CN114306191B

CN114306191B - Natural plant sun cream and preparation method thereof

Info

Publication number: CN114306191B
Application number: CN202210107521.1A
Authority: CN
Inventors: 庞艳阳; 王冬菊; 王武
Original assignee: Hainan Medical College
Current assignee: Hainan Medical College
Priority date: 2022-01-28
Filing date: 2022-01-28
Publication date: 2024-01-09
Anticipated expiration: 2042-01-28
Also published as: CN114306191A

Abstract

The invention provides a preparation method of natural plant sun cream, which is prepared from a component A, a component B and a component C in a mass ratio of 0.1-0.3:1.3-1.5:2-2.2, wherein the component A consists of a curcuma zedoary extract, a fructus amomi extract and a roselle flower extract; the component B consists of triacontyl PVP, bisabolol, dipotassium glycyrrhizinate, octyl polymethylsiloxane and dipropylene glycol; the component C is prepared from sunflower seed oil, hydrogenated C6-14 alkene polymer, tetrahydropyrimidine carboxylic acid and glycerin by different methods according to the effects of different components in the sun cream, and the sun cream prepared by the method has good stability, and the effective sun cream has an effective sun time of up to 4 hours and a sun factor of SPF50+ and PA++.

Description

Natural plant sun cream and preparation method thereof

Technical Field

The invention relates to the field of sun cream, in particular to a preparation method of natural plant sun cream.

Background

The wavelength range of ultraviolet radiation (UVR) is 100 to 400nm, and is classified into short wavelength (UVC, 100 to 290 nm), medium wavelength (UVB, 280 to 320 nm) and long wavelength ultraviolet (UVA, 320 to 400 nm) according to the length of the wavelength. Ultraviolet rays with certain intensity can disinfect and sterilize, promote bone development and play a positive role in the growth of human bodies, animals and plants. Skin is the physiological barrier of the body, protecting the body from pathogens, chemical or physical damage, but it is also most susceptible to uv damage. Excessive uv irradiation can lead to oxidative stress of the skin: skin erythema, pigmentation, skin aging, photosensitization, and even induction of skin tumors. Wherein UVA can cause skin dryness, wrinkling, loss of elasticity, and induce photoaging manifestations such as melanin pigmentation, belonging to chronic photodamage; UVB can cause acute photodamage such as skin erythema, photoreaction, solar dermatitis, and skin cancer.

At present, the exogenous ultraviolet rays on the market are mainly reflected on sun-screening products, and chemical components are mostly limited on macromolecular proteins or bran peptides. The sun-screening agent has two physical sun-screening and chemical sun-screening functions, namely, the chemical sun-screening agent plays a role in protecting skin by absorbing ultraviolet rays, and the main components of the chemical sun-screening agent are camphor, cinnamate, salicylic acid, benzoate, benzene ketone, triazine, benzoxazole and alkane, and alcohols are used as matrixes, but the chemical sun-screening agent is easy to cause secondary skin diseases such as contact dermatitis and the like, and also can cause adverse effects such as neurotransmitter change, estrogen-like action, thyroxine metabolism interference and the like. The physical sun-screening agent, namely ultraviolet screening agent, is mainly inorganic particles such as titanium dioxide, zinc oxide particles, silicate and ferric oxide, which are opaque particles, can be white on the skin and remain solid sticky groups, and form a sealing film after being coated, so that pores are easily blocked, and sebum overflow disorder is caused, and skin diseases are induced or aggravated. There are also currently technical solutions for applying plant extracts to sunscreens, for example: CN201710128685.1: a preparation method of radix Angelicae Dahuricae compound plant cool sun cream comprises adding radix Angelicae Dahuricae essential oil, glycerol Huang Caotong, green tea essential oil, herba Menthae essential oil, flos Lonicerae essential oil and hydrogenated castor oil into sun cream; CN201710129070.0: a method for preparing compound plant whitening sunscreen cream comprises adding propolis, licoflavone, flos Sophorae Immaturus essential oil, and Curcuma rhizome essential oil into the preparation of sunscreen cream. The sun cream does not describe the effect of repairing the skin after sun, so that the sun cream with sun protection effect and after sun repair effect is needed to reduce the damage of ultraviolet rays to the skin.

Disclosure of Invention

Therefore, the invention provides a preparation method of the natural plant sun cream, and the sun cream prepared by the preparation method not only has sun-proof effect, but also has post-sun repair effect.

The technical scheme of the invention is realized as follows:

the natural plant sun cream is prepared from a component A, a component B and a component C in a mass ratio of 0.1-0.3:1.3-1.5:2-2.2, wherein the component A, the component B and the component respectively comprise the following raw materials: the component A is curcuma zedoary extract, amomum villosum extract and roselle flower extract, and the component B is prepared from the following components in parts by weight: 1-3 parts of triacontyl PVP, 0.3-0.5 part of bisabolol, 1.5-2.5 parts of dipotassium glycyrrhizinate, 3-4 parts of octyl polymethyl siloxane and 5-7 parts of dipropylene glycol, wherein the component C comprises the following components in parts by weight: 7-9 parts of sunflower seed oil, 3-5 parts of hydrogenated C6-14 alkene polymer, 1-1.5 parts of tetrahydropyrimidine carboxylic acid and 15-17 parts of glycerol.

Further, the preparation method of the natural plant sun cream comprises the following steps:

(1) The preparation method of the phase A comprises the following steps:

s1: mixing a magnesium chloride solution, an aluminum chloride solution and deionized water in a volume ratio of 4-6:1.5-1.9:3-3.5 to prepare a suspension 1, stirring a sodium hydroxide solution by 950-1050rpm, adding the suspension 1 into the sodium hydroxide solution while stirring, after all the suspension 1 is added, preparing a suspension 2 by magnetic stirring for 5.5-6.5 hours, centrifuging the suspension 2 by using 4500-5500g for 4-6min, discarding the supernatant, collecting a precipitate 1, adding 3.5-4.5 times the volume of the suspension 1 into the precipitate 1, centrifuging the precipitate 1 by using 4500-5500g for 4-6min, discarding the supernatant, collecting the precipitate 2, adding 3.5-4.5 times the volume of the suspension 1 into the precipitate 2, and resuspending the ultrapure water to prepare the layered double hydroxide nanomaterial;

s2: preparing magnesium chloride hexahydrate and aluminum chloride hexahydrate into a salt solution with the molar ratio of magnesium to aluminum being 3:1 by using deionized water, wherein the mass ratio of feed liquid of the deionized water to the total mass of the magnesium chloride hexahydrate and the aluminum chloride hexahydrate is 5:1, stirring a sodium hydroxide solution in a nitrogen atmosphere, adding the salt solution into the mixture solution in the stirring process to prepare a mixed solution 1, wherein the volume ratio of the salt solution to the sodium hydroxide solution is 1:4, placing the mixed solution 1 into a water bath kettle with the temperature of 55-65 ℃ for stirring for 5-6h, centrifuging 4500-5500g of the mixed solution 1 after water bath stirring for 4-6min by using a centrifugal force, discarding supernatant, and collecting precipitate 3;

s3: weighing the curcuma zedoary extract, the amomum villosum extract and the roselle flower extract, adding the curcuma zedoary extract, the amomum villosum extract and the roselle flower extract into a sodium hydroxide solution, stirring until the materials are dissolved, preparing a mixed solution 2, wherein the mass concentration of the curcuma zedoary extract, the amomum villosum extract and the roselle flower extract in the mixed solution 2 is 7-8mg/mL, centrifuging the mixed solution 2 for 4-6min by using a centrifugal force of 4500-5500g, discarding the supernatant, and collecting a precipitate 4;

s4: mixing a layered double hydroxide nano material, a precipitate 3 and a precipitate 4 in a water bath, preparing a layered double hydroxide nano material mixed solution according to the usage amount of a sodium hydroxide solution, wherein the ratio of the layered double hydroxide nano material to the precipitate 3 to the precipitate 4 is 1:1:1, transferring the layered double hydroxide nano material mixed solution into water at 100 ℃, heating the water bath for 15-17h, naturally cooling, washing the water bath for 2 times by using deionized water, the volume ratio of the deionized water to the layered double hydroxide nano material mixed solution is 4:1, collecting precipitate 5, and re-suspending the precipitate 5 in the water to prepare a layered double hydroxide nano material particle suspension;

s5: adding a layered double hydroxide nano material particle suspension into an epidermal growth factor receptor nano antibody aqueous solution, wherein the concentration of the epidermal growth factor receptor nano antibody aqueous solution is 0.1-1mol/L, the mass ratio of the layered double hydroxide nano material particle suspension to the epidermal growth factor receptor nano antibody aqueous solution is 1:2-3, and magnetically stirring for 20-40min at 950-1050rpm to obtain a phase A;

(2) And B phase: adding the raw materials of the component B and water into a water phase pot, wherein the mass ratio of the raw materials of the component B to the water is 1:0.8-1.2, heating to 50-60 ℃, and stirring for 20-30min by using 50-70r/min to obtain a phase B;

(3) And C phase: adding the raw materials of the component C into an oil phase pot, heating to 70-80 ℃, and stirring for 10-15min by using 80-120r/min to obtain a C phase;

(4) Adding the phase A, the phase B and the phase C into the same container according to a certain proportion, stirring for 10-15min by using 200-220r/min to obtain a mixture 1, dispersing the mixture 1 for 1-3min by using a high-speed dispersing machine, wherein the rotating speed of the dispersing machine is 1200-1300r/min, homogenizing the dispersed mixture 1 for 5-8min by using a high-pressure homogenizer, and homogenizing the mixture under 30-35MPa to obtain a finished product.

Further, in step S1, the concentration of the magnesium chloride solution and the aluminum chloride solution is 0.5-0.7mol/L, and in steps S1, S2 and S3, the concentration of the sodium hydroxide solution is 0.15mol/L.

Further, the preparation method of the curcuma zedoary extract comprises the following steps:

(1) Pulverizing Curcumae rhizoma with superfine pulverizer, and sieving with 50 mesh sieve to obtain Curcumae rhizoma powder;

(2) Placing Curcumae rhizoma powder in a pressurized extraction tank, adding 10-15% ethanol solution, pressurized extracting at a mass ratio of 5-8:1 under 0.4-0.45MPa for 1-2 hr, and collecting supernatant to obtain Curcumae rhizoma crude extract;

(3) Decolorizing the crude extract of Curcumae rhizoma with active carbon at a mass ratio of 10:0.5 for 10-20min, filtering, and drying to obtain the extract.

Further, the preparation method of the fructus amomi extract comprises the following steps:

(1) Pulverizing fructus Amomi with superfine pulverizer, and sieving with 50 mesh sieve to obtain fructus Amomi powder;

(2) Putting fructus Amomi powder into a pressurized extraction tank, and adding a feed liquid ratio of 1g: mixing 20-30mL of water to obtain fructus Amomi powder solution, extracting under pressure of 0.6-0.8MPa for 30-40min, collecting supernatant, and concentrating under reduced pressure to a density of 0.8-1.2g/mL to obtain concentrated solution;

(3) Soaking the concentrated solution in 1mol/L sodium hydroxide solution for 3-4h, wherein the mass ratio of the concentrated solution to the sodium hydroxide solution is 1:1-1.5, and preparing extract 1;

(4) Eluting the extract 1 with macroporous resin, eluting with 20% ethanol solution with an amount of 3-5 times of column volume, collecting eluate, and drying to obtain fructus Amomi extract.

Further, the preparation method of the roselle flower extract comprises the following steps:

(1) Pulverizing dried calyx Hibisci Sabdariffae to 40-80 mesh to obtain calyx Hibisci Sabdariffae powder;

(2) Mixing roselle calyx powder and deionized water, wherein the ratio of the roselle calyx powder to the deionized water is 1g:80-120mL, carrying out reflux extraction for 2-3 times at 80-90 ℃ for 80-100min each time, collecting an extracting solution, and concentrating the extracting solution under reduced pressure until the density is 1.5-1.7g/mL to obtain roselle calyx concentrated solution;

(3) Adding malic acid into the roselle calyx concentrated solution, and then carrying out ultrasonic treatment for 20-40min at 40-50kHz at 60-70 ℃, wherein the mass ratio of the malic acid to the roselle calyx concentrated solution is 0.1-0.3:10, so as to obtain the roselle calyx concentrated solution after ultrasonic treatment;

(4) Adding 5-7% of active carbon according to the mass of the roselle calyx concentrated solution after ultrasonic treatment, controlling the temperature of the concentrated solution to be 35-37 ℃, stirring for 1-2min by using 300-320r/min, stirring for 10-15min by using 60-70r/min, standing the stirred roselle calyx concentrated solution for 30-40min, filtering, collecting filtrate, and drying to obtain the roselle calyx extract.

Further, the sun cream is prepared from a component A, a component B and a component C in a mass ratio of 0.2:1.4:2.1, wherein the component A, the component B and the component respectively consist of the following raw materials: the component A is curcuma zedoary extract, amomum villosum extract and roselle flower extract, and the component B is prepared from the following components in parts by weight: 2 parts of triacontyl PVP, 0.4 part of bisabolol, 2 parts of dipotassium glycyrrhizinate, 3.5 parts of octyl polymethylsiloxane and 6 parts of dipropylene glycol, wherein the component C comprises the following components in parts by weight: 8 parts of sunflower seed oil, 4 parts of hydrogenated C6-14 alkene polymer, 1.25 parts of tetrahydropyrimidine carboxylic acid and 16 parts of glycerol.

Compared with the prior art, the invention has the beneficial effects that: according to the invention, the fructus amomi extract, the curcuma zedoary extract and the roselle flower extract are used as active ingredients to prepare the sun cream, the epidermal growth factor receptor is used as a target, the epidermal growth factor receptor nano antibody is used as a guide antibody, and the fructus amomi extract and the curcuma zedoary extract are carried to prepare the A phase, so that the active ingredients can be quickly infiltrated into skin cells, the active ingredients can reduce the generation of excessive ultraviolet irradiation in vivo free radicals, enhance the antioxidant activity of the organism, reduce the MMPs content, maintain the dynamic balance between the oxidation of the skin bottom layer and an antioxidant system, and solve the problem that the natural extract is indissolvable in oil or water, so that the stability of a finished product is poor. According to the invention, the phase A, the phase B and the phase C are combined, so that the sun-screening cream with high stability can be obtained, the adsorption capacity of the sun-screening cream is improved, meanwhile, the phenomena of fake white and sticky skin feel do not occur after the sun-screening cream is smeared, and the effective sun-screening time of the sun-screening cream is as long as 4 hours, and the sun-screening coefficient is SPF50+, PA++.

Drawings

FIG. 1 SPF value variation curves for different time periods

FIG. 2 PFA value variation curves of different time periods

Detailed Description

In order to better understand the technical content of the present invention, the following provides specific examples to further illustrate the present invention.

The experimental methods used in the embodiment of the invention are conventional methods unless otherwise specified.

Materials, reagents, and the like used in the examples of the present invention are commercially available unless otherwise specified.

The preparation method of the A phase in examples 1-5 and comparative examples 1-2 is as follows:

(1) Mixing a magnesium chloride solution with the volume ratio of 5:1.7:3.3 and the concentration of 0.6mol/L, an aluminum chloride solution with the concentration of 0.6mol/L and deionized water, preparing a suspension 1, stirring a sodium hydroxide solution by using 1000rpm, adding the suspension 1 into the sodium hydroxide solution while stirring, after all the suspension 1 is added, magnetically stirring for 6 hours, preparing a suspension 2, centrifuging the suspension 2 by using 5000g of centrifugal force for 5min, discarding the supernatant, collecting a precipitate 1, adding 4 times of ultrapure water into the suspension by using 5000g of centrifugal force, resuspending the precipitate 1, preparing a precipitate 1 solution, centrifuging the precipitate 1 by using 5000g of centrifugal force for 5min, collecting a precipitate 2, adding 4 times of ultrapure water into the suspension by using the precipitate 2, and preparing the layered double hydroxide nanomaterial by using 4 times of the volume of the suspension.

(2) Preparing magnesium chloride hexahydrate and aluminum chloride hexahydrate into a salt solution with the molar ratio of magnesium to aluminum being 3:1 by using deionized water, stirring the salt solution with the concentration of 0.15mol/L in a nitrogen atmosphere by using the deionized water and the sodium hydroxide solution with the mass ratio of 5:1 of the magnesium to aluminum hexahydrate, adding the salt solution in the stirring process to prepare a mixed solution 1, stirring the mixed solution 1 in a water bath pot with the temperature of 60 ℃ for 5.5h by using 200r/min, centrifuging the mixed solution 1 subjected to water bath stirring for 4-6min by using the centrifugal force of 4500-5500g, discarding supernatant, and collecting precipitate 3.

(3) Weighing the curcuma zedoary extract, the amomum villosum extract and the roselle flower extract, adding the curcuma zedoary extract, the amomum villosum extract and the roselle flower extract into a sodium hydroxide solution with the concentration of 0.15mol/L, stirring until the materials are dissolved, preparing a mixed solution 2, wherein the mass concentration of the curcuma zedoary extract, the amomum villosum extract and the roselle flower extract in the mixed solution 2 is 7.5mg/mL, centrifuging the mixed solution 2 for 5min by using a centrifugal force of 5000g, discarding supernatant, and collecting a precipitate 4.

(4) Mixing the layered double hydroxide nano material, the sediment 3 and the sediment 4 in a water bath, according to the usage amount of sodium hydroxide solution, the ratio of the layered double hydroxide nano material to the sediment 3 to the sediment 4 is 1:1:1 to prepare layered double hydroxide nano material mixed solution, transferring the layered double hydroxide nano material mixed solution into water with the temperature of 100 ℃, heating the water bath for 16 hours, naturally cooling, washing the water bath for 2 times by using deionized water, the volume ratio of the deionized water to the layered double hydroxide nano material mixed solution is 4:1, collecting the sediment 5, and re-suspending the sediment 5 in the water to prepare the layered double hydroxide nano material particle suspension.

(5) Adding the layered double hydroxide nano material particle suspension into an epidermal growth factor receptor nano antibody aqueous solution, wherein the concentration of the epidermal growth factor receptor nano antibody aqueous solution is 0.5mol/L, the mass ratio of the layered double hydroxide nano material particle suspension to the epidermal growth factor receptor nano antibody aqueous solution is 1:2.5, and stirring for 30min by using 1000rpm magnetic force to prepare a phase A.

The preparation method of the curcuma zedoary extract in examples 1-5 and comparative examples 1-2 comprises the following steps:

(2) Placing Curcumae rhizoma powder in a pressurized extraction tank, adding 13% ethanol solution, pressurized extracting at a mass ratio of 7:1 under 0.43MPa for 1.5 hr, and collecting supernatant to obtain Curcumae rhizoma crude extract;

(3) Decolorizing the crude extract of Curcumae rhizoma with active carbon at a mass ratio of 10:0.5 for 15min, filtering, and drying the filtrate at 100deg.C for 5 hr to obtain the extract.

The preparation methods of the extracts of the fructus amomi in examples 1-5 and comparative examples 1-2 are:

(2) Putting fructus Amomi powder into a pressurized extraction tank, and adding 1g of fructus Amomi powder according to the weight ratio: mixing 25mL of water to obtain fructus Amomi powder solution, extracting under pressure of 0.7MPa for 35min, collecting supernatant, and concentrating under reduced pressure to obtain concentrated solution with density of 1 g/mL;

(3) Soaking the concentrated solution in a sodium hydroxide solution with the concentration of 1mol/L for 3.5 hours, wherein the mass ratio of the concentrated solution to the sodium hydroxide solution is 1:1.3, so as to prepare an extract 1;

(4) Eluting the extract 1 with macroporous resin, eluting with 20% ethanol solution with an amount of 4 times of column volume, collecting eluate, and drying the filtrate at 70deg.C for 8 hr to obtain fructus Amomi extract.

The preparation method of roselle flower extract in examples 1-5 and comparative examples 1-2 comprises the following steps:

(1) Taking dried roselle calyx, and crushing the roselle calyx to 80 meshes to obtain roselle calyx powder;

(2) Mixing roselle calyx powder and deionized water, wherein the ratio of the roselle calyx powder to the deionized water is 1g to 100mL, carrying out reflux extraction for 3 times at 85 ℃ for 90min each time, collecting an extracting solution, and concentrating the extracting solution under reduced pressure until the density is 1.6g/mL to obtain roselle calyx concentrated solution;

(3) Adding malic acid into the roselle calyx concentrated solution, and then using 45kHz ultrasonic for 30min at the ultrasonic temperature of 65 ℃, wherein the mass ratio of the malic acid to the roselle calyx concentrated solution is 0.2:10, so as to prepare the roselle calyx concentrated solution after ultrasonic treatment;

(4) Adding 5-7% of active carbon according to the mass of the roselle calyx concentrated solution after ultrasonic treatment, controlling the temperature of the concentrated solution to 36 ℃, stirring for 1.5min at 310r/min, stirring for 15min at 65r/min, standing the stirred roselle calyx concentrated solution for 40min, filtering, collecting filtrate, and drying for 6h at 85 ℃ to obtain the roselle calyx extract.

Example 1 preparation method of Natural plant sunscreen cream

The component B comprises the following components in parts by weight: 1 part of triacontyl PVP, 0.3 part of bisabolol, 1.5 parts of dipotassium glycyrrhizinate, 3 parts of octyl polymethyl siloxane and 5 parts of dipropylene glycol are weighed according to the weight parts: 7 parts of sunflower seed oil, 3 parts of hydrogenated C6-14 alkene polymer, 1 part of tetrahydropyrimidine carboxylic acid and 15 parts of glycerol are weighed for later use.

(2) And B phase: adding the raw materials of the component B and water into a water phase pot, wherein the mass ratio of the raw materials of the component B to the water is 1:0.8, heating to 50 ℃, and stirring for 20min by using 50r/min to obtain a phase B;

(3) And C phase: adding the raw materials of the component C into an oil phase pot, heating to 70 ℃, and stirring for 10min by using 80r/min to obtain a C phase;

(4) Adding the phase A, the phase B and the phase C into the same container according to the mass ratio of 0.1:1.3:2, stirring for 10min by using 200r/min to obtain a mixture 1, dispersing the mixture 1 for 1min by using a high-speed dispersing machine with the rotating speed of 1200r/min, homogenizing the dispersed mixture 1 for 5min by using a high-pressure homogenizer and the homogenizing pressure of 30MPa to obtain a finished product.

Example 2 preparation method of Natural plant sunscreen cream

(1) The component B comprises the following components in parts by weight: 3 parts of triacontyl PVP, 0.5 part of bisabolol, 2.5 parts of dipotassium glycyrrhizinate, 4 parts of octyl polymethyl siloxane and 7 parts of dipropylene glycol are weighed according to the weight parts: 9 parts of sunflower seed oil, 5 parts of hydrogenated C6-14 alkene polymer, 1.5 parts of tetrahydropyrimidine carboxylic acid and 17 parts of glycerol are weighed for later use.

(2) And B phase: adding the raw materials of the component B and water into a water phase pot, wherein the mass ratio of the raw materials of the component B to the water is 1:1.2, heating to 60 ℃, and stirring for 30min by using 70r/min to obtain a phase B;

(3) And C phase: adding the raw materials of the component C into an oil phase pot, heating to 80 ℃, and stirring for 15min at 120r/min to obtain a C phase;

(4) Adding the phase A, the phase B and the phase C into the same container according to the mass ratio of 0.3:1.5:2.2, stirring for 15min by using 220r/min to obtain a mixture 1, dispersing the mixture 1 for 3min by using a high-speed dispersing machine with the rotating speed of 1300r/min, homogenizing the dispersed mixture 1 for 8min by using a high-pressure homogenizer with the homogenizing pressure of 35MPa, and obtaining a finished product.

Example 3 preparation method of Natural plant sunscreen cream

(1) The component B comprises the following components in parts by weight: 2 parts of triacontyl PVP, 0.4 part of bisabolol, 2 parts of dipotassium glycyrrhizinate, 3.5 parts of octyl polymethyl siloxane and 6 parts of dipropylene glycol are weighed according to the weight parts: 8 parts of sunflower seed oil, 4 parts of hydrogenated C6-14 alkene polymer, 1.25 parts of tetrahydropyrimidine carboxylic acid and 16 parts of glycerol are weighed for later use.

(2) And B phase: adding the raw materials of the component B and water into a water phase pot, wherein the mass ratio of the raw materials of the component B to the water is 1:1, heating to 55 ℃, and stirring for 25min by using 60r/min to obtain a phase B;

(3) And C phase: adding the raw materials of the component C into an oil phase pot, heating to 75 ℃, and stirring for 13min by using 100r/min to obtain a C phase;

(4) Adding the phase A, the phase B and the phase C into the same container according to the mass ratio of 0.2:1.4:2.1, stirring for 13min by using 210r/min to obtain a mixture 1, dispersing the mixture 1 for 2min by using a high-speed dispersing machine with the rotating speed of 1250r/min, homogenizing the dispersed mixture 1 for 7min by using a high-pressure homogenizer and homogenizing the homogenized mixture at the homogenizing pressure of 33MPa to obtain a finished product.

Example 4 preparation method of Natural plant sunscreen cream

Based on the embodiment 3, the preparation methods of the steps (2), (3) and (4) are respectively adjusted, and the specific methods are shown in the following experimental groups:

experiment group 1: the preparation method of the adjustment step (2) comprises the following steps: adding the raw materials of the component B and water into a water phase pot, wherein the mass ratio of the raw materials of the component 3 to the water is 1:3, heating to 55 ℃, and stirring for 25min by using 60r/min to obtain a phase B.

Experiment group 2: the preparation method of the adjustment step (3) comprises the following steps: adding the raw materials of the component C into an oil phase pot, heating to 90 ℃, and stirring for 13min by using 100r/min to obtain a C phase.

Experiment group 3: the preparation method of the adjustment step (3) comprises the following steps: adding the raw materials of the component C into an oil phase pot, heating to 50 ℃, and stirring for 13min by using 100r/min to obtain a C phase.

Experiment group 4: the preparation method of the adjustment step (4) comprises the following steps: adding the phase A, the phase B and the phase C into the same container according to the mass ratio of 0.2:1:1, stirring for 13min by using 210r/min to obtain a mixture 1, dispersing the mixture 1 for 2min by using a high-speed dispersing machine, homogenizing the dispersed mixture 1 for 7min by using a high-pressure homogenizer at the rotating speed of 1250r/min, and obtaining a finished product, wherein the homogenizing pressure is 33 MPa.

Experimental group 5: the preparation method of the adjustment step (4) comprises the following steps: adding the phase A, the phase B and the phase C into the same container according to the mass ratio of 0.2:1.4:2.1, stirring for 13min by using 210r/min to obtain a mixture 1, dispersing the mixture 1 for 2min by using a high-speed dispersing machine with the rotating speed of 1250r/min, homogenizing the dispersed mixture 1 for 7min by using a high-pressure homogenizer and the homogenizing pressure of 20MPa to obtain a finished product.

The sunscreens prepared in experimental groups 1-5 were subjected to appearance and stability assays, including centrifugation tests and SPF value detection.

And the centrifugal test is to take 10mg of finished products, centrifuge for 20min at 3000r/min, and observe the properties of the finished products.

The SPF value of the sunscreen cream is detected by a sun protection factor tester (model: SPF 290 AS) according to the human body law test of cosmetic safety technical Specification.

Comparison with the results of example 1 shows that the preparation method and the proportion of component A, B, C in the invention are beneficial to improving the appearance and stability of the finished product. SPA value shows that the preparation method of the invention can also improve the sun-proof capacity of the finished product. Adjusting the ratio of component B feed to water in experimental group 1 resulted in a decrease in stability; in the experiment group 2-3, the emulsification temperature is adjusted, different raw materials have different physical properties, the emulsification effect is not good due to the fact that the temperature is too low, part of water can be recovered in the emulsification process due to the fact that the temperature is too high, the stability of a finished product is affected, the properties of part of raw materials are changed, and the sun-proof effect of the finished product is further reduced; the use proportion of the component A, the component B and the component C is adjusted in the experiment group 4, so that the appearance and the stability of the finished product are reduced; the experiment group 5 adjusts the homogenizing pressure to cause uneven particle distribution in the finished product, and the homogenizing pressure and the homogenizing time can be fully mixed by using three components, so that the appearance of the finished product is improved, and the use feeling of the finished product is further improved.

Example 5 preparation method of Natural plant sunscreen cream

On the basis of the embodiment 3, the raw materials or the proportions in the step (1) are respectively adjusted, and the specific components are shown in the following experimental groups:

experiment group 6: the component B comprises the following components in parts by weight: weighing 2 parts of triacontyl PVP, 0.4 part of bisabolol, 2 parts of dipotassium glycyrrhizinate, 2 parts of octyl polymethylsiloxane and 2 parts of dipropylene glycol, wherein the component C comprises the following components in parts by weight: 4 parts of sunflower seed oil, 4 parts of hydrogenated C6-14 alkene polymer, 4 parts of tetrahydropyrimidine carboxylic acid and 8 parts of glycerol are weighed for later use.

Experiment group 7: the component B comprises the following components in parts by weight: 2 parts of triacontyl PVP, 0.4 part of bisabolol, 2 parts of dipotassium glycyrrhizinate, 3.5 parts of octyl polymethylsiloxane and 6 parts of 1, 2-pentanediol are weighed, and the component C is calculated according to parts by weight: 8 parts of sunflower seed oil, 4 parts of diisopropyl sebacate, 1.25 parts of tocopherol and 16 parts of glycerol are weighed for later use.

Experiment group 8: the component B comprises the following components in parts by weight: 2 parts of trimethylsiloxysilicate, 0.4 part of dipotassium glycyrrhizinate, 2 parts of dipotassium glycyrrhizinate, 3.5 parts of octyl polymethylsiloxane and 6 parts of dipropylene glycol are weighed, and the component C is calculated according to parts by weight: 8 parts of sunflower seed oil, 4 parts of polydimethylsiloxane, 5 parts of sodium hyaluronate, 1.25 parts of tetrahydropyrimidine carboxylic acid and 16 parts of glycerol are weighed for later use.

The sunscreens prepared in experimental groups 6-8 were subjected to appearance and stability assays, including centrifugation tests and SPF value detection.

The detection method is described in example 5.

Experimental results show that, compared with example 1, experimental groups 6-8 change the raw material proportion or adjust the raw material types, resulting in reduced appearance and stability. The active ingredients and other components in the invention are compounded, so that the sun protection factor of the finished product can be improved, the addition of a physical sun protection agent or a chemical sun protection agent can be reduced, and the occurrence of skin damage caused by the additive can be reduced.

Comparative example 1

The preparation process of the curcuma zedoary extract is regulated, and the preparation process is specifically shown in experiment groups 9-10:

experiment group 9:

(2) Placing Curcumae rhizoma powder in a pressurized extraction tank, adding 35% ethanol solution, pressurized extracting at a mass ratio of ethanol solution to Curcumae rhizoma powder of 5:1 under 0.43MPa for 1.5 hr, and collecting supernatant to obtain Curcumae rhizoma crude extract;

Experimental group 10:

(2) Placing Curcumae rhizoma powder into a pressurized extraction tank, adding 13% ethanol solution at a mass ratio of 7:1 for 1.5 hr, and collecting supernatant to obtain Curcumae rhizoma crude extract;

Comparative example 2

Preparation method of fructus Amomi extract is adjusted, see experimental group 11-13:

experiment group 11:

(2) Putting fructus Amomi powder into a pressurized extraction tank, and adding 1g of fructus Amomi powder according to the weight ratio: mixing 25mL of water to obtain fructus Amomi powder solution, extracting under pressure of 0.4MPa for 35min, collecting supernatant, and concentrating under reduced pressure to obtain concentrated solution with density of 1 g/mL;

Experiment group 12:

(4) Diluting the concentrated solution with 1.3 times of water to obtain extract 1, eluting the extract 1 with macroporous resin, eluting with 20% ethanol solution with the amount of 4 times of column volume, collecting eluate, and drying the filtrate at 70deg.C for 8 hr to obtain fructus Amomi extract.

Experiment group 13:

(2) Mixing fructus amomi powder and an ethanol solution with the volume fraction of 80%, wherein the feed-liquid ratio is 1g:10mL, ultrasonic treating with 200w ultrasonic power for 2 times, collecting filtrate, and recovering solvent at 55deg.C under reduced pressure to obtain pasty extract;

(3) Dissolving the pasty extract with distilled water, wherein the mass ratio of the pasty extract to the distilled water is 1:2, and extracting with ethyl acetate to obtain fructus Amomi crude extract;

(4) Adding distilled water solution with mass 0.5 times of that of fructus Amomi crude extract, dissolving, and lyophilizing at-80deg.C to obtain fructus Amomi extract.

Comparative example 3

Preparation method of roselle extract, see experimental group 14-15:

experiment group 14:

(2) Mixing roselle calyx powder and deionized water, wherein the ratio of the roselle calyx powder to the deionized water is 1g to 100mL, carrying out reflux extraction for 3 times at 60 ℃ for 90min each time, collecting an extracting solution, and concentrating the extracting solution under reduced pressure until the density is 1.6g/mL to obtain roselle calyx concentrated solution;

Experiment group 15:

(2) Extracting roselle calyx powder by using 50% ethanol solution, wherein the ratio of the roselle calyx powder to the ethanol solution is 1g to 100mL, the extraction time is 4 hours, collecting an extracting solution, and concentrating the extracting solution under reduced pressure until the density is 1.6g/mL to obtain roselle calyx concentrated solution;

Comparative example 1-comparative example 3 the SPF value of the sunscreen cream was measured by a sun protection factor tester (model: SPF 290 AS) according to the human body law test of cosmetic safety technical Specification.

Experimental results show that the preparation methods of the postoperative extract, the fructus amomi extract and the roselle flower extract can extract more effective components suitable for the sun cream, and the sun-proof effect of the sun cream is improved.

Comparative example 4

The preparation method of the phase A is adjusted on the basis of the embodiment 3, and specifically comprises the following steps: adding water into the curcuma zedoary extract, the amomum villosum extract and the roselle flower extract to prepare a phase A, wherein the concentration of the curcuma zedoary extract, the amomum villosum extract and the roselle flower extract in the phase A is 7.5mg/mL.

Test example 1

The natural plant sunscreens prepared in examples 1 to 3 and comparative example 4 were examined for sun protection factor and stability.

Detection method referring to example 4, the pfa value detection method is the same as the SPF value detection method.

PA grading refers to cosmetic label identification management standard specifications.

The evaluation grades are shown in the following table:

evaluation results:

experimental results show that the sun cream prepared by the invention has strong sun protection effect and stability. In comparative example 4, the active ingredient is directly dissolved in water, so that the sun-proof effect is reduced, the epidermal growth factor receptor is used as a target, the epidermal growth factor receptor nanobody is used as a guide antibody, and the fructus amomi extract and the curcuma zedoary extract are carried to prepare the A phase, so that the active ingredient can be quickly infiltrated into skin cells, the active ingredient can reduce the generation of excessive ultraviolet irradiation in vivo free radicals, enhance the antioxidant activity of organisms, reduce the content of MMPs, maintain the dynamic balance between the oxidation of the bottom layer of the skin and an antioxidant system, and can solve the problem that the natural extract is difficultly dissolved in oil or water, so that the stability of a finished product is affected.

Test example 2

Randomly selecting 20 men and women, 10 men and women, and the ages are 18-30. The subjects did not eat food that affected the light sensation test prior to conducting the test. The test was performed using the sunscreen prepared in example 3.

(1) Selecting 10 persons for UVB irradiation test, and selecting the same part of the abdomen of all the subjects for UVB irradiation, wherein the specific operation is as follows: the lowest dose of irradiation at which erythema appears on the skin after 40 seconds and 20 hours of irradiation with the solar ultraviolet simulator UVB was used as the MED value of the skin of the subject.

(2) The sunscreen cream prepared in example 3 was applied to the skin of the back of the subject in an amount of 2mg/cm ² Respectively subjecting to 30min, 1h, 2h, 4h, and 6hSPF values at the respective time points were calculated by irradiation with medium-wave ultraviolet rays in which MED values appeared.

SPF value = sun protected MED/unprotected MED

(3) Selecting 10 persons for UVA irradiation test, and selecting the same part of the abdomen of all the subjects for UVA irradiation, wherein the specific operation is as follows: after 35min of irradiation with the solar ultraviolet simulator UVA for 2 hours, the minimum irradiation dose at which the skin became blackened was taken as the MPPD value of the subject's skin.

(4) The sunscreen cream prepared in example 3 was applied to the skin of the back of the subject in an amount of 2mg/cm ² The PFA values at the respective time points were calculated by using long-wave ultraviolet irradiation at which the MPPD values appeared at 30min, 1h, 2h, 4h, and 6h, respectively.

PFA value = sun protected MPPD/unprotected MPPD

Referring to fig. 1-2, the sun cream prepared by the invention has good sun effect in 4 hours after being coated, and the sun protection capability is reduced in 4-6 hours. A small amount of supplementary sun cream is needed to keep the sun protection effect.

The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims

1. The preparation method of the natural plant sun cream is characterized in that the sun cream is prepared from a component A, a component B and a component C in a mass ratio of 0.1-0.3:1.3-1.5:2-2.2, wherein the component A, the component B and the component C respectively comprise the following raw materials: the component A is curcuma zedoary extract, amomum villosum extract and roselle flower extract, and the component B is prepared from the following components in parts by weight: 1-3 parts of triacontyl PVP, 0.3-0.5 part of bisabolol, 1.5-2.5 parts of dipotassium glycyrrhizinate, 3-4 parts of octyl polymethyl siloxane and 5-7 parts of dipropylene glycol, wherein the component C comprises the following components in parts by weight: 7-9 parts of sunflower seed oil, 3-5 parts of hydrogenated C6-14 alkene polymer, 1-1.5 parts of tetrahydropyrimidine carboxylic acid and 15-17 parts of glycerol;

the preparation method of the fructus amomi extract comprises the following steps:

(4) Eluting the extract 1 with macroporous resin, eluting with 20% ethanol solution with an amount of 3-5 times of column volume, collecting eluate, and drying to obtain fructus Amomi extract;

the preparation method of the roselle extract comprises the following steps:

(4) Adding 5-7% of active carbon according to the mass of the roselle calyx concentrated solution after ultrasonic treatment, controlling the temperature of the concentrated solution to be 35-37 ℃, stirring for 1-2min by using 300-320r/min, stirring for 10-15min by using 60-70r/min, standing the stirred roselle calyx concentrated solution for 30-40min, filtering, collecting filtrate, and drying to obtain roselle calyx extract;

the preparation method of the curcuma zedoary extract comprises the following steps:

(3) Decolorizing the crude extract of Curcumae rhizoma with active carbon at a mass ratio of 10:0.5 for 10-20min, filtering, and drying to obtain the extract of Curcumae rhizoma;

the preparation method of the natural plant sun cream comprises the following steps:

(1) The preparation method of the phase A comprises the following steps:

s1: mixing a magnesium chloride solution with the volume ratio of 4-6:1.5-1.9:3-3.5 and the concentration of 0.5-0.7mol/L, an aluminum chloride solution with the concentration of 0.5-0.7mol/L and deionized water, preparing a suspension 1, adding the suspension 1 into a sodium hydroxide solution with the concentration of 0.15mol/L while stirring at 950-1050rpm, after all the suspension 1 is added, preparing a suspension 2 by using a magnetic stirring for 5.5-6.5 hours, using a centrifugal force of 4500-5500g for the suspension 2, collecting a supernatant, adding the suspension 1 into ultrapure water with the volume of 3.5-4.5 times of the suspension 1, preparing a precipitation 1 solution, using a centrifugal force of 4500-5500g for 4-6 minutes, discarding the supernatant, and adding the supernatant into a laminar double hydroxide material with the volume of 2.5-3.5 times of the suspension 2;

s2: preparing magnesium chloride hexahydrate and aluminum chloride hexahydrate into a salt solution with the molar ratio of magnesium to aluminum being 3:1 by using deionized water, stirring the salt solution with the concentration of 0.15mol/L in a nitrogen atmosphere by using the deionized water and the sodium hydroxide solution with the concentration of 0.15mol/L with the mass ratio of 5:1, preparing a mixed solution 1 by adding the salt solution into the mixed solution in the stirring process, placing the mixed solution 1 into a water bath kettle with the temperature of 55-65 ℃ for stirring for 5-6 hours, centrifuging 4500-5500g of the mixed solution 1 after water bath stirring for 4-6 minutes by using centrifugal force, discarding supernatant, and collecting precipitate 3;

s3: weighing the curcuma zedoary extract, the amomum villosum extract and the roselle flower extract, adding the curcuma zedoary extract, the amomum villosum extract and the roselle flower extract into a sodium hydroxide solution with the concentration of 0.15mol/L, stirring until the materials are dissolved, preparing a mixed solution 2, wherein the mass concentration of the curcuma zedoary extract, the amomum villosum extract and the roselle flower extract in the mixed solution 2 is 7-8mg/mL, centrifuging the mixed solution 2 for 4-6min by using a centrifugal force of 4500-5500g, discarding supernatant, and collecting precipitate 4;

2. The preparation method of the natural plant sun cream according to claim 1, wherein the sun cream is prepared from a component A, a component B and a component C in a mass ratio of 0.2:1.4:2.1, and the component A, the component B and the component C are respectively composed of the following raw materials: the component A is curcuma zedoary extract, amomum villosum extract and roselle flower extract, and the component B is prepared from the following components in parts by weight: 2 parts of triacontyl PVP, 0.4 part of bisabolol, 2 parts of dipotassium glycyrrhizinate, 3.5 parts of octyl polymethylsiloxane and 6 parts of dipropylene glycol, wherein the component C comprises the following components in parts by weight: 8 parts of sunflower seed oil, 4 parts of hydrogenated C6-14 alkene polymer, 1.25 parts of tetrahydropyrimidine carboxylic acid and 16 parts of glycerol.

3. A natural plant sunscreen prepared according to the process of any one of claims 1-2.