Mineral moisturizing, whitening and sunscreen isolation lotion and preparation method thereof

Abstract

The invention provides a mineral moisturizing, whitening and sunscreen isolation lotion and a preparation method thereof, and belongs to the technical field of cosmetics. The raw materials comprise a phase A, a phase B and a phase C. The preparation method comprises the following steps: heating water in the phase A to 80-90 DEG C, adding other raw materials in the phase A, and uniformly stirring and dispersing; uniformly mixing, stirring and dispersing the phase B; dropwise adding the mixed and dispersed phase A into the phase B, and uniformly stirring and dispersing; finally, adding the phase C, and emulsifying for 10-15 minutes at the speed of 5000-7000 r / min to obtain the mineral moisturizing, whitening and sunscreen isolation lotion. The mineral moisturizing, whitening and sunscreen isolation lotion prepared by the invention is simple in preparation method, good in moisturizing performance, relatively good in whitening, anti-ultraviolet, anti-oxidation and anti-inflammatory effects, non-irritant, safe, not easy to cause anaphylactic reaction, appropriate in consistency, uniform, fine, easy to smear and comfortable in skin feeling; and meanwhile, a relatively strong ultraviolet protection effect is achieved.

Description

Technical Field

[0001] The invention relates to the technical field of cosmetics, and in particular to a mineral moisturizing, whitening, sunscreen and isolation lotion and a preparation method thereof. Background Art

[0002] Sunlight is one of the basic elements for human survival and health, but the ultraviolet rays of the sun can also cause great harm to the skin. Excessive sun exposure can easily cause various skin diseases. With the improvement of people's quality of life, the concept of skin care has gradually extended from facial care to the whole body. Under the strong ultraviolet rays in summer, the skin barrier is easily damaged, and the skin collagen and elastic fiber tissue will also be damaged, which will weaken the ductility of the skin and cause symptoms such as tanning, sunburn, erythema, itching, pain and even ulcers. Long-term exposure to ultraviolet rays can cause allergic reactions such as skin allergies, swelling, and tingling. Ultraviolet rays can also cause the skin to lose elasticity, causing aging phenomena such as skin wrinkles, rough skin, and sagging skin. The nutrient structure in the skin will also change, and even lead to serious diseases such as skin cancer, melanoma, and actinic keratosis.

[0003] In response to this phenomenon, various sunscreen products such as sunscreen have appeared on the market. Sunscreen is a skin care product made using the sunscreen principle to protect the skin from ultraviolet rays, thereby avoiding the production and accumulation of melanin. It is applied on the skin to prevent sunlight from contacting the skin, and has the effects of full-body sun protection, refreshing and moisturizing, and nourishing the skin. In the hot summer, ultraviolet rays seriously affect people's skin condition and cause varying degrees of damage to human skin, but existing products have the disadvantages of low sunscreen or sunscreen ability but easy to make the skin dry. Summary of the invention

[0004] The purpose of the present invention is to provide a mineral moisturizing, whitening, sunscreen and isolation lotion and a preparation method thereof. The preparation method is simple, the moisturizing performance is good, the whitening, UV protection, antioxidant and anti-inflammatory effects are good, the lotion is non-irritating, safe and not easy to cause allergic reactions, the consistency is suitable, the lotion is uniform and delicate, the lotion is easy to apply, the skin feels comfortable, and at the same time, it has a strong UV protection effect.

[0005] The technical solution of the present invention is achieved in this way:

[0006] The present invention provides a mineral moisturizing, whitening, sunscreen and isolation lotion, the raw materials of which are composed of phase A, phase B and phase C, and the weight proportions of the raw materials are as follows:

[0007] Phase A: 20-30 parts of water, 0.05-0.15 parts of methylparaben, 0.05-0.15 parts of disodium EDTA, 0.8-1.3 parts of sodium chloride, 0.1-0.3 parts of allantoin collagen conjugate liposome, 0.05-0.15 parts of hydrolyzed hyaluronic acid salicylate, 0.1-0.2 parts of betaine, 5-8 parts of glycerol, 10-15 parts of butylene glycol;

[0008] Phase B: 2-3 parts of cetyl PEG / PPG-10 / 1 polydimethylsiloxane, 0.8-1.3 parts of sorbitan sesquioleate, 5-8 parts of mineral oil, 0.2-0.3 parts of aluminum hydroxide, 0.1-0.3 parts of polydimethylsiloxane, 0.2-0.3 parts of triethoxycaprylylsilane, 3-5 parts of modified titanium dioxide, 3-5 parts of hydrogenated polyisobutene, 3-5 parts of capric triglyceride, 3-5 parts of isopropyl myristate, 0.05-0.2 parts of bisabolol, 1-2 parts of C12-15 alcohol benzoate, 0.5-1 parts of magnesium stearate, 0.1-0.2 parts of polyglyceryl-3 polyricinoleate, and 0.1-0.2 parts of lecithin;

[0009] Phase C: 0.5-1 part of trehalose, 0.01-0.015 part of phenoxyethanol, 0.1-0.2 part of hydroxyethyl cellulose, 1-2 parts of oat (AVENA SATIVA) peptide, 0.1-0.2 parts of 1,2-hexanediol, 0.2-0.3 parts of ethylhexylglycerin, and 0.05-0.2 parts of fragrance.

[0010] As a further improvement of the present invention, the preparation method of the allantoin-collagen conjugate liposome is as follows:

[0011] S1. Add collagen peptide to water, add NHS and EDC, stir to activate, add allantoin, stir to react, and prepare allantoin collagen conjugate;

[0012] S2. Mix hydrogenated lecithin and cholesterol, add chloroform to dissolve, add allantoin collagen conjugate, remove the solvent under reduced pressure, then add poloxamer 188, heat and stir to hydrate, and perform ultrasonic crushing to obtain allantoin collagen conjugate liposomes.

[0013] As a further improvement of the present invention, the mass ratio of collagen peptide, NHS, EDC and allantoin in step S1 is 10:2-3:3-4:5-7, the stirring activation temperature is 0-4°C, the time is 20-30min, and the stirring reaction time is 7-10h.

[0014] As a further improvement of the present invention, the mass ratio of hydrogenated lecithin, cholesterol, allantoin collagen conjugate and poloxamer 188 in step S2 is 3-5:1-2:0.8-1.5:0.2-0.3, the temperature of the heating and stirring hydration is 55-65°C, the rotation speed is 20-30r / min, the time is 20-30min, and the power of the ultrasonic crushing treatment is 1000-2000W, and the time is 15-25min.

[0015] As a further improvement of the present invention, the preparation method of the hydrolyzed hyaluronic acid salicylate is as follows:

[0016] T1. Add hyaluronic acid to water, add hyaluronidase, perform microenzyme hydrolysis, inactivate the enzyme, and obtain hydrolyzed hyaluronic acid;

[0017] T2. Add hydrolyzed hyaluronic acid into toluene, add salicylic acid and concentrated sulfuric acid, heat to reflux and stir to react, remove the solvent under reduced pressure to obtain hydrolyzed hyaluronic acid salicylate.

[0018] As a further improvement of the present invention, the mass ratio of hyaluronic acid and hyaluronidase in step T1 is 100:2-3, the temperature of the micro-enzymatic hydrolysis is 20-30°C, the time is 10-20min, and the enzyme inactivation method is heating to 100-110°C and inactivating the enzyme for 15-20min; the mass ratio of hydrolyzed hyaluronic acid, salicylic acid and concentrated sulfuric acid in step T2 is 15-20:4-7:2-3, and the heating reflux stirring reaction time is 5-7h.

[0019] As a further improvement of the present invention, the preparation method of the modified titanium dioxide is as follows:

[0020] U1. Preparation of regenerated silk fibroin solution: add mulberry silk to sodium carbonate solution, heat and boil to degumming, filter, dissolve in lithium bromide solution, dialyze, freeze-dry the non-permeated solution to obtain regenerated silk fibroin;

[0021] U2. Preparation of tannic acid modified titanium dioxide: adding nano titanium dioxide powder to water, adding tannic acid and a catalyst, heating and stirring to react, centrifuging, washing, and drying to obtain tannic acid modified titanium dioxide;

[0022] U3. Preparation of modified titanium dioxide: Add tannic acid-modified titanium dioxide into water, add NHS and EDC, stir to activate, add regenerated silk fibroin, stir to react, centrifuge, wash, and dry to obtain modified titanium dioxide.

[0023] As a further improvement of the present invention, the concentration of the sodium carbonate solution in step U1 is 0.4-0.6wt%, the heating and boiling degumming time is 30-50min, the concentration of the lithium bromide solution is 8-10mol / L, the dialysis bag pore size used in the dialysis is 10-15kDa, and the time is 36-72h.

[0024] As a further improvement of the present invention, the average particle size of the nano titanium dioxide powder described in step U2 is 200-500nm, the mass ratio of the nano titanium dioxide powder, tannic acid and catalyst is 10:2-3:0.5-1, the pH of the catalyst is Tris-HCl solution of 9-10, the temperature of the heating and stirring reaction is 40-50°C, and the time is 2-4h; the mass ratio of tannic acid-modified titanium dioxide, NHS, EDC and regenerated silk fibroin described in step U3 is 12-15:3-4:4-5:7-10, the stirring activation time is 10-20min, and the stirring reaction time is 4-6h.

[0025] The present invention further protects a method for preparing the above-mentioned mineral moisturizing, whitening and sunscreen isolation lotion, comprising the following steps:

[0026] (1) Heat the water in phase A to 80-90°C and then add other raw materials in phase A and stir to disperse evenly;

[0027] (2) Mix and stir phase B to disperse evenly;

[0028] (3) Add the mixed and dispersed phase A to phase B and stir to disperse evenly;

[0029] (4) Finally, add phase C and emulsify at 5000-7000 r / min for 10-15 min to obtain a mineral moisturizing, whitening and sunscreen isolation lotion.

[0030] The present invention has the following beneficial effects:

[0031] The present invention prepares an allantoin collagen conjugate liposome. After allantoin and collagen are coupled to obtain an allantoin collagen conjugate, the liposome is prepared. On the one hand, the skin irritation caused by allantoin when used alone is overcome. Long-term use may cause skin intolerance, rash may occur, accompanied by redness, peeling and other phenomena and poor water solubility. The water solubility of the product is greatly improved, and the prepared liposome has a transdermal absorption promotion effect, can disturb the skin phospholipid bilayer, promote the skin's absorption efficiency of active components, and can also increase and promote the hydration capacity of the skin stratum corneum, so that the skin retains more moisture and reduces water loss, thereby effectively improving the condition of dry skin, promoting the effect of cell proliferation and epithelial tissue growth, and accelerating the healing process of skin wounds. For skin after slight abrasions, sunburns or acne damage, allantoin can help repair damaged skin tissue, has good anti-inflammatory and antioxidant effects, can supplement the collagen content of the skin muscle bottom layer, and has the effects of anti-aging, anti-wrinkle, and promoting skin metabolism.

[0032] Hyaluronic acid has a large molecular weight and may cause allergic reactions. After micro-hydrolysis, its molecular weight is reduced and its comprehensive performance is improved. Although salicylic acid has good exfoliation and acne improvement effects when used alone, it is easy to cause inflammation and allergic reactions. The hydrolyzed hyaluronic acid salicylate obtained by esterification of salicylic acid and hydrolyzed hyaluronic acid has significantly reduced allergenicity, can form a protective film on the skin surface, lock in moisture, and improve its moisturizing and water retention properties. It can neutralize free radicals, inhibit oxidation reactions, protect cells from environmental pollution and ultraviolet radiation damage, delay the skin aging process, accelerate wound healing, promote skin cell regeneration, reduce inflammatory reactions, prevent wound infections, increase skin elasticity and firmness, and help reduce wrinkles after filling them, making the skin look younger and smoother.

[0033] Regenerated silk fibroin has anti-inflammatory and antioxidant properties, and can be used to reduce skin inflammation and promote the repair of damaged skin. Amino acid components such as leucine, serine, and threonine can accelerate cell metabolism, delay skin aging, and have moisturizing effects. Tryptophan and tyrosine can absorb ultraviolet rays and protect the skin. At the same time, they have good biocompatibility and can be fixed and modified on the surface of titanium dioxide by coupling with tannic acid to increase the content of β-sheet structure. The presence of β-sheet structure can enhance its stability, slow down the degradation rate of silk fibroin, and improve its antioxidant and ultraviolet absorption properties. Titanium dioxide has a good white color, which can absorb ultraviolet rays, reflect and scatter ultraviolet rays, and reduce the damage of ultraviolet rays to the skin. At the same time, under the modification of regenerated silk fibroin, the modified titanium dioxide obtained has a good pearly white color, which increases the beauty effect of the isolation milk.

[0034] The mineral moisturizing, whitening, sunscreen and isolation lotion prepared by the invention has a simple preparation method, good moisturizing performance, good whitening, ultraviolet protection, anti-oxidation and anti-inflammatory effects, is non-irritating, safe and not prone to allergic reactions, has a suitable consistency, is even and delicate, is easy to apply, feels comfortable on the skin, and has a strong ultraviolet protection effect. DETAILED DESCRIPTION

[0035] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0036] NHS, N-hydroxysuccinimide; EDC, 1-ethyl-(3-dimethylaminopropyl)carbodiimide, commercially available. Hyaluronidase, 50,000 U / g, purchased from Shanghai Yuanye Biotechnology Co., Ltd.; nano-titanium dioxide powder, with an average particle size of 200-500 nm, purchased from Hubei Huifu Nanomaterial Co., Ltd.; collagen, purchased from Hainan Huayan Collagen Technology Co., Ltd.

[0037] Preparation Example 1 Preparation of allantoin-collagen conjugate liposomes

[0038] Here’s how:

[0039] S1. 10g collagen peptide was added to water, 2g NHS and 3g EDC were added, and the mixture was stirred and activated at 0℃ for 20min. 5g allantoin was added, and the mixture was stirred and reacted for 7h. The mixture was dialyzed with a 5kDa dialysis bag for 12h, and the non-permeated liquid was freeze-dried to obtain allantoin collagen conjugate.

[0040] S2. Mix 3g of hydrogenated lecithin with 1g of cholesterol, add 100mL of chloroform to dissolve, then add 0.8g of allantoin-collagen conjugate, remove the solvent under reduced pressure, then add 0.2g of poloxamer 188, heat to 55°C, stir and hydrate at 20r / min for 20min, treat with 1000W ultrasonic wave for 15min, and freeze-dry to obtain allantoin-collagen conjugate lipid.

[0041] Preparation Example 2 Preparation of Allantoin-Collagen Conjugate Liposomes

[0042] Here’s how:

[0043] S1. 10g collagen peptide was added to water, 3g NHS and 4g EDC were added, and the mixture was stirred and activated at 4℃ for 30min. 7g allantoin was added, and the mixture was stirred and reacted for 10h. The mixture was dialyzed with a 5kDa dialysis bag for 12h, and the non-permeated liquid was freeze-dried to obtain allantoin collagen conjugate.

[0044] S2. Mix 5g of hydrogenated lecithin and 2g of cholesterol, add 100mL of chloroform to dissolve, then add 1.5g of allantoin-collagen conjugate, remove the solvent under reduced pressure, then add 0.3g of poloxamer 188, heat to 65°C, stir and hydrate at 30r / min for 30min, ultrasonically crush with 2000W for 25min, and freeze-dry to obtain allantoin-collagen conjugate lipid.

[0045] Preparation Example 3 Preparation of allantoin-collagen conjugate liposomes

[0046] Here’s how:

[0047] S1. 10g collagen peptide was added to water, 2.5g NHS and 3.5g EDC were added, and the mixture was stirred and activated at 2℃ for 25min. 6g allantoin was added, and the mixture was stirred and reacted for 8h. The mixture was dialyzed with a 5kDa dialysis bag for 12h, and the non-permeated liquid was freeze-dried to obtain allantoin collagen conjugate.

[0048] S2. Mix 4 g hydrogenated lecithin with 1.5 g cholesterol, add 100 mL chloroform to dissolve, then add 1.2 g allantoin collagen conjugate, remove the solvent under reduced pressure, then add 0.25 g poloxamer 188, heat to 60°C, stir and hydrate at 25 r / min for 25 min, ultrasonically crush with 1500 W for 20 min, and freeze-dry to obtain allantoin collagen conjugate lipid.

[0049] Comparative Preparation Example 1

[0050] Compared with Preparation Example 3, the difference is that step S2 is not performed.

[0051] 10g collagen peptide was added into water, 2.5g NHS and 3.5g EDC were added, and the mixture was activated by stirring at 2℃ for 25min. 6g allantoin was added, and the mixture was reacted by stirring for 8h. The mixture was dialyzed with a 5kDa dialysis bag for 12h, and the non-permeated liquid was freeze-dried to obtain allantoin collagen conjugate.

[0052] Comparative Preparation Example 2

[0053] Compared with Preparation Example 3, the difference is that step S1 is not performed.

[0054] 4 g of hydrogenated lecithin was mixed with 1.5 g of cholesterol, and 100 mL of chloroform was added to dissolve the mixture. Then, 0.75 g of collagen and 0.45 g of allantoin were added. The solvent was removed under reduced pressure. Then, 0.25 g of poloxamer 188 was added. The mixture was heated to 60°C, stirred and hydrated at 25 r / min for 25 min, and subjected to 1500 W ultrasonic crushing for 20 min. The mixture was freeze-dried to obtain allantoin-collagen conjugate lipid.

[0055] Preparation Example 4 Preparation of Hydrolyzed Hyaluronic Acid Salicylate

[0056] Here’s how:

[0057] T1. Add 10 g of hyaluronic acid (number average molecular weight of 200,000 Da) to 500 mL of water, add 0.2 g of hyaluronidase, enzymatically hydrolyze at 20°C for 10 min, heat to 100°C, and inactivate the enzyme for 15 min to obtain hydrolyzed hyaluronic acid;

[0058] T2. Add 1.5 g of hydrolyzed hyaluronic acid into 200 mL of toluene, add 0.4 g of salicylic acid and 0.2 g of concentrated sulfuric acid, heat under reflux and stir to react for 5 h, remove the solvent under reduced pressure, separate by column chromatography (the volume ratio of ethyl acetate and petroleum ether is 1:1), and obtain hydrolyzed hyaluronic acid salicylate.

[0059] Preparation Example 5 Preparation of Hydrolyzed Hyaluronic Acid Salicylate

[0060] Here’s how:

[0061] T1. Add 10 g of hyaluronic acid (number average molecular weight of 200,000 Da) to 500 mL of water, add 0.3 g of hyaluronidase, hydrolyze at 30°C for 20 min, heat to 110°C, inactivate the enzyme for 20 min, and obtain hydrolyzed hyaluronic acid;

[0062] T2. Add 2 g of hydrolyzed hyaluronic acid into 200 mL of toluene, add 0.7 g of salicylic acid and 0.3 g of concentrated sulfuric acid, heat under reflux and stir to react for 7 h, remove the solvent under reduced pressure, separate by column chromatography (the volume ratio of ethyl acetate and petroleum ether is 1:1), and obtain hydrolyzed hyaluronic acid salicylate.

[0063] Preparation Example 6 Preparation of Hydrolyzed Hyaluronic Acid Salicylate

[0064] Here’s how:

[0065] T1. Add 10 g of hyaluronic acid (number average molecular weight of 200,000 Da) to 500 mL of water, add 0.25 g of hyaluronidase, hydrolyze at 25°C for 15 min, heat to 105°C, inactivate the enzyme for 17 min, and obtain hydrolyzed hyaluronic acid;

[0066] T2. Add 1.7 g of hydrolyzed hyaluronic acid into 200 mL of toluene, add 0.55 g of salicylic acid and 0.25 g of concentrated sulfuric acid, heat under reflux and stir to react for 6 h, remove the solvent under reduced pressure, separate by column chromatography (the volume ratio of ethyl acetate and petroleum ether is 1:1), and obtain hydrolyzed hyaluronic acid salicylate.

[0067] Comparative Preparation Example 3

[0068] Compared with Preparation Example 6, the difference is that step T1 is not performed.

[0069] 1.7 g of hyaluronic acid (number average molecular weight of 200,000 Da) was added to 200 mL of toluene, and 0.55 g of salicylic acid and 0.25 g of concentrated sulfuric acid were added. The mixture was heated under reflux and stirred for 6 h. The solvent was removed under reduced pressure and separated by column chromatography (the volume ratio of ethyl acetate to petroleum ether was 1:1) to obtain hydrolyzed hyaluronic acid salicylate.

[0070] Comparative Preparation Example 4

[0071] Compared with Preparation Example 6, the difference is that step T2 is not performed.

[0072] 10 g of hyaluronic acid (number average molecular weight of 200,000 Da) was added to 500 mL of water, and 0.25 g of hyaluronidase was added. The mixture was hydrolyzed at 25° C. for 15 min, heated to 105° C., and the enzyme was inactivated for 17 min to obtain hydrolyzed hyaluronic acid.

[0073] Preparation Example 7 Preparation of modified titanium dioxide

[0074] Here’s how:

[0075] U1. Preparation of regenerated silk fibroin solution: 10 g of mulberry silk was added to 200 mL of 0.4 wt% sodium carbonate solution, heated and boiled for 30 min, filtered, dissolved in 200 mL of 8 mol / L lithium bromide solution, dialyzed for 36 h using a dialysis bag with a pore size of 10 kDa, and the non-permeated solution was freeze-dried to obtain regenerated silk fibroin;

[0076] U2. Preparation of tannic acid modified titanium dioxide: 10 g of nano titanium dioxide powder was added to 200 mL of water, 2 g of tannic acid and 0.5 g of catalyst were added, heated to 40°C, stirred for reaction for 2 h, centrifuged, washed, and dried to obtain tannic acid modified titanium dioxide;

[0077] A Tris-HCl solution of the catalyst with a pH of 9;

[0078] U3. Preparation of modified titanium dioxide: Add 12g of tannic acid-modified titanium dioxide into 200mL of water, add 3g of NHS and 4g of EDC, stir and activate for 10min, add 7g of regenerated silk fibroin, stir and react for 4h, centrifuge, wash, and dry to obtain modified titanium dioxide.

[0079] Preparation Example 8 Preparation of modified titanium dioxide

[0080] Here’s how:

[0081] U1. Preparation of regenerated silk fibroin solution: 10 g of mulberry silk was added to 200 mL of 0.6 wt% sodium carbonate solution, heated and boiled for degumming for 50 min, filtered, dissolved in 200 mL of 10 mol / L lithium bromide solution, dialyzed for 72 h using a dialysis bag with a pore size of 15 kDa, and the non-permeated liquid was freeze-dried to obtain regenerated silk fibroin;

[0082] U2. Preparation of tannic acid modified titanium dioxide: 10 g of nano titanium dioxide powder was added to 200 mL of water, 3 g of tannic acid and 1 g of catalyst were added, heated to 50°C, stirred for 4 h, centrifuged, washed, and dried to obtain tannic acid modified titanium dioxide;

[0083] A Tris-HCl solution of the catalyst with a pH of 10;

[0084] U3. Preparation of modified titanium dioxide: 15 g of tannic acid-modified titanium dioxide was added to 200 mL of water, 4 g of NHS and 5 g of EDC were added, and the mixture was stirred for activation for 20 min. 10 g of regenerated silk fibroin was added, and the mixture was stirred for reaction for 6 h. The mixture was centrifuged, washed, and dried to obtain modified titanium dioxide.

[0085] Preparation Example 9 Preparation of modified titanium dioxide

[0086] Here’s how:

[0087] U1. Preparation of regenerated silk fibroin solution: 10 g of mulberry silk was added to 200 mL of 0.5 wt% sodium carbonate solution, heated and boiled for 40 min, filtered, dissolved in 200 mL of 9 mol / L lithium bromide solution, dialyzed for 48 h using a dialysis bag with a pore size of 12 kDa, and the non-permeated solution was freeze-dried to obtain regenerated silk fibroin;

[0088] U2. Preparation of tannic acid modified titanium dioxide: 10 g of nano titanium dioxide powder was added to 200 mL of water, 2.5 g of tannic acid and 0.7 g of catalyst were added, heated to 45 ° C, stirred for 3 h, centrifuged, washed, and dried to obtain tannic acid modified titanium dioxide;

[0089] The catalyst has a pH of 9.5 in a Tris-HCl solution;

[0090] U3. Preparation of modified titanium dioxide: 13 g of tannic acid-modified titanium dioxide was added to 200 mL of water, 3.5 g of NHS and 4.5 g of EDC were added, and the mixture was stirred for activation for 15 min. 8 g of regenerated silk fibroin was added, and the mixture was stirred for reaction for 5 h. The mixture was centrifuged, washed, and dried to obtain modified titanium dioxide.

[0091] Comparative Preparation Example 5

[0092] Compared with Preparation Example 9, the difference is that steps U1 and U3 are not performed.

[0093] 10 g of nano titanium dioxide powder was added to 200 mL of water, 2.5 g of tannic acid and 0.7 g of catalyst were added, heated to 45°C, stirred for reaction for 3 h, centrifuged, washed, and dried to obtain tannic acid modified titanium dioxide;

[0094] The catalyst was a Tris-HCl solution with a pH of 9.5.

[0095] Example 1

[0096] This embodiment provides a mineral moisturizing, whitening, sunscreen and isolation lotion.

[0097] Its raw materials are composed of phase A, phase B and phase C, and the proportions of each raw material are as follows:

[0098] Phase A: 20 g water, 0.05 g methylparaben, 0.05 g disodium EDTA, 0.8 g sodium chloride, 0.1 g allantoin-collagen conjugate liposome prepared in Preparation Example 1, 0.05 g hydrolyzed hyaluronic acid salicylate prepared in Preparation Example 4, 0.1 g betaine, 5 g glycerol, 10 g butylene glycol;

[0099] Phase B: 2 g of cetyl PEG / PPG-10 / 1 polydimethylsiloxane, 0.8 g of sorbitan sesquioleate, 5 g of mineral oil, 0.2 g of aluminum hydroxide, 0.1 g of polydimethylsiloxane, 0.2 g of triethoxycaprylylsilane, 3 g of modified titanium dioxide obtained in Preparation Example 6, 3 g of hydrogenated polyisobutene, 3 g of capric triglyceride, 3 g of isopropyl myristate, 0.05 g of bisabolol, 1 g of C12-15 alcohol benzoate, 0.5 g of magnesium stearate, 0.1 g of polyglyceryl-3 polyricinoleate, and 0.1 g of lecithin;

[0100] Phase C: trehalose 0.5g, phenoxyethanol 0.01g, hydroxyethylcellulose 0.1g, oat (AVENA SATIVA) peptide 1g, 1,2-hexanediol 0.1g, ethylhexylglycerin 0.2g, and fragrance 0.05g.

[0101] The preparation method comprises the following steps:

[0102] (1) Heat the water in phase A to 80°C and then add the other raw materials in phase A and stir and disperse for 20 minutes;

[0103] (2) Mix and stir phase B for 20 minutes;

[0104] (3) Add the mixed and dispersed phase A to phase B and stir and disperse for 20 minutes;

[0105] (4) Finally, add phase C and emulsify at 5000 r / min for 10 min to obtain a mineral moisturizing, whitening and sunscreen isolation lotion.

[0106] Example 2

[0107] This embodiment provides a mineral moisturizing, whitening, sunscreen and isolation lotion.

[0108] Its raw materials are composed of phase A, phase B and phase C, and the proportions of each raw material are as follows:

[0109] Phase A: 30 g water, 0.15 g methylparaben, 0.15 g disodium EDTA, 1.3 g sodium chloride, 0.3 g allantoin-collagen conjugate liposome prepared in Preparation Example 2, 0.15 g hydrolyzed hyaluronic acid salicylate prepared in Preparation Example 5, 0.2 g betaine, 8 g glycerol, 15 g butylene glycol;

[0110] Phase B: 3 g of cetyl PEG / PPG-10 / 1 polydimethylsiloxane, 1.3 g of sorbitan sesquioleate, 8 g of mineral oil, 0.3 g of aluminum hydroxide, 0.3 g of polydimethylsiloxane, 0.3 g of triethoxycaprylylsilane, 5 g of modified titanium dioxide obtained in Preparation Example 7, 5 g of hydrogenated polyisobutene, 5 g of capric triglyceride, 5 g of isopropyl myristate, 0.2 g of bisabolol, 2 g of C12-15 alcohol benzoate, 1 g of magnesium stearate, 0.2 g of polyglyceryl-3 polyricinoleate, and 0.2 g of lecithin;

[0111] Phase C: trehalose 1g, phenoxyethanol 0.015g, hydroxyethylcellulose 0.2g, oat (AVENA SATIVA) peptide 2g, 1,2-hexanediol 0.2g, ethylhexylglycerin 0.3g, and fragrance 0.2g.

[0112] The preparation method comprises the following steps:

[0113] (1) Heat the water in phase A to 90°C and add other raw materials in phase A and stir to disperse for 20 minutes;

[0114] (2) Mix and stir phase B for 20 minutes;

[0115] (3) Add the mixed and dispersed phase A to phase B and stir and disperse for 20 minutes;

[0116] (4) Finally, add phase C and emulsify at 7000 r / min for 15 min to obtain a mineral moisturizing, whitening and sunscreen isolation lotion.

[0117] Example 3

[0118] This embodiment provides a mineral moisturizing, whitening, sunscreen and isolation lotion.

[0119] Its raw materials are composed of phase A, phase B and phase C, and the proportions of each raw material are as follows:

[0120] Phase A: 25 g water, 0.1 g methylparaben, 0.1 g disodium EDTA, 1 g sodium chloride, 0.2 g allantoin-collagen conjugate liposome prepared in Preparation Example 3, 0.1 g hydrolyzed hyaluronic acid salicylate prepared in Preparation Example 6, 0.15 g betaine, 6 g glycerol, 12 g butylene glycol;

[0121] Phase B: 2.5 g of cetyl PEG / PPG-10 / 1 polydimethylsiloxane, 1 g of sorbitan sesquioleate, 6 g of mineral oil, 0.25 g of aluminum hydroxide, 0.2 g of polydimethylsiloxane, 0.25 g of triethoxycaprylylsilane, 4 g of modified titanium dioxide obtained in Preparation Example 9, 4 g of hydrogenated polyisobutene, 4 g of capric triglyceride, 4 g of isopropyl myristate, 0.1 g of bisabolol, 1.5 g of C12-15 alcohol benzoate, 0.7 g of magnesium stearate, 0.15 g of polyglyceryl-3 polyricinoleate, and 0.15 g of lecithin;

[0122] Phase C: trehalose 0.7g, phenoxyethanol 0.012g, hydroxyethylcellulose 0.15g, oat (AVENA SATIVA) peptide 1.5g, 1,2-hexanediol 0.15g, ethylhexylglycerin 0.25g, and fragrance 0.1g.

[0123] The preparation method comprises the following steps:

[0124] (1) Heat the water in phase A to 85°C and add other raw materials in phase A and stir to disperse for 20 minutes;

[0125] (2) Mix and stir phase B for 20 minutes;

[0126] (3) Add the mixed and dispersed phase A to phase B and stir and disperse for 20 minutes;

[0127] (4) Finally, add phase C and emulsify at 6000 r / min for 12 min to obtain a mineral moisturizing, whitening and sunscreen isolation lotion.

[0128] Comparative Example 1

[0129] Compared with Example 3, the difference is that the allantoin collagen conjugate liposome is replaced by the product prepared in Comparative Preparation Example 1.

[0130] Comparative Example 2

[0131] Compared with Example 3, the difference is that the allantoin-collagen conjugate liposome is replaced by the product prepared in Comparative Preparation Example 2.

[0132] Comparative Example 3

[0133] Compared with Example 3, the difference is that the hydrolyzed hyaluronic acid salicylate is replaced by the product prepared in Comparative Preparation Example 3.

[0134] Comparative Example 4

[0135] Compared with Example 3, the difference is that the hydrolyzed hyaluronic acid salicylate is replaced by the product prepared in Comparative Preparation Example 4.

[0136] Comparative Example 5

[0137] Compared with Example 3, the difference is that the modified titanium dioxide is replaced by the product prepared in Comparative Preparation Example 5.

[0138] Test Example 1

[0139] The mineral moisturizing, whitening, sunscreen and isolation lotion prepared in Examples 1-3 or Comparative Examples 1-5 was diluted 100 times with deionized water to prepare a sample solution.

[0140] RAW264.7 cells were cultured in DMEM complete medium containing 10% FBS and 1% double antibody, and the cells were digested with trypsin (containing 1 mmol / LEDTA), counted, and plated in 96-well plates at 2×10 4 Each well was incubated for 24 hours, and 162 μL of cell suspension was added to each well, with 3 replicates per group. After 24 hours, 18 μL of lipopolysaccharide solution (1 mg / L) was added to each well except the control well, and 20 μL of sample solution was added to each well, and 20 μL of PBS buffer was added to the model group. Compared with the model group, the lipopolysaccharide solution in the control group was replaced with 18 μL of PBS buffer. After incubation for 24 hours, the cell supernatant was collected, and the content of NO and TNF-α in the cell supernatant was detected according to the instructions of the kit.

[0141] The results are shown in Table 1.

[0142] Table 1

[0143]

[0144]

[0145] Note: * compared with the control group, P < 0.05, # compared with the model group, P < 0.05.

[0146] It can be seen from the above table that the mineral moisturizing, whitening and sunscreen isolation lotions prepared in Examples 1-3 of the present invention have good anti-inflammatory effects.

[0147] Test Example 2

[0148] The mineral moisturizing, whitening, sunscreen and isolation lotion prepared in Examples 1-3 or Comparative Examples 1-5 was diluted 100 times with deionized water to prepare a sample solution.

[0149] NIH-3T3 cells were cultured in DMEM complete medium containing 10% FBS and 1% double antibody, and the cells were digested with trypsin (containing 1mmol / LEDTA), counted, and plated in 96-well plates at 5×10 4 135 μL of cell suspension was added to each well, and 4 wells were added to each group. After 24 hours, ultraviolet irradiation was performed, using UVB with a wavelength of 311 nm and an irradiation intensity of 13 mW / cm 2 The distance between the cells and the irradiation source was 11 cm, and the irradiation dose was set to 4000 mJ / cm 2 After irradiation, the sample solution was added immediately. Deionized water was used instead of mineral moisturizing, whitening and sunscreen for the UVB group. After incubation, the cells were cultured for 24 h. 20 μL (5 mg / mL) of MTT solution was added to each well. The cells were cultured for 4 h. Then, 100 μL of triple lysis buffer was added to each well. After overnight at 37 °C, the OD was detected by an enzyme-labeled instrument. 570 The control group was not exposed to ultraviolet rays, and deionized water was used instead of mineral moisturizing, whitening and sunscreen lotion.

[0150] The results are shown in Table 2.

[0151] Table 2

[0152]

[0153]

[0154] Note: * compared with the control group, P < 0.05, # compared with the UVB group, P < 0.05.

[0155] It can be seen from the above table that the mineral moisturizing, whitening and sunscreen isolation lotions prepared in Examples 1-3 of the present invention have good anti-ultraviolet effects.

[0156] Test Example 3: Removal rate of OH

[0157] The mineral moisturizing, whitening, sunscreen and isolation lotion prepared in Examples 1-3 or Comparative Examples 1-5 was diluted 100 times with deionized water to prepare a sample solution.

[0158] Take 2mL 1.00×10 -2 mol / L salicylic acid-ethanol solution, 2mL 9.00×10 -3 mol / L FeSO4 solution and sample solution were added to the test tube, and then 2mL 8.8×10 -2 mol / L H2O2 solution, shake well and place in a 37℃ water bath for 30 min, and measure the absorbance A at 510 nm. i ; Use 2mL pure water instead of salicylic acid solution to measure the absorbance A j; 2 mL of pure water was used instead of the sample solution to determine the absorbance A0. The OH clearance rate (%) was calculated according to the formula. Vitamin C (0.1 mg / mL) was used as the control group.

[0159] ·OH removal rate (%) = [1-(A i -A j ) / A0]×100%

[0160] The results are shown in Table 3.

[0161] Table 3

[0162]

[0163]

[0164] It can be seen from the above table that the mineral moisturizing, whitening and sunscreen isolation lotions prepared in Examples 1-3 of the present invention have good antioxidant effects.

[0165] Test Example 4: Human skin patch test and allergy test

[0166] Subjects with an age distribution of 22-50 years old were selected and randomly divided into 8 groups, with 10 people in each group. Among them, a 5cm×5cm area was marked on the flexor side of the right forearm of the subject and medical disinfection was used to create a wound in the marked area. A 36-pin microneedle was used to introduce the nutrient solution for 30s, and the residual liquid was gently wiped with a cotton ball to keep the marked area dry; the test samples (mineral moisturizing, whitening and sunscreen isolation milk prepared in Examples 1-3 of the present invention and Comparative Examples 1-5) were placed in the No. 1-8 spot tester holes respectively, with a dosage of 15μL. Bathing was prohibited during the test, and a negative reaction was normal. The test samples were applied to the face, neck and back of the ear of the subject, and the skin condition of the subject was observed after 10 minutes.

[0167] The results are shown in Table 4.

[0168] Table 4

[0169]

[0170]

[0171] It can be seen from the above table that the patch reactions of the mineral moisturizing, whitening, sunscreen and isolation lotions prepared in Examples 1-3 of the present invention are negative reactions, and are safe to use without any allergic reactions.

[0172] Test Example 5 Skin Moisturizing Test

[0173] Female subjects aged 19-53 were selected on a voluntary basis and randomly divided into 17 groups, each with 6 people, including Examples 1-3 and Comparative Examples 1-5. No products irrelevant to the test were applied during the test, and the subjects used samples on both sides of their faces. The sample group used the mineral moisturizing, whitening, sunscreen and isolation milk prepared in Examples 1-3 and Comparative Examples 1-5. Once a day for 2 weeks, before the test, the subjects washed the test area with clean water, wiped it dry, and sat quietly for 20 minutes in a constant environment of 25±1°C and a relative humidity of 45±5%.

[0174] The stratum corneum moisture content was measured before the test, and the stratum corneum moisture content of the subjects was tested 1 hour after using the sample on the 14th day, and the skin moisture content change rate (%) was calculated. The stratum corneum moisture content of the test site was tested using a skin moisture tester, and the average value was taken for 5 times.

[0175] Skin moisture content change rate (%) = (moisture content after use - moisture content before use) / moisture content before use × 100%

[0176] The results are shown in Table 5.

[0177] Table 5

[0178]

[0179]

[0180] It can be seen from the above table that the mineral moisturizing, whitening, sunscreen and isolation lotions prepared in Examples 1-3 of the present invention have good moisturizing effects.

[0181] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A mineral moisturizing, whitening, sunscreen and isolation lotion, characterized in that: The raw materials are composed of phase A, phase B and phase C, and the weight proportions of the raw materials are as follows: Phase A: 20-30 parts of water, 0.05-0.15 parts of methylparaben, 0.05-0.15 parts of disodium EDTA, 0.8-1.3 parts of sodium chloride, 0.1-0.3 parts of allantoin collagen conjugate liposome, 0.05-0.15 parts of hydrolyzed hyaluronic acid salicylate, 0.1-0.2 parts of betaine, 5-8 parts of glycerol, 10-15 parts of butylene glycol; Phase B: 2-3 parts of cetyl PEG / PPG-10 / 1 polydimethylsiloxane, 0.8-1.3 parts of sorbitan sesquioleate, 5-8 parts of mineral oil, 0.2-0.3 parts of aluminum hydroxide, 0.1-0.3 parts of polydimethylsiloxane, 0.2-0.3 parts of triethoxycaprylylsilane, 3-5 parts of modified titanium dioxide, 3-5 parts of hydrogenated polyisobutene, 3-5 parts of capric triglyceride, 3-5 parts of isopropyl myristate, 0.05-0.2 parts of bisabolol, 1-2 parts of C12-15 alcohol benzoate, 0.5-1 parts of magnesium stearate, 0.1-0.2 parts of polyglyceryl-3 polyricinoleate, and 0.1-0.2 parts of lecithin; Phase C: 0.5-1 part of trehalose, 0.01-0.015 part of phenoxyethanol, 0.1-0.2 part of hydroxyethyl cellulose, 1-2 parts of oat (AVENASATIVA) peptide, 0.1-0.2 parts of 1,2-hexanediol, 0.2-0.3 parts of ethylhexylglycerin, and 0.05-0.2 parts of fragrance.

2. The mineral moisturizing, whitening, sunscreen and isolation lotion according to claim 1, characterized in that: The preparation method of the allantoin-collagen conjugate liposome is as follows: S1. Add collagen peptide to water, add NHS and EDC, stir to activate, add allantoin, stir to react, and prepare allantoin collagen conjugate; S2. Mix hydrogenated lecithin and cholesterol, add chloroform to dissolve, add allantoin collagen conjugate, remove the solvent under reduced pressure, then add poloxamer 188, heat and stir to hydrate, and perform ultrasonic crushing to obtain allantoin collagen conjugate liposomes.

3. The mineral moisturizing, whitening, sunscreen and isolation lotion according to claim 2, characterized in that: In step S1, the mass ratio of collagen peptide, NHS, EDC and allantoin is 10:2-3:3-4:5-7, the stirring activation temperature is 0-4°C, the time is 20-30min, and the stirring reaction time is 7-10h.

4. The mineral moisturizing, whitening and sunscreen isolation lotion according to claim 2, characterized in that: The mass ratio of hydrogenated lecithin, cholesterol, allantoin collagen conjugate and poloxamer 188 in step S2 is 3-5:1-2:0.8-1.5:0.2-0.3, the temperature of the heating and stirring hydration is 55-65°C, the speed is 20-30r / min, the time is 20-30min, and the power of the ultrasonic crushing treatment is 1000-2000W, and the time is 15-25min.

5. The mineral moisturizing, whitening, sunscreen and isolation lotion according to claim 1, characterized in that: The preparation method of the hydrolyzed hyaluronic acid salicylate is as follows: T1. Add hyaluronic acid to water, add hyaluronidase, perform microenzyme hydrolysis, inactivate the enzyme, and obtain hydrolyzed hyaluronic acid; T2. Add hydrolyzed hyaluronic acid into toluene, add salicylic acid and concentrated sulfuric acid, heat to reflux and stir to react, remove the solvent under reduced pressure to obtain hydrolyzed hyaluronic acid salicylate.

6. The mineral moisturizing, whitening, sunscreen and isolation lotion according to claim 5, characterized in that: In step T1, the mass ratio of hyaluronic acid and hyaluronidase is 100:2-3, the temperature of the micro-enzymatic hydrolysis is 20-30°C, the time is 10-20min, and the enzyme inactivation method is heated to 100-110°C and the enzyme inactivation treatment is 15-20min; in step T2, the mass ratio of hydrolyzed hyaluronic acid, salicylic acid and concentrated sulfuric acid is 15-20:4-7:2-3, and the heating reflux stirring reaction time is 5-7h.

7. The mineral moisturizing, whitening, sunscreen and isolation lotion according to claim 1, characterized in that: The preparation method of the modified titanium dioxide is as follows: U1. Preparation of regenerated silk fibroin solution: add mulberry silk to sodium carbonate solution, heat and boil to degumming, filter, dissolve in lithium bromide solution, dialyze, freeze-dry the non-permeated solution to obtain regenerated silk fibroin; U2. Preparation of tannic acid modified titanium dioxide: adding nano titanium dioxide powder to water, adding tannic acid and a catalyst, heating and stirring to react, centrifuging, washing, and drying to obtain tannic acid modified titanium dioxide; U3. Preparation of modified titanium dioxide: Add tannic acid-modified titanium dioxide into water, add NHS and EDC, stir to activate, add regenerated silk fibroin, stir to react, centrifuge, wash, and dry to obtain modified titanium dioxide.

8. The mineral moisturizing, whitening, sunscreen and isolation lotion according to claim 7, characterized in that: The concentration of the sodium carbonate solution in step U1 is 0.4-0.6wt%, the heating and boiling degumming time is 30-50min, the concentration of the lithium bromide solution is 8-10mol / L, the dialysis bag pore size used in the dialysis is 10-15kDa, and the time is 36-72h.

9. The mineral moisturizing, whitening, sunscreen and isolation lotion according to claim 7, characterized in that: The average particle size of the nano titanium dioxide powder described in step U2 is 200-500nm, the mass ratio of the nano titanium dioxide powder, tannic acid and catalyst is 10:2-3:0.5-1, the pH of the catalyst is Tris-HCl solution of 9-10, the temperature of the heating and stirring reaction is 40-50°C, and the time is 2-4h; the mass ratio of tannic acid-modified titanium dioxide, NHS, EDC and regenerated silk fibroin described in step U3 is 12-15:3-4:4-5:7-10, the stirring activation time is 10-20min, and the stirring reaction time is 4-6h.

10. A method for preparing the mineral moisturizing, whitening, sunscreen and isolation lotion according to any one of claims 1 to 9, characterized in that: The following steps are involved: (1) Heat the water in phase A to 80-90°C and then add other raw materials in phase A and stir to disperse evenly; (2) Mix and stir phase B to disperse evenly; (3) Add the mixed and dispersed phase A to phase B and stir to disperse evenly; (4) Finally, add phase C and emulsify at 5000-7000 r / min for 10-15 min to obtain a mineral moisturizing, whitening and sunscreen isolation lotion.

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