Preparation method of sunscreen cream

Abstract

The invention relates to the technical field of skin care products, in particular to a preparation method of sunscreen cream. The preparation method of the sunscreen cream comprises the following steps: step 1, respectively selecting a proper amount of rhodiola rosea, polygonum cuspidatum, roses and green tea, crushing, and then respectively adding 70% ethanol with a solid-liquid ratio of 8-15 times to the rhodiola rosea, the polygonum cuspidatum, the roses and the green tea; step 2, taking a rhodiola rosea extracting solution, a polygonum cuspidatum extracting solution, a rose extracting solution and a green tea extracting solution as plant compound solutions; 3, preparing a proper amount of 1% sodium ethylene diamine tetracetate solution as a water phase; 4, selecting a proper amount of titanium dioxide, stearic acid, C16-C18 alcohol, vaseline, olive oil, methylparaben and the plant compound liquid as raw materials, heating in a water bath, stirring to form an oil phase, and then adding the mixed emulsifier; step five, adding the oil phase into the water phase while stirring, and then carrying out homogeneous emulsification by using a homogenizer; and 6, carrying out thermal insulation emulsification for 20 min, cooling to 50 DEG C, adding essence, fully stirring, cooling to room temperature (25 DEG C), stopping stirring, and carrying out discharging and filling.

Description

Technical Field

[0001] The present invention relates to the technical field of skin care products, and particularly relates to a preparation method of a sunscreen. Background Art

[0002] Physical sunscreens, also known as inorganic sunscreens, have broad-spectrum sun protection effects and light stability. If high concentrations of physical sunscreens are used for a long time, skin problems such as pore blockage will easily occur; chemical sunscreens, also known as organic sunscreens, are widely used because of their advantages such as low price, high transparency, and refreshing use feeling.

[0003] Due to the disadvantages of chemical sunscreens such as photo-instability and photosensitivity, they generally need to be combined with stable sunscreens to achieve stable and good sun protection effects. Most of the sunscreen products widely sold on the market now are physical-chemical combined sunscreens to achieve broad-spectrum, high-efficiency, and stable sun protection effects. However, with recent research findings, some organic sunscreens have serious harm to marine organisms. For example, organic sunscreen oxybenzone will cause the death of sea anemones and exacerbate coral bleaching under light conditions. Therefore, the use of chemical sunscreens needs to strengthen the study of the phototoxicity of their metabolites to reduce the impact on the safety of marine organisms.

[0004] Different from chemical sunscreens, natural sunscreens are mainly active ingredients with ultraviolet absorption ability extracted from natural plants, such as flavonoids, phenols, and anthraquinones. These components mostly have double bonds, conjugated double bonds or triple bond structures, which can produce similar effects to chemical sunscreens to achieve ultraviolet protection effects, and at the same time also have functions such as antioxidant, whitening, repairing skin damage, soothing, and anti-inflammatory. Summary of the Invention

[0005] The purpose of the present invention is to provide a preparation method of a sunscreen to solve the problem of the harm caused by the phototoxicity of chemical sunscreens to the natural environment.

[0006] To solve the above technical problems, the present invention adopts the following technical solutions:

[0007] A preparation method of a sunscreen, comprising the following steps:

[0008] Step 1: Respectively select appropriate amounts of Rhodiola rosea, Polygonum cuspidatum, Rosa rugosa, and green tea, crush them, then add 70% ethanol with a material-liquid ratio of 8-15 times to each, ultrasonicate for 30-60 min and soak overnight, and then filter each solution and concentrate it under reduced pressure to 1 / 10 volume of the extract at 50-80 °C for standby;

[0009] Step 2: Take 8-15 parts of Rhodiola rosea extract, 8-15 parts of Polygonum cuspidatum extract, 2-6 parts of Rosa rugosa extract, and 3-7 parts of green tea extract according to the volume ratio, mix and stir evenly, and refrigerate to obtain a plant compound liquid;

[0010] Step 3: Prepare an appropriate amount of 1% sodium ethylenediaminetetraacetate solution as the aqueous phase;

[0011] Step 4: Select an appropriate amount of titanium dioxide, stearic acid, C16-C18 alcohol, vaseline, olive oil, methylparaben, and plant compound solution as raw materials, heat and stir them in a water bath to form an oil phase, and then add emulsifiers of Tween-80 and sodium dodecyl sulfate to the mixed raw materials. The emulsifier is an O / W type emulsifier;

[0012] Step 5: Heat the oil phase and the aqueous phase to 80°C respectively, stir until completely dissolved, add the oil phase to the aqueous phase under stirring, and then use a homogenizer for homogenization emulsification;

[0013] Step 6: Keep the temperature for emulsification for 20 minutes and then cool down. When the temperature drops to 50°C, add essence and stir well. Stop stirring when it reaches room temperature (25°C), and then discharge and fill to obtain the product.

[0014] A further technical solution is that in the said Step 1, a traditional Chinese medicine grinder is used to crush rhodiola, polygonum cuspidatum, rose, and green tea respectively, and pass through a 40-100 mesh sieve.

[0015] A further technical solution is that in the said Step 1, a rotary evaporator and a vacuum pump combination instrument are used for vacuum concentration.

[0016] A further technical solution is that in the said Step 2, according to the response surface optimization software, a comprehensive score is given to the sunscreen mechanisms of the four raw materials to obtain the optimized compounding ratio.

[0017] A further technical solution is that in the said Step 3, the amount of the oil phase is 8.5%, and the mass ratio of each raw material is: 3.5 parts of stearic acid, 2 parts of C16-C18 alcohol, 2 parts of vaseline, 1 part of olive oil, 0.3 part of Tween-80, and 0.9 part of sodium dodecyl sulfate.

[0018] A further technical solution is that in the said Step 3, the HLB value of the emulsifier is 13.5.

[0019] A further technical solution is that in the said Step 4, the homogenization time is 10-15 min, the temperature is 50°C, and the homogenization speed is 1000 r / min.

[0020] Compared with the prior art, the beneficial effects of the present invention are:

[0021] 1. The raw materials are derived from plants with both medicinal and cosmetic uses. The components of the selected materials are mostly polyphenols and flavonoids, which have the functions of anti-inflammatory, free radical scavenging, and freckle lightening. In addition to having broad-spectrum sunscreen and whitening effects, it also has a repair effect on sunburned skin.

[0022] 2. The product is an O / W emulsion with a fresh skin feel, good emulsifying effect of the sunscreen, and a delicate overall texture.

[0023] 3. The natural plant composite sunscreen has an SPF value of 21.02 and a PA+++, which can meet the daily sunscreen needs, and its protection effect in the UVA band is better than that of the positive control (Dabao with an SPF value of 30 and a PA+++); at the same time, it has a certain whitening effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is the ultraviolet absorption spectrogram of the extraction solutions and the compound solution of the four medicinal materials in the present invention;

[0025] Figure 2 It is the DPPH free radical scavenging ability diagram of the extraction solutions and the compound solution of the four medicinal materials in the present invention;

[0026] Figure 3 It is the ultraviolet protection ability diagram of the product in the present invention;

[0027] Figure 4 It is the DPPH free radical scavenging ability diagram of the product and the matrix in the present invention;

[0028] Figure 5 It is the diagram of the determination result of the tyrosinase inhibition rate in the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0029] In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0030] Example 1:

[0031] A preparation method of a sunscreen, comprising the following steps:

[0032] Step 1: Appropriate amounts of Rhodiola rosea, Polygonum cuspidatum, Rosa rugosa, and Camellia sinensis are respectively selected and crushed, and then 70% ethanol with a material-liquid ratio of 8-15 times is added to each, ultrasonicated for 30-60 min and then soaked overnight, and then the solutions are filtered and concentrated under reduced pressure to 1 / 10 volume of the extraction solution at 50-80 °C for standby;

[0033] Step 2: Take 8-15 parts of the Rhodiola rosea extraction solution, 8-15 parts of the Polygonum cuspidatum extraction solution, 2-6 parts of the Rosa rugosa extraction solution, and 3-7 parts of the Camellia sinensis extraction solution according to the volume ratio, mix and stir evenly, and refrigerate to obtain a plant compound solution;

[0034] Step 3: Prepare an appropriate amount of 1% sodium ethylenediaminetetraacetate solution as the aqueous phase;

[0035] Step 4: Select appropriate amounts of titanium dioxide, stearic acid, C16-C18 alcohol, petrolatum, olive oil, methylparaben, and plant compound solution as raw materials, heat and stir them in a water bath to form an oil phase, and then add an emulsifier with a mixture of raw materials being Tween-80 and sodium dodecyl sulfate. The emulsifier is an O / W type emulsifier;

[0036] Step 5: Heat the oil phase and the water phase to 80°C respectively, stir until completely dissolved, add the oil phase to the water phase under stirring, and then use a homogenizer for homogenization emulsification;

[0037] Step 6: After heat-preserving and emulsifying for 20 minutes, cool down. When the temperature drops to 50°C, add essence and stir well. Stop stirring when it reaches room temperature (25°C), and then discharge and fill to obtain the product.

[0038] Further, in Step 1, use a traditional Chinese medicine grinder to crush rhodiola, polygonum cuspidatum, rose, and green tea respectively, and pass through a 40-100 mesh sieve.

[0039] Further, in Step 1, use a combined instrument of a rotary evaporator and a vacuum pump for vacuum concentration.

[0040] Further, in Step 2, according to the response surface optimization software, comprehensively score the sunscreen mechanisms of the four raw materials to obtain the optimized compounding ratio. Specifically, use the Box-Behnken model for the response surface optimization design of a three-level four-factor experiment. After designing the experimental scheme table according to the response surface level coding table, conduct experiments according to the experimental scheme. Take the ultraviolet absorption ability, DPPH scavenging rate, and tyrosinase inhibition rate as indicators, establish a quadratic regression model, respond with the response surface method, and obtain the optimal ratio after analyzing the results.

[0041] Response surface level coding table

[0042]

[0043] Response surface experimental scheme design table

[0044]

[0045] Further, in Step 3, the amount of the oil phase is 8.5%, and the mass fraction ratio of each raw material is: 3.5 parts of stearic acid, 2 parts of C16-C18 alcohol, 2 parts of petrolatum, 1 part of olive oil, 0.3 parts of Tween-80, and 0.9 parts of sodium dodecyl sulfate.

[0046] Further, in Step 3, the HLB value of the emulsifier is 13.5.

[0047] Further, in Step 4, the homogenization time is 10 - 15 min, the temperature is 50°C, and the homogenization speed is 1000 r / min.

[0048] Example 2

[0049] Using the plant extract in the present invention as a sample, the whitening and sunscreen capabilities were measured according to the following method:

[0050] 1. Measurement of ultraviolet absorption ability

[0051] Preheat the ultraviolet spectrophotometer for 30 min. Dilute the plant extract with 70% ethanol solution to a solution of 0.2 mg / ml, zero with 75% ethanol, and scan and measure the absorbance of the plant extract in the range of 280 nm to 420 nm. Each sample was measured in parallel 3 times.

[0052] 2. Measurement of tyrosinase inhibition rate

[0053] Add the prepared reagents to the microplate in sequence. After incubating at 37 °C for half an hour on a microplate reader, measure the absorbance at 475 nm. Add the reagents according to the following table, and each sample was measured three times repeatedly.

[0054] Reagent addition table (volume: μL)

[0055]

[0056] The inhibition rate calculation formula is as follows:

[0057]

[0058] Note: A: Substrate + enzyme; A0: Enzyme; A1: Enzyme + substrate + sample; A2: Enzyme + sample

[0059] 1. Measurement of DPPH free radical scavenging rate

[0060] Six concentration gradients were set for each plant extract, and DPPH solution (0.08 mg / mL) was added respectively. The absorbance was measured at 517 nm. Each sample was measured in parallel 3 times, and vitamin C was used as a positive control. The scavenging rate was calculated according to the following formula:

[0061]

[0062] Note: a: Absorbance of 2 ml of the sample solution to be measured + 2 ml of DPPH solution;

[0063] b: Absorbance of 2 ml of the sample solution to be measured + 2 ml of ethanol solution;

[0064] c: Absorbance of 2 ml of ethanol solution + 2 ml of DPPH solution.

[0065] Example 3

[0066] Using the finished product of the present invention as a sample, the physicochemical properties were determined and evaluated according to the following methods:

[0067] 1. Sensory evaluation

[0068] Take an appropriate amount and apply it to the back of the hand, and compare its viscosity, ductility, spreadability and skin feel. Visually observe the color of the prepared sunscreen, the fineness of the paste, and whether there are any abnormalities such as uneven color.

[0069] 2. Emulsion type

[0070] Dyeing method: Drop the water-based dye methyl blue on the emulsion. If the dye diffuses and dissolves, and the external phase is observed to be dyed blue under the microscope, it can be considered that the external phase of the emulsion is the water phase and the emulsion is of the O / W type. If the situation is the opposite, it is a W / O type emulsion.

[0071] 3. pH value

[0072] Weigh 1.0 g of the prepared sample, stir it with 10 mL of boiled distilled water until dissolved, and use a pH meter to measure the pH value of the sunscreen.

[0073] 4. Stability

[0074] (1) Heat and cold resistance test

[0075] Put the sample into a refrigerator at -15°C to -20°C, take it out after 24 hours; then put the sample into a 37°C constant temperature incubator, take it out after 24 hours, and visually observe whether there is any stratification, whether there are small water droplets and particles, etc. after cooling to room temperature.

[0076] (2) Centrifugation experiment

[0077] Put the sample into a centrifuge tube and centrifuge it at 2000 r / min, 3000 r / min, and 4000 r / min for 30 minutes to observe whether there is any stratification.

[0078] Centrifugation experiment result grade evaluation form

[0079]

[0080] 5. Waterproofness

[0081] Attach a medical breathable tape to the light-transmitting side of a quartz dish, and accurately weigh (2.2 ± 0.2) mg / cm 2 , as the coating sample group (referred to as the sample plate); prepare 10 sample plates in the same way (5 for the control group and 5 for the sample group), and use 3 empty quartz plates (empty plates) with tape attached but no coating as the reference.

[0082] Place the blank plate and the control group at room temperature for 30 min for measurement; put the sample group into 0.9% NaCl solution, stir at a speed of 50 r / min for 40 min, take it out and dry it in an oven at 40 °C for 40 min. Use the blank plate to zero, and measure the absorbance of the control group and the sample group at wavelengths of 280 - 320 nm and 320 - 400 nm. The evaluation table of the water resistance index level is as follows.

[0083]

[0084] Evaluation Table of Water Resistance Index Level

[0085]

[0086]

[0087] Example 4

[0088] Using the finished product of the present invention as a sample, the efficacy is determined and evaluated according to the following method:

[0089] 1. UV protection ability

[0090] Weigh 2 ± 0.2 mg / cm 2 of the sample on the 3M Company Transpore Tape, and use gloves to evenly apply the sunscreen to cover the entire tape surface. Let the sample dry for 20 min, and use a quartz cuvette to measure the absorbance at 280 - 400 nm.

[0091] (1) Calculation of SPF value

[0092] Measure the absorbance in the wavelength range of 280 - 320 nm, and calculate the UV absorbance value through the following formula.

[0093]

[0094] CF: 10

[0095] Table for looking up the value of EE(λ)×I(λ)

[0096]

[0097] (2) Calculation of PA value

[0098] Perform three groups of repeated experiments by the above method, measure the transmittance in the range of 320 nm - 400 nm, and calculate through the following formula:

[0099] T1 = (T 320 + T 330 + T 340 + …… + T 400 ) / 9 ………………

[0100] T2 = (T1 + T2 + T3) / 3………………………………

[0101] T x — is the transmittance value measured at each wavelength of 320nm, 330 - 400nm for each sample.

[0102] T1— is the arithmetic value of the transmittance measured at nine wavelengths for each sample.

[0103] T2— is the arithmetic mean of the transmittance in this wavelength band.

[0104] UVA Band Sunscreen Index PA Value Evaluation Table

[0105]

[0106] 2. Whitening Efficacy Determination

[0107] Prepare gradient solutions of the sample with concentrations of 10mg / ml, 50mg / ml, 300mg / ml, 500mg / ml, and 1000mg / ml using a mixed solvent (dimethyl sulfoxide: phosphate buffer = 1:4, V / V); add the reagents to the microplate as follows in sequence, react at 37°C for 30 min on a microplate reader, and measure the absorbance at 475nm. Repeat each sample three times.

[0108]

[0109] Among them, A: substrate + enzyme; B: enzyme; C: substrate + enzyme + sample; D: enzyme + sample.

[0110] Reagent Loading Table (μl)

[0111]

[0112] 3. Exploration of Post - sun Repair of Animal Skin

[0113] Weigh 0.05g / cm 2 sample, apply it to the skin of mice (SPF female mice), irradiate the skin of mice with ultraviolet light (365nm), the irradiation intensity is 1.58J / cm 2 , irradiate for 5 min every day for 3 consecutive days, and observe whether there are redness, skin patches, etc. on the skin of mice.

[0114] Example 5

[0115] Using the finished product of the present invention as a sample, conduct safety evaluation according to the following method:

[0116] 1. Microbiological Detection

[0117] (1) Heat - resistant Escherichia coli

[0118] Take 10 mL of the sample solution diluted 1:10 with distilled water, add it to 10 mL of double lactose bile salt (containing neutralizer) medium, and incubate it in an incubator at 44.5°C ± 0.5°C for 48 h. Observe every 24 h to see if acid and gas are produced; if neither acid nor gas is produced, report it as negative for thermotolerant coliforms.

[0119] (2) Pseudomonas aeruginosa

[0120] Take 10 mL of the sample solution diluted 1:10 with distilled water, add it to 90 mL of SCDLP liquid medium, and incubate it at 36°C ± 1°C for 18 h - 24 h. If Pseudomonas aeruginosa grows, there is often a thin bacterial film on the surface of the culture solution, and the culture solution is often yellowish-green or bluish-green.

[0121] If a bacterial film is produced, pick the culture from the film of the culture solution, streak it on cetrimonium bromide agar plate, and incubate it at 36°C ± 1°C for 18 h - 24 h. Select the suspicious colonies for microscopic examination, oxidase test and pyocyanin test for determination.

[0122] 2. Evaluation of animal skin irritation

[0123] Depilate the two sides of the spine of the test animals (SPF-grade female mice) with an area of 1 cm × 2 cm, one on each side. Weigh about 0.5 mL (g) of the test substance, apply it on the skin of the test animals, cover it with two layers of gauze (3.5 cm × 3.5 cm) and a layer of cellophane or similar material, and then fix it with non-irritating adhesive tape and bandage. The skin on the other side is used as a control. Remove the test sample with a non-irritating reagent, and observe at 24 h, 48 h, and 72 h after removing the test sample to see if there is an irritating reaction.

[0124] Although the present invention has been described herein with reference to several illustrative embodiments of the invention, it should be understood that those skilled in the art can design many other modifications and embodiments that will fall within the scope of the principles and spirit disclosed in this application. More specifically, within the scope of the disclosure, the drawings and the claims of this application, various variations and improvements can be made to the components and / or the layout of the subject combination layout. In addition to the variations and improvements made to the components and / or the layout, other uses will also be obvious to those skilled in the art.

Claims

1. A method for preparing a sunscreen, characterized in that: It includes the following steps: Step 1: Appropriately select an amount of Rhodiola rosea, Polygonum cuspidatum, rose, and green tea, crush them respectively, then add 70% ethanol with a material-liquid ratio of 8 - 15 times, ultrasonic for 30 - 60 min, soak overnight, and then filter each solution and concentrate it under reduced pressure to 1 / 10 volume of the extract at 50 - 80 °C for standby; Step 2: Take 8 - 15 parts of Rhodiola rosea extract, 8 - 15 parts of Polygonum cuspidatum extract, 2 - 6 parts of rose extract, and 3 - 7 parts of green tea extract according to the volume ratio, mix and stir evenly, and refrigerate to obtain a plant compound solution; Step 3: Prepare an appropriate amount of 1% sodium ethylenediaminetetraacetate solution as the aqueous phase; Step 4: Select an appropriate amount of titanium dioxide, stearic acid, C16 - C18 alcohol, petrolatum, olive oil, methylparaben, and the plant compound solution as raw materials, heat and stir in a water bath to form an oil phase, and then add an emulsifier with a mixture of raw materials being Tween - 80 and sodium dodecyl sulfate. The emulsifier is an O / W type emulsifier; Step 5: Heat the oil phase and the aqueous phase to 80 °C respectively, stir until completely dissolved, add the oil phase to the aqueous phase under stirring, and then use a homogenizer for homogenization emulsification; Step 6: Keep warm and emulsify for 20 minutes, then cool down. When the temperature drops to 50 °C, add essence and stir well. Stop stirring when it reaches room temperature (25 °C), and discharge and fill to obtain the product.

2. The preparation method of a sunscreen according to claim 1, characterized in that: In Step 1, use a traditional Chinese medicine crusher to crush Rhodiola rosea, Polygonum cuspidatum, rose, and green tea respectively, and pass through a 40 - 100 mesh sieve.

3. The preparation method of a sunscreen according to claim 1, wherein: In Step 1, use a combination instrument of a rotary evaporator and a vacuum pump for concentration under reduced pressure.

4. The preparation method of a sunscreen according to claim 1, characterized in that: In Step 2, comprehensively score the sunscreen mechanisms of the four raw materials according to the response surface optimization software to obtain the optimized compounding ratio.

5. The preparation method of a sunscreen according to claim 1, characterized in that: In Step 3, the oil phase dosage is 8.5%, and the mass fraction ratio of each raw material: stearic acid is 3.5 parts, C16 - C18 alcohol is 2 parts, petrolatum is 2 parts, olive oil is 1 part, Tween - 80 is 0.3 parts, and sodium dodecyl sulfate is 0.9 parts.

6. The preparation method of a sunscreen according to claim 1, characterized in that: In Step 3, the HLB value of the emulsifier is 13.

5.

7. The preparation method of a sunscreen according to claim 1, characterized in that: In Step 4, the homogenization time is 10 - 15 min, the temperature is 50 °C, and the homogenization speed is 1000 r / min.

Images