containing 2% of liposome embedding is used, the skin cutin barrier is better repaired, the transepidermal water loss rate is reduced, namely the skin water retention capacity is improved, the skin self moisture retention performance is improved, and the skin health degree is improved. The improvement of the skin barrier function of the control group mainly derives from sodium hyaluronate, which indicates that the improvement effect of the peony seed oil nanoliposome on the skin trans-epidermal water loss rate is superior to that of sodium hyaluronate, and the synergistic effect of the peony seed oil nanoliposome and the sodium hyaluronate is not excluded.

2) Skin melanin content, the test probe is a skin color test probe, a tester cleans the face with warm water before measurement, and the test probe is used for measurement after sitting still for 30 minutes in an environment with humidity of 40% -60% and 20+/-1 ℃. The results were as follows:

the darkness, color spots, acne marks and the like of the human skin are directly related to pigmentation, and the change of the melanin content in the human skin before and after the sample is used can be directly judged, so that the effect of the used sample on the pigmentation of the skin can be directly judged. From the above table, after 10 volunteers use the samples of the test group, the reduction rate of the content of the cheek melanin at the left side is-4.1% -25.2%, the total effective rate is 90%, wherein the face of the volunteer 1 is provided with color spots, the face of the volunteer 7 is provided with acne marks, the reduction rate of the cheek skin melanin at the left side of the two

volunteers

1 and 7 is more than 25%, which indicates that after the essence containing 2% peony seed oil nanoliposome is used, the improvement effect on skin pigmentation is achieved, and the improvement effect on the skin with color deposition problems such as color spots, acne marks and the like is more remarkable. The right cheek of the control group showed irregular melanin decline, and no effect of lightening pigmentation was considered.

3) The skin elasticity test probe is an elastic fiber tissue test probe, a tester cleans the face with warm water before measurement, and the tester sits still for 30 minutes under the environment of 20+/-1 ℃ and humidity of 40-60 percent. The results were as follows:

the index is measured to be the collagen fiber density of the dermis layer, and when the measured value is increased, the increase of the collagen fiber density, namely the increase of the collagen content of the skin and the increase of the skin elasticity, indicates that the product has good effects of increasing the skin elasticity and resisting aging. From the above table, after 10 volunteers use the samples of the test group, the increase rate of the collagen density of the left cheek is 0.4% -28.7%, the total effective rate is 100%, and after all the subjects use the samples for 28 days continuously, the collagen density of the skin is increased, which means that after the 2% peony seed oil nano liposome essence is used, the collagen density of the skin is increased, namely the collagen content is increased, and the skin is more young. The right cheek of the control group is used, the increase rate of the collagen density is-3.4% -8.3%, the overall irregularity can be considered to have no obvious effect on increasing collagen meter, and the decrease of the collagen density can be related to factors such as life habits. Therefore, the peony seed oil nano-liposome has good effects of increasing the collagen content of skin and improving the skin elasticity.

The outermost layer of the epidermis layer of human skin, namely the stratum corneum, is formed compact 'brick wall structure' by keratinocyte and intercellular lipid together, forms permeability barrier at the skin top layer, prevents the inside moisture of skin from volatilizing on the one hand, prevents external harmful substance invasion on the other hand, however, simultaneously, also directly has influenced the penetration absorption to the deep skin of the efficacy composition in the skin care product. How to improve the transdermal absorption rate of the functional components is always a key and difficult point of the efficacy of skin care products and even topical medicines. The liposome embedding technology is applied to the functional components which are not easy to permeate the skin horny layer, so that the transdermal absorption rate of the functional components is increased, and the skin care effect is greatly improved.

The complete peony seed oil nano-liposome has a certain targeting effect on skin, can penetrate through a cutin barrier to enter the deep layer of the skin, and meanwhile, because of the amphiphilicity of the liposome, the liposome-embedded components have higher osmotic absorptivity than water-based or oil-based components, that is, the peony seed oil nano-liposome can realize higher transdermal absorptivity than the peony seed oil in essential oil or emulsion, and the liposome has better affinity with a bilayer on the surface of a cell, even fuses with the lipid of the cutin layer, so that the lipid structure of the cutin layer is changed, a granular structure with gaps is formed, holes, cracks and folds are formed, and the functional components can enter the deep layer of the skin through the holes and the cracks. Therefore, the peony seed oil nanoliposome is beneficial to the transdermal absorption of other functional components while maintaining the self-high transdermal absorption rate. Therefore, the peony seed oil nanoliposome is added into the water-based essence, so that the skin care effect of the peony seed oil can be maximally realized, and the absorption of other nutrient components in the water-based essence can be promoted.

Besides being easier to penetrate through the stratum corneum penetration barrier, the peony seed oil nanoliposome can also penetrate through skin accessory structures such as hair follicles, sebaceous glands and the like to be absorbed by the skin, and the absorption rate of the peony seed oil nanoliposome penetrating through the hair follicles is 5-8 times that of a common water-based product.

The peony seed oil nano liposome also has a certain slow release effect, and can form a temporary 'warehouse' in the epidermis and even the dermis layer, so that the effective components in the peony seed oil can be directly and permanently released.

Claims

1. The repair essence containing the peony seed oil nano liposome is characterized by comprising the following components in percentage by mass:

80% -94% of water;

1.0% -5.0% of polyalcohol;

0.1% -3% of thickener;

0.5% -1% of p-hydroxyacetophenone;

0.5% -1% of 1, 2-hexanediol;

0.01% -0.2% of sodium hyaluronate;

0.5% -5.0% of peony seed oil nanoliposome;

0-0.5% of daily essence;

the preparation method of the peony seed oil nano liposome specifically comprises the following steps:

(1) Weighing 24 parts of surfactant, 2.4-12 parts of cholesterol and 2.4-12 parts of peony seed oil according to parts by weight; the surfactant is selected from soybean lecithin or egg yolk lecithin;

(2) Mixing and stirring a surfactant and cholesterol to obtain an oil phase I, and then cooling to room temperature;

2. The repair essence containing peony seed oil nanoliposomes according to claim 1, wherein the thickener is acrylic acid (esters)/C10-30 alkanol acrylate cross-linked polymer, ammonium acryloyldimethyl taurate/VP copolymer or polyacrylate cross-linked polymer-6;

3. The repair essence containing peony seed oil nano-liposomes according to claim 2, wherein the alkaline neutralizing agent is sodium hydroxide or triethanolamine, and the mass ratio of sodium hydroxide to acrylic acid (esters)/C10-30 alkanol acrylate cross-linked polymer is 0.4:1 when sodium hydroxide is adopted;

4. The repair essence containing peony seed oil nanoliposomes according to claim 1, wherein the polyol is one or more of glycerol, 1, 3-butanediol and 1, 2-pentanediol.

5. The repair essence containing peony seed oil nanoliposome according to claim 1, wherein the particle size of the peony seed oil nanoliposome is 212-332 nm, and the encapsulation rate of the nanoliposome is 79% -96%.

6. A method for preparing the repair essence containing peony seed oil nanoliposomes according to any one of claims 1 to 5, comprising the following steps:

s1, adding a thickener into water, soaking the thickener in the water, and standing for 1-2 hours to obtain a mixed solution A;

uniformly dispersing sodium hyaluronate with polyalcohol, adding into water, stirring and heating to dissolve completely to obtain mixed solution B; heating the mixed solution B to 60 ℃, adding p-hydroxyacetophenone and 1, 2-hexanediol, stirring and heating until the mixed solution B is completely dissolved, and obtaining a mixed solution C;

s3, cooling the mixed solution D to 42-45 ℃, adding peony seed oil nanoliposomes, and stirring until the mixed solution D is uniformly dispersed to obtain a mixed solution E;

s3, the preparation method of the peony seed oil nanoliposome specifically comprises the following steps:

(6) Performing ultrasonic dispersion on the colostrum to obtain peony seed oil nanoliposome;

7. The preparation method according to claim 6, wherein the thickener is one of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, ammonium acryloyldimethyl taurate/VP copolymer or polyacrylate cross-linked polymer-6;

8. The preparation method of claim 6, wherein the mass ratio of the surfactant, the cholesterol and the peony seed oil is 6:1:1.

9. The method according to claim 6, wherein the homogenization is carried out at a rotational speed of 10000-20000 r/min.