Ultra-fine emulsified spray cream containing oryzanol and preparation method of ultra-fine emulsified spray cream

Abstract

The invention relates to the technical field of cosmetics, in particular to ultra-fine emulsified spray cream containing oryzanol and a preparation method thereof.The ultra-fine emulsified spray cream is prepared from, by weight, 0.1%-8% of oryzanol, 0.1%-10% of emulsifier, 10%-30% of grease, 4%-10% of polyhydric alcohol, 1%-10% of thickener and the balance water; the critical stacking parameter of the emulsifier is 0.8 to 1.2; the thickening agent is prepared from at least one of a thickening agent GT-730, a thickening agent Tinovis GTC UP, a thickening agent Volalen FL, a thickening agent Aristoflex BLV, a thickening agent Carbomer U20, a thickening agent Carbomer U30 and a thickening agent Cosmedia SP, and the thickening agent is prepared from at least one of the thickening agent GT-730, the thickening agent Tinovis GTC UP, the thickening agent Volalen FL, the thickening agent Aristoflex BLV, the thickening agent Carbomer U20, the thickening agent Carbomer U30 and the thickening agent Cosmedia SP. By compounding the specific emulsifier, the polar grease and the thickening agent, the stability and uniformity of the system are ensured, meanwhile, the viscosity of the system is maintained, the spraying smoothness is realized, and the cosmetic application requirements are met.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, specifically to an ultrafine emulsified spray cream containing oryzanol and its preparation method. Background Technology

[0002] Oryzanol is a natural active ingredient derived from rice, composed mainly of ferulic acid esters of cycloarpine and sterols, with cycloarpine ferulic acid esters comprising approximately 80%. It possesses excellent anti-inflammatory, UV absorption, whitening, and antioxidant properties, and has wide applications in the food and pharmaceutical industries. For example, Chinese invention patent CN105997927A provides a formulation and preparation process for oryzanol nanocrystalline capsules; Chinese invention patent CN111529500A provides a pharmaceutical preparation for improving the solubility of oryzanol and its preparation method.

[0003] However, the application and research of oryzanol in the skincare industry are still relatively limited. Among the many dosage forms of skincare products, spray formulations are widely used in the market due to their convenience and low risk of contamination. However, spray formulations generally require low product viscosity, which greatly limits the formulation options. The oil content cannot usually be increased significantly, especially for poorly soluble active ingredients like oryzanol, making it difficult to meet its dissolution requirements. Furthermore, oryzanol emulsions prepared using traditional emulsification techniques have larger particle sizes, making it difficult to penetrate the stratum corneum of the skin, resulting in low bioavailability and insufficient efficacy. Summary of the Invention

[0004] To address the problems in the prior art, the first aspect of the present invention provides an ultrafine emulsified spray cream containing oryzanol, wherein, by weight percentage, the ultrafine emulsified spray cream comprises: Oryzanol 0.1-8% Emulsifier 0.1-10% Oil 10-30% Polyols 4-10% Thickener 1-10% Water to replenish the remaining amount; The critical packing parameter of the emulsifier is 0.8-1.2; the thickener includes at least one of the following: thickener GT-730, thickener Tinovis GTC UP, thickener Volarest FL, thickener Aristoflex BLV, thickener Carbomer U20, thickener Carbomer U30, and thickener Cosmedia SP.

[0005] In one embodiment, the ultrafine emulsified spray cream comprises, by weight percentage: Oryzanol 0.1-5% Emulsifier 0.1-1.5% Oil 10-20% Polyols 4-10% Thickener 1-6% Add water to make up the remaining amount.

[0006] In one embodiment, the grease includes polar grease.

[0007] In a preferred embodiment, the polar grease is a medium polar grease or a low polar grease.

[0008] In a more preferred embodiment, the polar oil comprises at least one of the following: caprylic / capric triglyceride, isopropyl myristate, ethylhexyl palmitate, C12-15 alkyl benzoate, ethylhexyl stearate, cetyl ethylhexanoate, caprylic / capric / myristic / stearic triglyceride, C10-18 fatty acid triglycerides, dioctyl carbonate, triglyceride (ethylhexanoate), isononyl isononanoate, pentaerythritol tetrastearate, pentaerythritol tetraisostearate, myristyl myristate, pentaerythritol tetra(ethylhexanoate), and hydrogenated polydecene.

[0009] In one embodiment, the emulsifier includes one or more of the following: sodium subtilisin, polyglycerol emulsifier, polyether emulsifier, and sucrose emulsifier.

[0010] In a preferred embodiment, the emulsifier has an HLB value ≥ 12.

[0011] In one embodiment, the polyglycerol emulsifier includes at least one of polyglycerol-10 stearate, polyglycerol-10 oleate, polyglycerol-10 myristate, and polyglycerol-2 oleate.

[0012] In a preferred embodiment, the polyglycerol emulsifier comprises polyglycerol-10 stearate, brand name NIKKOL Decaglyn 1-SV, from Nikko Chemical Co., Ltd.

[0013] In one embodiment, the polyether emulsifier includes at least one of octyldodecyl alcohol polyether-16, octyldodecyl alcohol polyether-20, and octyldodecyl alcohol polyether-25.

[0014] In a preferred embodiment, the polyether emulsifier includes octyldodecyl alcohol polyether-16, brand name EMLEX OD-16, from Nippon Emulsification Co., Ltd.

[0015] In one embodiment, the sucrose emulsifier includes at least one of sucrose laurate, sucrose palmitate, sucrose stearate, sucrose oleate, and sucrose decanoate.

[0016] In a preferred embodiment, the sucrose emulsifier is sucrose laurate and sucrose stearate, and the mass ratio of sucrose laurate to sucrose stearate is (0.3-0.5):(0.1-0.2).

[0017] In a preferred embodiment, the mass ratio of sucrose laurate to sucrose stearate is (0.3-0.4):(0.1-0.2).

[0018] More preferably, the mass ratio of sucrose laurate to sucrose stearate is 0.3:0.1.

[0019] In one embodiment, the polyol includes one or more of glycerol, sorbitol, and butylene glycol.

[0020] In a preferred embodiment, the polyol comprises glycerol.

[0021] In one embodiment, the raw materials for preparation further include a preservative; the preservative includes at least one selected from p-hydroxyacetophenone, 1,2-hexanediol, phenoxyethanol, octyl glycol, chlorophenoxyethanol, and sodium benzoate.

[0022] In a preferred embodiment, the preservative is hydroxyacetophenone and 1,2-hexanediol, wherein the mass ratio of hydroxyacetophenone to 1,2-hexanediol is 1:1.

[0023] In one embodiment, the preservative accounts for 0.5-5% of the raw materials. Preferably, the preservative accounts for 0.5-1.5% of the raw materials. More preferably, the preservative accounts for 1% of the raw materials.

[0024] A second aspect of the present invention provides a method for preparing an ultrafine emulsified spray cream containing oryzanol, comprising at least the following steps: S1. Heat the oil to dissolve oryzanol, forming phase A; S2. Disperse and dissolve the emulsifier in the polyol to form phase B; S3. While stirring, pour phase A into phase B, continue stirring for 10-20 minutes, then homogenize under high pressure at 4000-5000 rpm for 2-5 minutes to form phase C; S4. Disperse the thickener in water, add the preservative, and stir until homogeneous to form phase D; S5. Mix the C phase and D phase evenly, and load them into a spray pump bottle to obtain an ultrafine emulsified spray cream containing oryzanol.

[0025] In one embodiment, when the thickener is Volarest FL, sodium hydroxide is used to adjust the pH of the system to 6.5-7.0 in the S5 mixing step.

[0026] In one embodiment, the heating temperature in step S1 is 65-75°C.

[0027] In a preferred embodiment, the heating temperature in step S1 is 68-72°C; more preferably, the heating temperature in step S1 is 70°C.

[0028] In one embodiment, the stirring rate in step S3 is 800-1000 rpm.

[0029] In a preferred embodiment, the stirring rate in step S3 is 800-900 rpm; more preferably, the stirring rate in step S3 is 800 rpm.

[0030] In one embodiment, the stirring rate in step S4 is 4000-4500 rpm; preferably, the stirring rate in step S4 is 4000 rpm.

[0031] Beneficial effects 1. This application uses a specific blend of emulsifiers, polar oils and thickeners, which greatly improves the solubility of oryzanol in oils and avoids problems such as layering and precipitation in the system, thus ensuring the stability and uniformity of the system.

[0032] 2. This application uses a specific blend of emulsifiers, polar oils and thickeners to maintain the system viscosity at 9000-14000cps, achieving smooth spraying and meeting the needs of cosmetic applications.

[0033] 3. The preparation method of the ultrafine emulsified spray cream provided in this application results in the particle size of the active ingredient oryzanol being between 100-600nm, which allows oryzanol in emulsified products to better penetrate the skin and exert its effects.

[0034] 4. The ultrafine emulsified spray cream containing oryzanol provided in this application and its preparation method can effectively solve the application problem of oryzanol in spray formulations, making its application in spray formulations possible and expanding the application scope of oryzanol in the field of skin care products. Attached Figure Description

[0035] Fig. 1 The images show the appearance of the products prepared in Examples 1-8.

[0036] Fig. 2 Appearance images of the products prepared for comparative examples 1-7.

[0037] Fig. 3 Appearance of the product prepared for comparative examples 8-14. Detailed Implementation

[0038] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to embodiments and accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. Experimental methods not specifying specific conditions in the embodiments were performed under conventional conditions or conditions recommended by the manufacturer. Reagents not specifying manufacturers are all commercially available conventional products.

[0039] The raw material information used in each embodiment and comparative example is as follows: Polyglycerol-10 stearate, brand name NIKKOL Decaglyn 1-SV, is from Nikko Chemical Co., Ltd.

[0040] Stearyl alcohol polyether-21, model SP BRIJ S721 MBAL-PA-(SG), is from CRODA.

[0041] Stearyl alcohol polyether-2, model number BRIJTM S2-PA-(SG), is from CRODA.

[0042] Polysorbate-60, model number Tween 60, is from CRODA.

[0043] Polyglycerol-3-methylglucose distearate, model TEGO Care 450, is from Evonik in Germany.

[0044] PEG-20 glyceryl isostearate, model number M-FINE OIL ISG-20M, is from Miyoshi Oils Co., Ltd. of Japan.

[0045] Example 1 The first aspect of this example provides an ultra-fine emulsified spray cream containing oryzanol, which, by weight percentage, comprises: 1% oryzanol Emulsifier 0.4% 15% oil 4% polyols Thickener 6% 1% preservative Water to replenish the remaining amount; The thickener is GT-730, sourced from Adico (Shanghai) Trading Co., Ltd.

[0046] The oil is caprylic / capric triglyceride.

[0047] The emulsifier is sucrose laurate.

[0048] The polyol is glycerol.

[0049] The preservative is p-hydroxyacetophenone and 1,2-hexanediol, and the mass ratio of p-hydroxyacetophenone to 1,2-hexanediol is 1:1.

[0050] The second aspect of this example provides a method for preparing an ultrafine emulsified spray cream containing oryzanol, comprising the following steps: S1. Heat the oil to 70℃ to dissolve oryzanol, forming phase A; S2. Disperse and dissolve the emulsifier in the polyol to form phase B; S3. While stirring at 800 rpm, pour phase A into phase B, continue stirring for 10 minutes, and then homogenize under high pressure at 4000 rpm for 3 minutes to form phase C. S4. Disperse the thickener in water, add the preservative, and stir until homogeneous to form phase D; S5. Mix the C phase and D phase evenly, and load them into a spray pump bottle to obtain an ultrafine emulsified spray cream containing oryzanol.

[0051] Example 2 The specific implementation method in this example is the same as in Example 1, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol Emulsifier 0.4% 15% oil 4% polyols Thickener 1.5% 1% preservative Water to replenish the remaining amount; The thickener is Tinovis GTC UP, which is from BASF.

[0052] Example 3 The specific implementation method in this example is the same as in Example 1, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol Emulsifier 0.4% 15% oil 4% polyols Thickener 1.5% 1% preservative Water to replenish the remaining amount; The thickener is Volalest FL, sourced from CRODA.

[0053] In the S5 mixing step, sodium hydroxide is used to adjust the pH of the system to 6.5-7.0.

[0054] Example 4 The specific implementation method in this example is the same as in Example 1, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol Emulsifier 0.15% 15% oil 4% polyols Thickener 6% 1% preservative Add water to make up the remaining amount.

[0055] The emulsifier is sodium subtilisin.

[0056] Example 5 The specific implementation method in this example is the same as in Example 2, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol Emulsifier 0.15% 15% oil 4% polyols Thickener 1.5% 1% preservative Water to replenish the remaining amount; The emulsifier is sodium subtilisin.

[0057] Example 6 The specific implementation method in this example is the same as in Example 3, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol Emulsifier 0.4% 15% oil 4% polyols Thickener 1.5% 1% preservative Water to replenish the remaining amount; The emulsifier is sodium subtilisin.

[0058] Example 7 The specific implementation method in this example is the same as in Example 2, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol Emulsifier 0.4% 15% oil 4% polyols Thickener 1.5% 1% preservative Water to replenish the remaining amount; The emulsifier is polyglycerol-10 stearate.

[0059] Example 8 The specific implementation method in this example is the same as in Example 2, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol Emulsifier 0.4% 15% oil 4% polyols Thickener 1.5% 1% preservative Water to replenish the remaining amount; The emulsifier is sucrose laurate and sucrose stearate, and the mass ratio of sucrose laurate to sucrose stearate is 0.3:0.1.

[0060] Comparative Example 1 The specific implementation method in this example is the same as in Example 7, except that the emulsifier is glyceryl stearate.

[0061] Comparative Example 2 The specific implementation method in this example is the same as in Example 1, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol 1% emulsifier 15% oil 4% polyols Thickener 6% 1% preservative Water to replenish the remaining amount; The emulsifier is glyceryl stearate.

[0062] Comparative Example 3 The specific implementation method in this example is the same as in Example 3, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol 1% emulsifier 15% oil 4% polyols Thickener 1.5% 1% preservative Water to replenish the remaining amount; The emulsifier is glyceryl stearate.

[0063] Comparative Example 4 The specific implementation method of this example is the same as that of Example 7, except that the emulsifier is stearyl alcohol polyether-21.

[0064] Comparative Example 5 The specific implementation method in this example is the same as in Example 8, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol Emulsifier 1.4% 15% oil 4% polyols Thickener 1.5% 1% preservative Water to replenish the remaining amount; The emulsifiers are stearyl alcohol polyether-2 and stearyl alcohol polyether-21, and the mass ratio of stearyl alcohol polyether-2 to stearyl alcohol polyether-21 is 0.4:1.

[0065] Comparative Example 6 The specific implementation method in this example is the same as in Example 7, except that the emulsifier is polysorbate-60.

[0066] Comparative Example 7 The specific implementation method of this example is the same as that of Example 7, except that the emulsifier is C14-22 alcohol / C12-20 alkyl glucoside.

[0067] Comparative Example 8 The specific implementation method in this example is the same as in Example 7, except that the emulsifier is arachidonic acid / behenol / arachidonic acid glucoside.

[0068] Comparative Example 9 The specific implementation method in this example is the same as in Example 7, except that the emulsifier is polyglycerol-3-methylglucose distearate.

[0069] Comparative Example 10 The specific implementation method of this example is the same as that of Example 7, except that the emulsifier is PEG-20 glyceryl isostearate.

[0070] Comparative Example 11 The specific implementation method in this example is the same as in Example 8, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol Emulsifier 0.5% 15% oil 4% polyols Thickener 1% 1% preservative Water to replenish the remaining amount; The emulsifier is sucrose laurate and sucrose stearate, and the mass ratio of sucrose laurate to sucrose stearate is 0.4:0.1.

[0071] The thickener is Carbomer 940.

[0072] Comparative Example 12 The specific implementation method in this example is the same as that in Comparative Example 11, except that the thickener is Carbomer 980.

[0073] Comparative Example 13 The specific implementation method in this example is the same as that in Comparative Example 11, except that the thickener is Carbomer U10.

[0074] Comparative Example 14 The specific implementation method in this example is the same as that in Comparative Example 11, except that, by weight percentage, the ultrafine emulsified spray cream comprises: 1% oryzanol Emulsifier 0.5% 15% oil 4% polyols Thickener 0.8% 1% preservative Water to replenish the remaining amount; The thickener is gellan gum and sodium chloride, and the mass ratio of gellan gum to sodium chloride is 0.5:0.3.

[0075] Performance testing 1. Observe whether the samples prepared in Examples 1-8 and Comparative Examples 1-14 form a homogeneous phase. Simultaneously, perform viscosity tests on the samples prepared in Examples 1-8 and Comparative Examples 11-14. The results are as follows: Figs. 1-3 As shown in Table 1.

[0076] 2. Spray comparison tests were conducted on the samples prepared in Examples 1-8 and Comparative Examples 11-14 using ordinary water-based spray bottles found in cosmetics. The test results are shown in Table 1; √ in the table represents that a spray can be formed, and × represents that a spray cannot be formed.

[0077] Table 1

[0078] As can be seen from Table 1 and the figures, the products prepared in Examples 1-8 of this application all exhibited a uniform appearance without any layering. In contrast, the products in Comparative Examples 1-10 showed more obvious layering and could not form a uniform phase, so viscosity tests were not performed. Although Comparative Examples 11-14 also exhibited a uniform appearance like the examples, their viscosity was higher and they could not form a spray.

Claims

1. An ultrafine emulsified spray cream containing oryzanol, characterized by, The superfine emulsified spray cream comprises, by weight percentage: Oat fiber 0.1-8% Emulsifier 0.1-10% Oil 10-30% Polyol 4-10% Thickening agent 1-10% Water makes up the balance. The critical packing parameter of the emulsifier is 0.8-1.2; the thickening agent comprises at least one of thickening agent GT-730, thickening agent Tinovis GTC UP, thickening agent Volarest FL, thickening agent Aristoflex BLV, thickening agent Carbomer U20, thickening agent Carbomer U30, and thickening agent Cosmedia SP.

2. The oryzanol-containing ultrafine emulsified spray cream according to claim 1, characterized by, The superfine emulsified spray cream comprises, by weight percentage: Oat fiber 0.1-5% Emulsifier 0.1-1.5% Oil 10-20% Polyol 4-10% Thickening agent 1-6% Water makes up the balance.

3. The oryzanol-containing microemulsified spray cream of claim 1, wherein, The oil comprises polar oil.

4. The oryzanol-containing microemulsified spray cream of claim 3, wherein, The polar oil comprises at least one of caprylic / capric triglyceride, isopropyl myristate, ethylhexyl palmitate, C12-15 alkyl benzoate, ethylhexyl stearate, cetyl ethylhexanoate, caprylic / capric / myristic / stearic triglyceride, C10-18 fatty acid triglyceride, dicaprylyl carbonate, glyceryl triethylhexanoate, isononyl isononanoate, pentaerythrityl tetra(stearate), pentaerythrityl tetraisostearate, myristyl myristate, pentaerythrityl tetra(ethylhexanoate), hydrogenated polydecene.

5. The oryzanol-containing microemulsified spray cream of claim 1, wherein, The emulsifier comprises one or more of sodium mycobacterial lipopeptide, polyglycerol emulsifier, polyether emulsifier, sucrose emulsifier.

6. The oryzanol-containing microemulsified spray cream of claim 5, wherein, The HLB value of the emulsifier is ≥12.

7. The oryzanol-containing microemulsified spray cream of claim 6, wherein, The sucrose emulsifier comprises at least one of sucrose laurate and sucrose stearate.

8. The oryzanol-containing microemulsified spray cream of claim 1, wherein, The polyol comprises one or more of glycerol, sorbitol, and butanediol.

9. The oryzanol-containing microemulsified spray cream of claim 1, wherein, The preparation raw material further comprises a preservative; the preservative comprises at least one of para-hydroxyacetophenone and 1,2-hexanediol.

10. A process for the preparation of an ultrafine emulsified spray cream containing oryzanol according to any one of claims 1 to 9, characterized in that, At least comprising the following steps: S1, heating and dissolving the oil to dissolve the oat fiber to form a phase A; S2, dispersing and dissolving the emulsifier in the polyol to form a phase B; S3, pouring the phase A into the phase B under stirring, continuously stirring for 10-20 min, and then high-pressure homogenizing at 4000-5000 rpm for 2-5 min to form a phase C; S4, dispersing the thickening agent in water, adding the preservative, and stirring uniformly to form a phase D; S5, mixing the phase C and the phase D uniformly, filling into a spray pump bottle, and obtaining the superfine emulsified spray cream containing oat fiber.

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