A water-dispersed children's sunscreen lotion and preparation method thereof

Abstract

The present invention relates to a water-dispersed children's sunscreen lotion and a preparation method thereof. The raw materials for preparing the children's sunscreen lotion include sunscreen, moisturizer, thickener, emulsifier and water. The sunscreen includes titanium dioxide and silica composite, and the silica is coated on the surface of the titanium dioxide. The present invention wraps titanium dioxide in silica. When ultraviolet rays are irradiated, the irregular surface of silica causes light to bend and scatter, increases light scattering and light propagation length, prolongs the propagation path of light in the sunscreen coating, increases the possibility of ultraviolet rays contacting the sunscreen, and thus improves the sunscreen effect, so that a higher sunscreen value can be achieved even with less titanium dioxide. At the same time, less sunscreen is added, the burden on children's skin is reduced, the false white phenomenon is weakened, and the skin feel is improved. Then, through water dispersion treatment, the hydrophobic powder titanium dioxide is stably dispersed in water, so that it can be unloaded with clean water, and the stability of the product in the water-in-oil system is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics and relates to a water-dispersed children's sunscreen lotion and a preparation method thereof. Background Art

[0002] With the development of social economy and the improvement of people's awareness of sun protection, people are increasingly aware that excessive ultraviolet radiation will not only damage the human immune system, but also accelerate skin aging, leading to various skin diseases and even skin cancer. Therefore, the market share of sunscreen products is increasing. More and more sunscreen products are favored by consumers, and consumers have become more rational, changing from simply looking at the sun protection index to choosing safer, more comfortable and efficient sunscreen products. Especially for more segmented children's sunscreen products, the great difference in structure and function between children's skin and adult skin prompts them to put forward higher requirements for the safety and efficacy of sunscreen products. Pure physical sunscreen products, which are recognized as relatively safe, are bound to become a trend. Pure physical sunscreen products also have certain skills in formula design to take into account skin feel and sun protection index.

[0003] On August 31, 2023, the China Food and Drug Inspection Institute issued a notice on the "Technical Guidelines for Children's Cosmetics" (No. 1 of 2023). The guidelines state that children's products are not allowed to add raw materials prepared with new technologies such as nanotechnology. If there are no alternative raw materials and they must be used, the reasons should be stated and the safety of the use of children's cosmetics should be evaluated; it is clearly stated that the use of nanomaterials in children's products must state the reason for the use is that there is no alternative and a full safety assessment must be conducted.

[0004] From the above information, it can be seen that children's sunscreen products are limited in the choice of physical sunscreens. Compared with nanotechnology, non-nano sunscreen technology has certain disadvantages in terms of contributed sun protection value and skin feel. The sun protection index provided by non-nano physical sunscreens is not high, and the sun protection effect is not good, so more physical sunscreens need to be added to achieve a higher sun protection value. Non-nano particles themselves are prone to problems such as false white, coarseness, and mud. Too high a content of sunscreen is also likely to cause a burden on children's skin. In addition, because zinc oxide is prone to instability in the water-in-oil system, titanium dioxide has a higher reflectivity and higher whiteness than zinc oxide. Therefore, at this stage, the amount of sunscreen added to the water-in-oil pure titanium dioxide children's sunscreen formula is relatively high, and the false white phenomenon is more obvious. In addition, titanium dioxide itself is a hydrophobic powder. When added to the water-in-oil system at a high content, it is easy to cause surface roughness, powder aggregation, and material instability. Summary of the invention

[0005] In view of the deficiencies in the prior art, the object of the present invention is to provide a water-dispersed children's sunscreen lotion and a preparation method thereof.

[0006] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0007] In a first aspect, the present invention provides a water-dispersed children's sunscreen lotion, wherein the raw materials for preparing the children's sunscreen lotion include a sunscreen agent, a moisturizer, a thickener, an emulsifier and water, wherein the sunscreen agent includes a titanium dioxide and a silica composite, and the silica is coated on the surface of the titanium dioxide.

[0008] The water dispersion refers to the use of C20-22 alcohol phosphate, C20-22 alcohol mixture and di(laurylamide glutamine) lysine sodium to stably disperse the hydrophobic substance titanium dioxide in water, obtain better water dispersibility, and improve the stability of the product in the water-in-oil system. The di(laurylamide glutamine) lysine sodium used is a plant-derived dipeptide anionic gemini amphiphilic compound with extremely high surface activity and a gemini structure similar to the ceramide structure. It has good affinity for hair and skin, good anti-allergic properties, and is suitable for children's products; it is matched with anionic surfactants C20-22 alcohol phosphate and C20-22 alcohol mixture to assist in improving powder dispersion (especially lipophilic powder). Moreover, it has a unique liquid crystal morphology structure, which can provide the product with a velvety soft and light touch.

[0009] The present invention wraps titanium dioxide in silica. The irregular surface of silica causes light to bend and scatter, increasing light scattering and light propagation length, thereby extending the propagation path of light in the sunscreen coating, increasing the possibility of ultraviolet rays contacting the sunscreen agent, and thus increasing the sunscreen agent's absorption, reflection or scattering of ultraviolet rays, thereby improving the sunscreen effect, achieving a higher sun protection value while using less titanium dioxide. At the same time, the amount of sunscreen added is reduced, the burden on children's skin is reduced, the false white phenomenon is weakened, the skin feel is improved simultaneously, and the sunscreen can be washed off with clean water.

[0010] Preferably, the raw materials for preparing the children's sunscreen lotion include, by mass percentage, 5-20% sunscreen, 5-20% moisturizer, 0.5-6% thickener, 1-10% emulsifier and water.

[0011] The mass percentage of the sunscreen agent can be selected from 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, etc., and the mass percentage of the moisturizer can be selected from 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, etc. , 20%, etc., the mass percentage of the thickener can be selected from 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, etc., the mass percentage of the emulsifier can be selected from 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, etc., and other specific point values ​​within the above numerical range can be selected, so they will not be described one by one here.

[0012] Preferably, the mass ratio of titanium dioxide to silica is (5-10):(0.5-2).

[0013] Among them, the specific point values ​​in (5-10) can be selected as 5, 5.2, 5.5, 5.8, 6, 6.2, 6.5, 6.8, 7, 7.2, 7.5, 7.8, 8, 8.2, 8.5, 8.8, 9, 9.2, 9.5, 9.8, 10, etc., and the specific point values ​​in (0.5-2) can be selected as 0.5, 0.6, 0.7, 0.8, 0.9, 1, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2, etc. Other specific point values ​​within the above numerical range can be selected, so they will not be listed here one by one.

[0014] Preferably, the children's sunscreen lotion further comprises any one of an emollient, an antioxidant or a pH adjuster, or a combination of at least two of them.

[0015] Preferably, the children's sunscreen lotion further comprises any one of 7-15% of an emollient, 0.5-2% of an antioxidant, or 0.2-0.6% of a pH adjuster, or a combination of at least two thereof.

[0016] The mass percentage of the emollient can be selected from 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, etc., the mass percentage of the antioxidant can be selected from 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, 2%, etc., the mass percentage of the pH regulator can be selected from 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, 0.55%, 0.6%, etc., and other specific point values ​​within the above numerical range can be selected, which will not be repeated here one by one.

[0017] Preferably, the emulsifier comprises C20-22 alcohol phosphate and C20-22 alcohol mixture and / or sodium di(laurylamide glutamine) lysine, preferably a combination of C20-22 alcohol phosphate and C20-22 alcohol mixture and sodium di(laurylamide glutamine) lysine.

[0018] Titanium dioxide is a hydrophobic powder. When a high content of titanium dioxide is added into a water-in-oil system, it is easy to cause surface roughness, powder aggregation, and material instability. The present invention adds a plant-derived double-locked anionic emulsifier, namely sodium di(laurylamide glutamine) lysine, in combination with C20-22 alcohol phosphate and C20-22 alcohol mixture with good powder dispersibility, so that the hydrophobic powder can be stably dispersed in water, and the two have a mutually coordinated effect.

[0019] Preferably, the moisturizing agent includes any one of butylene glycol, glycerin, 1,2-pentanediol or stearyl glycyrrhetinate or a combination of at least two thereof.

[0020] Preferably, the thickener includes any one of hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polysorbate-60, sorbitan isostearate, bentonite or xanthan gum, or a combination of at least two thereof.

[0021] Preferably, the pH adjuster comprises arginine and / or citric acid.

[0022] Preferably, the antioxidant comprises p-hydroxyacetophenone and / or tocopherol acetate.

[0023] Preferably, the emollient comprises any one of tri(ethylhexanoin), coconut oil alcohol-caprylate / caprate, polydimethylsiloxane or squalane, or a combination of at least two thereof; more preferably, it is a combination of tri(ethylhexanoin), coconut oil alcohol-caprylate / caprate, polydimethylsiloxane and squalane.

[0024] The present invention finds that triethylhexanoin, coconut oil alcohol caprylate / caprate, polydimethylsiloxane and squalane have a mutually complementary effect in terms of skin emollient effect.

[0025] In a second aspect, the present invention provides a method for preparing the water-dispersed children's sunscreen lotion according to the first aspect, the preparation method comprising: mixing a sunscreen agent, a thickener, a moisturizer and water, and homogenizing; and then mixing with an emulsifier, and homogenizing to obtain the sunscreen lotion.

[0026] Preferably, the homogenization time is independently 5-15 min, for example 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, etc. Other specific point values ​​within the above numerical range can be selected, which will not be described here one by one.

[0027] Preferably, the mixing temperature is independently 60-80°C, for example, 60°C, 62°C, 64°C, 66°C, 68°C, 70°C, 72°C, 74°C, 76°C, 78°C, 80°C, etc. Other specific point values ​​within the above numerical range can be selected, which will not be elaborated here.

[0028] Preferably, the mixing with the emulsifier is performed under vacuum conditions.

[0029] Preferably, the sunscreen, thickener, moisturizer and water are mixed together with a pH adjuster.

[0030] Preferably, the mixing with the emulsifier also includes mixing with an emollient and / or an antioxidant.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] The present invention wraps titanium dioxide in silica. When ultraviolet rays are irradiated, the irregular surface of silica causes light to bend and scatter, increasing light scattering and the propagation length of light, thereby extending the propagation path of light in the sunscreen coating, increasing the possibility of ultraviolet rays contacting the sunscreen agent, and increasing the absorption, reflection or scattering of ultraviolet rays by the sunscreen agent, thereby improving the sunscreen effect, achieving a higher sunscreen value with less titanium dioxide, and at the same time, the amount of sunscreen agent added is reduced, the burden on children's skin is reduced, the false white phenomenon is weakened, and the skin feel is improved simultaneously. Then, through water dispersion treatment, the hydrophobic powder titanium dioxide is stably dispersed in water, and the stability of the product in the water-in-oil system is improved. DETAILED DESCRIPTION

[0033] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0034] The sources of the functional ingredients contained in the products involved in the following embodiments and comparative examples are as follows (only the functional ingredients are reflected, and the necessary auxiliary ingredients contained in other commercially available raw materials are not repeated):

[0035] The polydimethylsiloxane was obtained from a product purchased from Dow Chemical Company under the trade name PMX-200 Silicone Fluid 100 cSt;

[0036] The C20-22 alcohol phosphate and C20-22 alcohol mixture are obtained from a product called SensonovWR purchased from Seppic Corporation;

[0037] Di(laurylamide glutamine) lysine was purchased from Huilang Company under the trade name PELLICER TM Products of L-30;

[0038] Hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer was purchased from Seppic under the trade name SEPINOV TM Products of EMT 10;

[0039] Polysorbate-60 was obtained from Croda Corporation under the trade name TWEEN 60;

[0040] Coco-caprylate / caprate was obtained from Bio-Hollow Corporation under the trade name Liponate CCC MB.

[0041] Example 1

[0042] The present embodiment provides a water-dispersed children's sunscreen lotion, which includes, by mass percentage, titanium dioxide, 12% of silica composite, 2% of C20-22 alcohol phosphate and C20-22 alcohol mixture, 2% of di(laurylamide glutamine) lysine, 3% of butylene glycol, 3% of glycerol, 3% of 1,2-pentanediol, 3% of stearyl glycyrrhetinate, 0.5% of hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, 0.5% of polysorbate-60, 0.5% of sorbitan isostearate, and 0.5% of stilbene glycol. 0.5% soil, 0.5% xanthan gum, 0.4% arginine, 0.08% citric acid, 0.5% p-hydroxyacetophenone, 0.5% tocopheryl acetate, 2.5% triethylhexanoin, 2.5% coconut oil alcohol-caprylate / caprate, 3.5% polydimethylsiloxane, 2.5% squalane and the balance water, the mass ratio of C20-22 alcohol phosphate and C20-22 alcohol is 1:1, and in the titanium dioxide and silica composite, silica is coated on the surface of titanium dioxide, and the mass ratio of titanium dioxide to silica is 9:1.

[0043] Its preparation method is:

[0044] (1) mixing butylene glycol, glycerin, bentonite, sodium di(laurylamide glutamine) lysine and xanthan gum, homogenizing, and then mixing with titanium dioxide, silica composite and arginine, homogenizing for 8 minutes, and homogenizing at 78° C. for 12 minutes to obtain a first mixture;

[0045] Mixing triethylhexanoin, coconut oil alcohol caprylate / caprate, C20-22 alcohol phosphate and C20-22 alcohol mixture, dimethicone, squalane, tocopheryl acetate, and stearyl glycyrrhetinate at 78° C. to obtain a second mixture;

[0046] (2) mixing the first mixture and the second mixture at -0.06 MPa and homogenizing at 78° C. for 8 min;

[0047] (3) 1,2-pentanediol and p-hydroxyacetophenone are mixed at 68° C., and then mixed with the second mixture, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polysorbate-60 and sorbitan isostearate, and homogenized for 4 minutes to obtain a third mixture;

[0048] (4) Mix water and citric acid, then mix with the third mixture and homogenize for 1 minute to obtain the product.

[0049] Example 2

[0050] The present embodiment provides a water-dispersed children's sunscreen lotion, which comprises, by mass percentage, titanium dioxide, 5% silica composite, 1% C20-22 alcohol phosphate and C20-22 alcohol mixture, 1% di(laurylamide glutamine) lysine, 2% butylene glycol, 2% glycerol, 2% 1,2-pentanediol, 2% stearyl glycyrrhetinate, 0.3% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, 0.3% polysorbate-60, 0.3% sorbitan isostearate, and 0.3% stilbene glycol. 0.3% of moistening clay, 0.3% of xanthan gum, 0.3% of arginine, 0.06% of citric acid, 0.25% of p-hydroxyacetophenone, 0.25% of tocopheryl acetate, 2% of triethylhexanoin, 2% of coconut oil alcohol-caprylate / caprate, 2.8% of polydimethylsiloxane, 2% of squalane and the balance of water, the mass ratio of C20-22 alcohol phosphate to C20-22 alcohol is 1:1, and in the titanium dioxide and silica composite, silica is coated on the surface of titanium dioxide, and the mass ratio of titanium dioxide to silica is 10:1.

[0051] Its preparation method is:

[0052] (1) mixing butylene glycol, glycerin, bentonite, sodium di(laurylamide glutamine) lysine and xanthan gum, homogenizing, and then mixing with titanium dioxide, silica composite and arginine, homogenizing for 5 minutes, and homogenizing at 75° C. for 10 minutes to obtain a first mixture;

[0053] Mixing tri(ethylhexanoin)glyceryl, coconut oil alcohol caprylate / caprate, C20-22 alcohol phosphate and C20-22 alcohol mixture, polydimethylsiloxane, squalane, tocopheryl acetate, and stearyl glycyrrhetinate at 75° C. to obtain a second mixture;

[0054] (2) mixing the first mixture and the second mixture at -0.06 MPa and homogenizing at 75° C. for 5 min;

[0055] (3) 1,2-pentanediol and p-hydroxyacetophenone are mixed at 65° C., and then mixed with the second mixture, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polysorbate-60 and sorbitan isostearate, and homogenized for 3 minutes to obtain a third mixture;

[0056] (4) Mix water and citric acid, then mix with the third mixture and homogenize for 1 minute to obtain the product.

[0057] Example 3

[0058] The present embodiment provides a water-dispersed children's sunscreen lotion, which includes, by mass percentage, titanium dioxide, 18% of silica composite, 3% of C20-22 alcohol phosphate and C20-22 alcohol mixture, 3% of di(laurylamide glutamine) lysine, 4% of butylene glycol, 4% of glycerol, 4% of 1,2-pentanediol, 4% of stearyl glycyrrhetinate, 0.8% of hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, 0.8% of polysorbate-60, and 0.08% of sorbitan isostearate. .8%, bentonite 0.8%, xanthan gum 0.8%, arginine 0.2%, citric acid 0.04%, p-hydroxyacetophenone 1%, tocopheryl acetate 1%, triethylhexanoin 3%, coconut oil alcohol caprylate / caprate 4%, polydimethylsiloxane 4%, squalane 4% and water as the balance, the mass ratio of C20-22 alcohol phosphate and C20-22 alcohol is 1:1, and in the titanium dioxide and silica composite, silica is coated on the surface of titanium dioxide, and the mass ratio of titanium dioxide to silica is 5:1.

[0059] Its preparation method is:

[0060] (1) mixing butylene glycol, glycerin, bentonite, sodium di(laurylamide glutamine) lysine and xanthan gum, homogenizing, and then mixing with titanium dioxide, silica composite and arginine, homogenizing for 10 minutes, and homogenizing at 80° C. for 15 minutes to obtain a first mixture;

[0061] Glyceryl tri(ethylhexanoate), coconut oil alcohol caprylate / caprate, C20-22 alcohol phosphate and C20-22 alcohol mixture, polydimethylsiloxane, squalane, tocopheryl acetate, and stearyl glycyrrhetinate are mixed at 80° C. to obtain a second mixture;

[0062] (2) mixing the first mixture and the second mixture at -0.06 MPa and homogenizing at 80° C. for 10 min;

[0063] (3) 1,2-pentanediol and p-hydroxyacetophenone are mixed at 70° C., and then mixed with the second mixture, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polysorbate-60 and sorbitan isostearate, and homogenized for 5 minutes to obtain a third mixture;

[0064] (4) Mix water and citric acid, then mix with the third mixture and homogenize for 2 minutes to obtain the product.

[0065] Example 4

[0066] This embodiment provides a water-dispersed children's sunscreen lotion, which differs from Embodiment 1 only in that it does not contain C20-22 alcohol phosphate and C20-22 alcohol mixture, and its reduced mass is allocated to the mass of di(lauroyl glutamine) lysine, while other ingredients and contents remain unchanged.

[0067] The preparation method is similar to that of Example 1.

[0068] Example 5

[0069] This embodiment provides a water-dispersible children's sunscreen lotion, which differs from Embodiment 1 only in that it does not contain di(laurylamide glutamine)lysine, and its reduced mass is distributed to the mass of C20-22 alcohol phosphate and C20-22 alcohol mixture, while other ingredients and contents remain unchanged.

[0070] The preparation method is similar to that of Example 1.

[0071] Example 6

[0072] This embodiment provides a water-dispersible children's sunscreen lotion, which differs from Example 1 only in that it does not contain triethylhexanoin, and its reduced mass is proportionally distributed to the masses of coconut oil alcohol caprylate / caprate, polydimethylsiloxane and squalane, and other ingredients and contents remain unchanged.

[0073] The preparation method is similar to that of Example 1.

[0074] Example 7

[0075] This embodiment provides a water-dispersible children's sunscreen lotion, which is different from Example 1 only in that it does not contain coconut oil alcohol caprylate / caprate, and its reduced mass is proportionally distributed to the mass of triethylhexanoin, polydimethylsiloxane and squalane, while other ingredients and contents remain unchanged.

[0076] The preparation method is similar to that of Example 1.

[0077] Example 8

[0078] This embodiment provides a water-dispersible children's sunscreen lotion, which is different from Example 1 only in that it does not contain polydimethylsiloxane, and its reduced mass is proportionally distributed to the masses of triethylhexanoin, coconut oil alcohol-caprylate / caprate and squalane, and other ingredients and contents remain unchanged.

[0079] The preparation method is similar to that of Example 1.

[0080] Example 9

[0081] This embodiment provides a water-dispersible children's sunscreen lotion, which differs from Example 1 only in that it does not contain squalane, and its reduced mass is proportionally distributed to the masses of triethylhexanoin, polydimethylsiloxane and coconut oil alcohol-caprylate / caprate, and other ingredients and contents remain unchanged.

[0082] The preparation method is similar to that of Example 1.

[0083] Example 10

[0084] This comparative example provides a water-dispersed children's sunscreen lotion, which differs from Example 1 only in that polydimethylsiloxane is replaced by diphenylsiloxyphenyl trimethicone in equal amounts, and other ingredients and contents remain unchanged.

[0085] The preparation method is similar to that of Example 1.

[0086] Embodiment 11

[0087] This comparative example provides a water-dispersed children's sunscreen lotion, which differs from Example 1 only in that polydimethylsiloxane is replaced by diethylhexyl succinate in an equal amount, and other ingredients and contents remain unchanged.

[0088] The preparation method is similar to that of Example 1.

[0089] Example 12

[0090] This comparative example provides a water-dispersed children's sunscreen lotion, which differs from Example 1 only in that polydimethylsiloxane is replaced by isohexadecane in equal amounts, and other ingredients and contents remain unchanged.

[0091] The preparation method is similar to that of Example 1.

[0092] Comparative Example 1

[0093] This comparative example provides a water-dispersed children's sunscreen lotion, which differs from Example 1 only in that 12% of the titanium dioxide and silica composite is replaced by 10.8% of titanium dioxide and 1.2% of silica, and silica and titanium dioxide are added independently, while other ingredients and contents remain unchanged.

[0094] The preparation method is similar to that of Example 1.

[0095] Test Example 1

[0096] SPF value determination

[0097] Test samples: Examples 1-12, Comparative Example 1

[0098] Reference substance: SPF value 16.1±2.4, prepared according to the standard formula of medium-high SPF standard product (P2) in the "Technical Specification for Safety of Cosmetics" (2015 edition).

[0099] Subjects: A total of 10 subjects, 3 males and 7 females, aged 24 to 52 years old, with an average age of 35.4±10.0 years old, met the voluntary inclusion criteria, and the subjects tested each group of samples in turn.

[0100] Light source: Daylight simulator xenon arc lamp, all performance indicators meet the measurement specification requirements.

[0101] Test method: Test in accordance with the specific requirements of the "Technical Specifications for Safety of Cosmetics" (2015 edition). The subject lies prone and the back is irradiated. The minimum erythema dose (MED value) of the subject's skin to ultraviolet radiation is predicted 24 hours before the test, and the ultraviolet radiation dose is adjusted according to the predicted results for testing the test object. On the day of the test, a spot no less than 30 cm is selected on the subject's back. 2 Normal skin area, (2.00±0.05)mg / cm 2 The test object or reference substance is evenly applied to the above-mentioned area with the dosage of 100 mg / kg. Then the irradiation dose is selected according to the specification requirements, and irradiation is performed in three conditions: ① The test object is not applied to the subject's skin; ② The reference substance is applied; ③ The test object is applied. Observe the experimental results after 24 hours and record the MED values ​​in the three conditions respectively.

[0102] SPF value calculation method: The SPF value of the test object or reference product protecting a single subject is expressed as follows:

[0103]

[0104] The individual SPF value is required to be accurate to one decimal place. The arithmetic mean of the SPF values ​​of all subjects protected by the measured object is calculated, and the integer part is the SPF value of the measured sample. The sampling error of the estimated mean can calculate the standard deviation and standard error of the data set. The 95% confidence interval (95% CI) of the mean is required to be no more than 17% of the mean, otherwise the number of subjects should be increased (no more than 25) until the above requirements are met. The results are shown in Table 1.

[0105] Table 1

[0106] Group SPF value Example 1 20 Example 2 18 Example 3 17 Example 4 13 Example 5 11 Example 6 18 Example 7 18 Example 8 10 Example 9 17 Example 10 11 Embodiment 11 7 Example 12 7 Comparative Example 1 6

[0107] Test Example 2

[0108] PFA value determination

[0109] Test samples: Examples 1-12, Comparative Example 1

[0110] Reference substance: PFA value 4.4±0.6, prepared according to the standard formula of PFA determination standard substance in the "Technical Specification for Safety of Cosmetics" (2015 edition).

[0111] Subjects: A total of 10 subjects, 5 males and 5 females, aged 18 to 51 years old, with an average age of 36.1±11.3 years old, met the voluntary inclusion criteria, and the subjects tested each group of samples in turn.

[0112] Light source: Daylight simulator xenon arc lamp, all performance indicators meet the measurement specification requirements.

[0113] Test method: Test in accordance with the specific requirements of the "Technical Specifications for Safety of Cosmetics" (2015 edition). The subject lies prone and the back is exposed to the radiation. The minimum amount of darkening of the subject's skin to ultraviolet radiation (MPPD value) is predicted 24 hours before the test, and the amount of ultraviolet radiation is adjusted according to the predicted results for testing the test object. The test first selects a spot no less than 30cm on the subject's back. 2 For normal skin area, apply the test object or reference product evenly on the above area at a dosage of (2.00±0.05) mg / cm; then select the UVA exposure amount according to the specification requirements, and irradiate in three conditions: ① No test object applied to the subject's skin; ② Apply reference product; ③ Apply test object. Observe the experimental results after 4 hours, and record the MPPD values ​​in the three conditions respectively.

[0114] PFA value calculation method: The PFA value of the test substance or reference substance protecting a single subject is expressed as follows:

[0115]

[0116] The results are shown in Table 2.

[0117] Table 2

[0118]

[0119]

[0120] Test Example 3

[0121] Test method:

[0122] (1) Number of people: 30

[0123] (2) Gender: 90% female, 10% male

[0124] (3) Age range: 25% are between 18 and 30 years old, 30% are between 31 and 40 years old, 40% are between 41 and 50 years old, and 5% are over 50 years old

[0125] (4) Products: Examples 1-12, Comparative Example 1

[0126] (5) Number of times used: Blind test, use for 1 week each

[0127] (6) Evaluation method: Self-evaluation, with a 5-point scale, 5 points for the best effect and 1 point for the worst effect

[0128] (7) Evaluation dimensions: Moisturizing degree after use, skin softness after use, and gentleness of use

[0129] The results are shown in Table 3.

[0130] Table 3

[0131]

[0132]

[0133] Test Example 4

[0134] Human skin patch test

[0135] Test sample: Example 1

[0136] Negative control: blank control

[0137] Subjects: A total of 30 subjects, including 3 males and 27 females, aged 28 to 59 years old, with an average age of 42.4±9.5 years old, met the voluntary inclusion criteria.

[0138] Patch test method: Select qualified patch test equipment and use the closed patch test method. After shaking the test substance, take about 0.02g (white emulsion) and place it in the patch tester. Apply it to the back of the subject with low-allergenic tape. Remove the test substance after 24 hours, observe the skin reaction 0.5, 24, and 48 hours after removal, and record the results according to the skin reaction grading standards in the "Technical Specifications for Safety of Cosmetics" (2015 edition).

[0139] Table 4

[0140]

[0141]

[0142] It can be seen from the data in Table 4 that the product of the present invention is mild and no adverse reactions occurred among the 30 subjects.

[0143] Test Example 5

[0144] Multiple skin irritation tests

[0145] Test substance: Example 1

[0146] 1. Experimental Animal Information

[0147] Species: Rabbit;

[0148] Strain: New Zealand rabbit;

[0149] Level: General;

[0150] Number of animals: 4, female animals were selected that were not pregnant or had not given birth;

[0151] Weight: 2.3kg~2.5kg;

[0152] Source: Danyang Changyi Experimental Animal Breeding Co., Ltd.

[0153] Laboratory Animal Production License Number: SCXK(Su)2021-0002;

[0154] Quality certificate number: N0.202329951.

[0155] 2. Rearing environment information

[0156] Temperature: 20.0℃~25.6℃;

[0157] Relative humidity: 47.4%~69.8%;

[0158] Laboratory Animal Environment Use License Number: SYXK(Su)2020-0017.

[0159] 3. Feed information

[0160] Feed source: Suzhou Anmufei Biotechnology Co., Ltd.;

[0161] Feed qualification certificate: R02-20230329002.

[0162] 4. Test methods:

[0163] The samples submitted by the client were subjected to multiple skin irritation tests in accordance with the "Safety Technical Specifications for Cosmetics" (2015 edition). Before the test, the animals were adapted to the experimental animal room environment for 3 days. About 24 hours before the test, the hair on both sides of the spine of the experimental animals was shaved, and the hair removal range was about 3cm×3cm on the left and right. During the test, 0.5mL of the test substance was applied to the left skin, with an application area of ​​about 2.5cm×2.5cm, and the right skin was used as a control. Apply once a day for 14 consecutive days. Starting from the second day, shave before each application, use olive oil to remove the residual test substance, observe the skin reaction after one hour, and score the skin irritation reaction according to Table 1 in Chapter 6 4 Skin Irritation / Corrosion Test of the "Safety Technical Specifications for Cosmetics" (2015 edition). The average score of each animal per day was calculated according to the formula, and the skin irritation intensity was graded according to Table 2. The results are shown in Table 5.

[0164] Table 5

[0165]

[0166]

[0167] Test Example 6

[0168] Skin allergy test

[0169] 1. Test substance: Example 1

[0170] 2. Positive substances

[0171] Name: 1-Chloro-2,4-dinitrobenzene;

[0172] Lot number: WT6CA-LI;

[0173] Manufacturer: Tokyo Chemical Industry Co., Ltd.

[0174] Solvent: acetone sesame oil solution (acetone: sesame oil 1:1);

[0175] Induction and stimulation concentrations: 1%, 0.5%;

[0176] Dosage: 0.2mL.

[0177] 3. Experimental Animal Information

[0178] Species: Guinea pig;

[0179] Strain: Hartley guinea pig;

[0180] Level: General;

[0181] Number of animals: 20 in the sample test group, 10 in the negative control group, and 20 in the positive control group, half male and half female, and female animals were selected from those that were not pregnant and had not given birth;

[0182] Weight: 242.3g~285.0g;

[0183] Source: Danyang Changyi Experimental Animal Breeding Co., Ltd.

[0184] Laboratory Animal Production License Number: SCXK(Su)2021-0002;

[0185] Quality certificate number: NO.202328117.

[0186] 4. Rearing environment information

[0187] Temperature: 21.3℃~26.8℃;

[0188] Relative humidity: 41.5%~67.5%;

[0189] Laboratory Animal Environment Use License Number: SYXK(Su)2020-0017.

[0190] 5. Feed information

[0191] Feed source: Suzhou Anmufei Biotechnology Co., Ltd.;

[0192] Feed qualification certificate: G02-20230307001; G02-20230414002.

[0193] 6. Test methods

[0194] The samples submitted by the client were subjected to skin allergy test according to the "Technical Specifications for Safety of Cosmetics" (2015 edition). The animals were adapted to the experimental animal room environment for 3 days before the test. Induced contact: 24 hours before the test, the left side of the guinea pig's back was depilated, and the depilation range was about 4cm 2 . During the test, 0.2 mL of the test substance was applied to the hairless area of ​​the experimental animal, covered with two layers of gauze and one layer of cellophane, and then fixed with a non-irritating tape for 6 hours. The same method was repeated on the 7th and 14th days. The negative control group was treated with distilled water, and the positive control group was treated with 1% 1-chloro-2,4-dinitrobenzene. Provocative contact: 14 days after the last induction, 0.2 mL of the test substance was applied to the hairless area on the right side of the experimental animal (hair was removed 24 hours before contact), covered with two layers of gauze and one layer of cellophane, and then fixed with a non-irritating tape for 6 hours. The negative control group was treated with the test substance in the same way during the provocative contact, and the positive control group was treated with 0.5% 1-chloro-2,4-dinitrobenzene. Skin allergic reactions were observed 24 hours and 48 hours after the provocative contact, and the skin reaction scores and sensitization intensity were graded according to Table 3 of Chapter 6 Skin Allergy Test Table of "Safety Technical Specifications for Cosmetics" (2015 Edition). Table 6 shows the grouping and processing, and Table 7 shows the test results.

[0195] Table 6

[0196]

[0197] Table 7

[0198]

[0199] The results are shown in Table 7. No skin allergic reaction was observed.

[0200] Test Example 7

[0201] Skin phototoxicity test

[0202] 1. Test substance: Example 1

[0203] 2. Positive substance: 8-methoxypsoralea corylifolia

[0204] Batch number: H1927173;

[0205] Manufacturer: Aladdin;

[0206] Solvent: acetone;

[0207] Concentration: 0.05%;

[0208] Dosage: 0.2mL.

[0209] 3. Experimental Animal Information

[0210] Species: Guinea pig;

[0211] Strain: Hartley guinea pig;

[0212] Level: General;

[0213] Number of animals: 6, female animals were selected that were not pregnant or had not given birth; Weight: 244.8 g to 286.4 g;

[0214] Source: Danyang Changyi Experimental Animal Breeding Co., Ltd.

[0215] Laboratory Animal Production License Number: SCXK(Su)2021-0002;

[0216] Quality certificate number: NO.202327306.

[0217] 4. Rearing environment information

[0218] Temperature: 20.4°C to 27.7°C;

[0219] Relative humidity: 43.1%~59.0%;

[0220] Laboratory Animal Environment Use License Number: SYXK(Su)2020-0017.

[0221] 5. Feed information

[0222] Feed source: Suzhou Anmufei Biotechnology Co., Ltd.;

[0223] Feed qualification certificate: G02-20230307001; G02-20230414002.

[0224] 6. Instruments

[0225] Light source manufacturer: Tianjin Development Zone Hepu Industry and Trade Co., Ltd.:

[0226] Model: HOPE-MED 8130B Skin Phototoxicity Tester.

[0227] 7. Test methods:

[0228] The samples submitted by the client are subjected to skin phototoxicity test in accordance with the Technical Specifications for Safety of Cosmetics (2015 edition).

[0229] Determination of UV light intensity: Before the experiment, a radiation meter was used to measure the light intensity (mW / cm 2 ), calculated as average value. Calculation of UV light source irradiation time: irradiation dose is 10J / cm 2 , calculate the irradiation time according to the following formula.

[0230]

[0231] Average light intensity and exposure time: The average light intensity of UVA (wavelength 365nm) is 6.25mW / cm 2 The irradiation time was 26 minutes and 36 seconds.

[0232] Test steps: Animals were adapted to the experimental animal room environment for 3 days before the test. The guinea pigs were depilated on their backs 24 hours before the test. Four intact skins were selected on both sides of the back, each with a depilatory area of ​​about 2cm×2cm, with areas 1 and 3 on the left and areas 2 and 4 on the right. The animals were fixed, and 0.2mL of the test substance was applied to the depilatory areas 1 and 2 of the animals. After 30 minutes, the depilatory areas 1 and 3 were covered with aluminum foil, fixed with tape, and the right side was irradiated with UVA. After the test, the skin reaction was observed at 1, 24, 48 and 72 hours respectively. The positive control group was tested in the same way. The skin reaction was scored according to Table 2 of Chapter 6, 7 Skin Phototoxicity Test of the "Technical Specifications for Safety of Cosmetics" (2015 Edition). The results of the positive control test on the guinea pig skin phototoxicity are shown in Table 8, and the results of the test substance test on the guinea pig skin phototoxicity are shown in Table 9.

[0233] Table 8

[0234]

[0235] Table 9

[0236]

[0237] The results of the phototoxicity test of the test substance on guinea pig skin were: no skin phototoxicity was observed.

[0238] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate a water-dispersed children's sunscreen lotion and its preparation method of the present invention, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary ingredients, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0239] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0240] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A water-dispersed children's sunscreen lotion, characterized in that: The raw materials for preparing the children's sunscreen lotion include, by mass percentage, titanium dioxide, 12% silica composite, 2% C20-22 alcohol phosphate and C20-22 alcohol mixture, 2% di(lauryl glutamine) lysine, 3% butylene glycol, 3% glycerol, 3% 1,2-pentanediol, 3% stearyl glycyrrhetinate, 0.5% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, 0.5% polysorbate-60, 0.5% sorbitan isostearate, 0.5% bentonite, 0.5% xanthan gum and water, wherein the silica is coated on the surface of the titanium dioxide; The mass ratio of titanium dioxide to silica is 9:1; The mass ratio of the C20-22 alcohol phosphate to the C20-22 alcohol is 1:

1.

2. The water-dispersed children's sunscreen lotion according to claim 1, characterized in that: The children's sunscreen lotion further comprises any one or a combination of at least two selected from emollients, antioxidants or pH regulators.

3. The water-dispersed children's sunscreen lotion according to claim 2, characterized in that: The children's sunscreen lotion further comprises, by mass percentage, any one or a combination of at least two selected from 7-15% of a moisturizer, 0.5-2% of an antioxidant, or 0.2-0.6% of a pH adjuster.

4. The water-dispersed children's sunscreen lotion according to claim 2, characterized in that: The pH adjuster is selected from arginine and / or citric acid.

5. The water-dispersed children's sunscreen lotion according to claim 2, characterized in that: The antioxidant is selected from p-hydroxyacetophenone and / or tocopherol acetate.

6. The water-dispersed children's sunscreen lotion according to claim 2, characterized in that: The emollient is selected from any one of triethylhexanoin, coconut oil alcohol-caprylate / caprate, polydimethylsiloxane or squalane, or a combination of at least two thereof.

7. The water-dispersed children's sunscreen lotion according to claim 6, characterized in that: The emollient is a combination of triethylhexanoin, coco-caprylate / caprate, dimethicone and squalane.

8. The method for preparing the water-dispersed children's sunscreen lotion according to any one of claims 1 to 7, characterized in that: The preparation method comprises: mixing a sunscreen, a thickener, a moisturizer and water, and homogenizing them; and then mixing them with an emulsifier, and homogenizing them to obtain the sunscreen.

9. The method for preparing the water-dispersed children's sunscreen lotion according to claim 8, characterized in that: The homogenization time is independently 5-15 min.

10. The method for preparing the water-dispersed children's sunscreen lotion according to claim 8, characterized in that: The temperature of the mixing is independently 60-80°C.

11. The method for preparing the water-dispersed children's sunscreen lotion according to claim 8, characterized in that: The mixing with the emulsifier is carried out under vacuum conditions.

12. The method for preparing the water-dispersed children's sunscreen lotion according to claim 8, characterized in that: The sunscreen, thickener, moisturizer and water are mixed together with a pH adjuster.

13. The method for preparing the water-dispersed children's sunscreen lotion according to claim 8, characterized in that: The mixing with the emulsifier also includes mixing with an emollient and / or an antioxidant.

Images