An oily gel microbead, a preparation method thereof, a skin care product and application thereof

Abstract

The application discloses oily gel microbeads, a preparation method thereof, skin care products and application. The oily gel microbeads comprise polar oil 60-93%, oil phase gel 5-30%, low freezing point oil 2.5-20% and semi-solid oil 0.1-5%, % is the mass percentage of each component in the total mass of the gel microbeads; the polar oil is one or more of glyceryl tri(ethylhexanoate), white pool seed oil, isononyl isononanoate, dicaprylyl carbonate, diethylhexyl carbonate, C12-15 alcohol benzoate, isopropyl myristate, ethylhexyl stearate, ethylhexyl palmitate, castor seed oil, wheat germ oil, sunflower seed oil, wild soybean oil and coconut oil; the freezing point of the low freezing point oil is lower than-65 DEG C. The oily gel microbeads prepared by the application have good low-temperature stability, are spherical in shape, have good uniformity, are easy to spread and absorb, have strong skin adhesion, and have strong moisturizing and repairing functions.

Description

Technical Field

[0001] This invention discloses an oily gel microbead, its preparation method, skin care products, and applications. Background Technology

[0002] As the cosmetics industry has evolved, product varieties have become increasingly diverse. With technological advancements, consumers are not only pursuing the efficacy of cosmetics but also favoring products with unique and attractive designs. Currently, cosmetics containing microbeads are becoming more common. The gel particles added to commercially available cosmetics are primarily water-based gel particles or shelled gel microspheres, prepared from water-soluble polymers such as alginate, agar, and carrageenan (water-based gel beads) using a pelletizing process. While these particles can alter the visual effect of cosmetics, they leave a sticky feeling on the skin after application, require a special pump head to break the gel beads, and are difficult to spread evenly on the skin. Oil-based microbeads, on the other hand, are not commonly found in the market due to their complex preparation methods, poor particle size uniformity, and instability.

[0003] Microfluidics technology primarily achieves precise control of fluids by designing, fabricating, and manipulating various microchannel systems. Microfluidics includes three important branches: digital microfluidics, droplet microfluidics, and traditional microfluidics. Droplet microfluidics is a technique that controls the formation of monodisperse droplets by shearing immiscible multiphase fluids within microscale channels. Simply put, it involves allowing an oil phase to flow along a microchannel while an external aqueous phase flows through the outlet of the microchannel. This rapidly shears the oil phase exiting the microchannel, dispersing it into the external aqueous phase and forming tiny droplets.

[0004] Most existing technologies use micro-injection pumps to power the oil phase and the external aqueous phase, allowing them to converge at a relatively constant rate. When preparing microdroplets using this method, in order to ensure that the oil phase can be well dispersed into the external aqueous phase to form microdroplets, rather than forming a parallel stratified fluid with the external aqueous phase, the flow rate of the oil phase needs to be restricted to an extremely slow speed, resulting in low throughput and slow preparation rate. Summary of the Invention

[0005] The technical problem solved by this invention is to overcome the shortcomings of existing technologies, such as the sticky feel of existing gel particles after being added to skin care products, the need for a special pump head to break the gel beads, and the difficulty in evenly spreading the broken particles on the skin. This invention provides an oil-based gel microbead, its preparation method, skin care products, and applications. The oil-based gel microbeads prepared by this invention have good low-temperature stability, a regular spherical shape, moderate uniformity and hardness, are easy to spread evenly, are easily absorbed, have strong skin adhesion, and can melt upon contact with the skin without requiring a special pump head to break them. They also have strong moisturizing and repairing functions.

[0006] The present invention solves the above-mentioned technical problems through the following technical solutions:

[0007] This invention provides an oily gel microsphere comprising 60-93% polar oil, 5-30% oil phase gelling agent, 2.5-20% low pour point oil and 0.1-5% semi-solid oil, where % represents the percentage of each component by mass relative to the total mass of the gel microsphere.

[0008] The polar oil is one or more of the following: triglyceride (ethylhexanoate), meadowfoam seed oil, isononyl isononanoate, dioctyl carbonate, diethylhexyl carbonate, C12-15 alcohol benzoate, isopropyl myristate, ethylhexyl stearate, ethylhexyl palmitate, castor seed oil, wheat germ oil, sunflower seed oil, wild soybean oil, and coconut oil.

[0009] The low-freezing-point oil has a freezing point below -65°C.

[0010] In this invention, the inorganic-organic balance value (IOB value) of the polar oil can be 0.10-0.40, for example 0.12, 0.13, 0.16, 0.17, 0.18, 0.2, 0.23, 0.35 or 0.43.

[0011] In this invention, the polar oil is preferably triglyceride (ethylhexanoate) and / or meadowfoam seed oil.

[0012] In this invention, the amount of the polar oil is preferably 70-90%, more preferably 75-90%, for example 77.4%, 77.7%, 78.4%, 80.7%, 81%, 82.7%, 85.7%, 88.4% or 88.5%.

[0013] In this invention, the polar oil is preferably 70-90% triglyceride (ethylhexanoate) and 0.1-5% meadowfoam seed oil.

[0014] The amount of the glycerol tri(ethylhexanoate) ester is preferably 72-89%, for example 74.2%, 74.4%, 78.5%, 78.7%, 81.2%, 84.7%, 87.9% or 88%.

[0015] The preferred amount of meadowfoam seed oil used is 0.2-4%, for example, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5% or 4%.

[0016] In this invention, the oil phase gelling agent generally refers to a substance that thickens the oil phase, allowing the oil to form a gel.

[0017] In this invention, the oil phase gelling agent may be one or more of castor oil / IPDI copolymer, dextrin palmitate, dextrin myristate ester and HDI / trimethylolhexyl lactone crosspolymer, such as castor oil / IPDI copolymer.

[0018] The melting temperature of the castor oil / IPDI copolymer can be 80℃-110℃, preferably 95-100℃, for example 100℃.

[0019] In this invention, the amount of the oil phase gelling agent is preferably 5-20%, more preferably 6-18%, for example 7.5%, 8.0%, 8.5%, 9.5%, 11%, 12%, 13%, 14% or 15%.

[0020] In this invention, the freezing point of the low-freezing-point oil is preferably below -70°C, for example -80°C.

[0021] In this invention, the low pour point oil is preferably one or more of C13-16 isoparaffins, triheptane, diisooctyl succinate, and neopentyl glycol diheptyl ester, for example, C13-16 isoparaffins.

[0022] In this invention, the amount of the low-freezing-point oil can be 3-10%, for example 3%, 4%, 5%, 6%, 7% or 8%.

[0023] In this invention, the semi-solid grease generally refers to grease that is in a semi-solid or solidified state at room temperature (e.g., 25±5℃).

[0024] In this invention, the semi-solid oil is preferably one or more of bis-diglyceride polyacryladiate-2, shea butter, hydrogenated coconut oil glycerides, and C10-18 triglycerides, such as bis-diglyceride polyacryladiate-2 or shea butter.

[0025] In this invention, the amount of the semi-solid oil used is preferably 0.2-2%, for example 0.5% or 1%.

[0026] In this invention, the oily gel microbeads may also include functional additives.

[0027] The functional additives are preferably one or more of the following: antioxidant active ingredients, fragrance ingredients, whitening active ingredients, anti-aging active ingredients, and soothing active ingredients.

[0028] The functional additive is preferably 0.1-20% by mass, more preferably 0.2-5%, for example 0.5%, 0.6%, 0.8%, 1.1%, 1.3%, 1.5% or 1.8%.

[0029] The fragrance raw materials may be fragrances and / or essential oils.

[0030] When the functional additive includes a fragrance ingredient, the amount of the fragrance ingredient used is preferably 0.01-1%, more preferably 0.1-0.5%, for example 0.2%, 0.3% or 0.5%.

[0031] The antioxidant active ingredients may be flavonoid antioxidant active ingredients (e.g., silymarin, astragaloside, rutin, quercetin, cinnamyl glycoside, dihydrocinnamyl glycoside, mangiferin), tannin antioxidant active ingredients (e.g., epigallocatechin, epigallocatechin gallate, epicatechin gallate, catechin), quinone antioxidant active ingredients (e.g., shikonin), dipeptide amino acids (e.g., methionine, tryptophan, phenylalanine, proline), sugar alcohol antioxidant active ingredients (e.g., pentose, hexose monosaccharides, lily polysaccharides, fructose, sugar alcohols), and polyphenol antioxidant active ingredients. One or more of the following: (e.g., tocopheryl acetate, BHT (2,6-di-tert-butyl-4-methylphenol), cereal germ, grapeol, rosmarinicol, epirosmarinicol, isorrosmarinicol), alkaloid antioxidant active ingredients (e.g., ligustrazine, purslane, magnolol, papaverine, lysimachia foenum-graecum), vitamin antioxidant active ingredients (e.g., vitamin E, vitamin C, carotenoids), and plant extract antioxidant active ingredients (e.g., antioxidant active ingredients from *Alternaria solani* extract), preferably polyphenolic antioxidant active ingredients, such as tocopheryl acetate.

[0032] The antioxidant active ingredient is preferably present in a mass percentage of 0.3-0.8%, more preferably 0.3-0.7%, for example 0.5%.

[0033] The whitening active ingredient may be conventional in the art, and preferably one or more of arbutin and its derivatives, kojic acid and its derivatives, azelaic acid and its derivatives, linoleic acid and its derivatives, vitamin C and its derivatives, fruit acids and niacinamide and their derivatives.

[0034] The amount of the whitening active ingredient is preferably 0.3-0.8%, for example 0.5%.

[0035] The anti-aging active ingredient may be conventional in the art, and preferably one or more of the following: vitamin-based anti-aging active ingredients (e.g., vitamin A or vitamin B), peroxidases (e.g., superoxide dismutase (SOD), glutathione peroxidase (GPO), or catalase), and plant extracts (e.g., capernaum bud extract or sage extract).

[0036] The amount of the anti-aging active ingredient is preferably 0.3-0.8%, for example 0.5%.

[0037] The soothing active ingredient may be conventional in the art, and preferably one or more of dipotassium glycyrrhizate, allantoin, and biosaccharide gum-2.

[0038] The amount of the soothing active ingredient is preferably 0.3-0.8%, for example 0.5%.

[0039] In this invention, the oily gel microbeads are pure oil beads and do not contain water.

[0040] In this invention, the particle size of the oily gel microspheres can be 0.1-4 mm, preferably 0.5-3 mm.

[0041] The present invention also provides a method for preparing the oily gel microspheres, which includes the following steps:

[0042] (1) Preparation of oil phase: The low pour point oil and the semi-solid oil are added to a mixture formed by the polar oil and the oil phase gelling agent to obtain the oil phase;

[0043] (2) Preparation of aqueous phase:

[0044] The aqueous phase is prepared by uniformly mixing 95-99.9% water and 0.01-5% thickener, where % represents the mass percentage of each component in the aqueous phase.

[0045] (3) Method 1: The oily gel microspheres are prepared by using the oil phase and the aqueous phase through a microfluidic device;

[0046] Alternatively, method two: mix the oil phase and the aqueous phase to obtain the oily gel microbeads.

[0047] In step (1), there are no special requirements for the order in which the low-freezing-point oil and the semi-solid oil are added.

[0048] In step (1), when the oily gel microspheres also include the functional additive, it is preferable to add the low-pour-point oil, the semi-solid oil and the functional additive together to the mixture formed by the polar oil and the oil phase gelling agent.

[0049] In step (1), the preferred method for preparing the mixture formed by the polar oil and the oil phase gelling agent is to heat the polar oil and the oil phase gelling agent and then homogenize them.

[0050] The heating is generally carried out under stirring conditions. The stirring speed can be 100-500 rpm / min, for example, 300 rpm / min.

[0051] The heating temperature can be 100-105℃, for example 102℃.

[0052] The homogenization time can be 10-30 minutes, for example, 15 minutes.

[0053] The rotational speed of the homogenizer can be 4000-8000 rpm / min, for example, 6000 rpm / min.

[0054] After homogenization, the temperature generally needs to be lowered to 80-85℃, for example, 82℃.

[0055] In step (2), the water can be conventional in the art, generally deionized water.

[0056] In step (2), the amount of water used can be 99-99.9%, for example 99.3%, 99.31985% or 99.32%.

[0057] In step (2), the thickener may be one or more of carbomer, xanthan gum, polyacrylic acid, acrylate / C10-30 alkanol acrylate crosspolymer and acrylate / vinyl isodecanoate crosspolymer, such as acrylate / C10-30 alkanol acrylate crosspolymer or acrylate / vinyl isodecanoate crosspolymer.

[0058] In step (2), the amount of the thickener is preferably 0.01 to 0.8%, for example 0.08% or 0.1%.

[0059] In step (2), the order in which the deionized water, the thickener, and the preservative are added can be arbitrary.

[0060] The order of steps (1) and (2) can be arbitrary.

[0061] In step (2), the aqueous phase may also include one or more of preservatives, colorants and humectants.

[0062] The preservative may be conventional in the art, such as phenoxyethanol.

[0063] The amount of the preservative can be 0.1-1%, preferably 0.3-0.8%, for example 0.5%, 0.6%, 0.65% or 0.665%.

[0064] The colorant may be conventional in the art, such as CI 14700.

[0065] The amount of the colorant can be 0.00001-0.0005%, for example, 0.00015%.

[0066] The humectant may be one or more of glycerin, butylene glycol, 1,3-propanediol, pentanediol, and caprylyl glycol.

[0067] The amount of the humectant used can be 0.1-1%.

[0068] In step (2), when the aqueous phase includes a preservative, the deionized water, the thickener, and the preservative can be added together.

[0069] In step (2), when the aqueous phase includes a colorant, the deionized water, the thickener, the preservative and the colorant can be added together.

[0070] In step (2), the viscosity of the aqueous phase can be 20-40 CP, for example 20 CP or 38 CP.

[0071] In Method 1, the mass ratio of the oil phase to the aqueous phase can be 1:(0.5-5.5), for example, 1:0.5, 1:1, 1:2, 1:3, 1:4.5, or 1:5.5, preferably 1:(1-5). Excessive oil phase makes the prepared oily gel microspheres difficult to disperse and easily leads to the formation of irregularly shaped microspheres; excessive aqueous phase results in high energy consumption during stirring, a low final throughput, and the formation of tiny microspheres.

[0072] In Method 1, the channel of the microfluidic device can be a T-shaped channel, a Y-shaped channel, a cross-shaped channel, or a 3D coaxial channel, preferably a T-shaped channel.

[0073] The principle of the Y-shaped channel is that the mixture appears at the contact surface between two fluids and mainly relies on the diffusion process that occurs at the interface, which easily forms laminar flow.

[0074] The principle of the cross-shaped channel is that three flow paths converge in one pipe, the dispersed phase and the mobile phase meet at the cross-shaped pipe, and the symmetrical flow paths simultaneously compress the dispersed phase to break it up, thereby forming droplets.

[0075] The 3D coaxial droplet channel is formed by two nested conical capillaries, creating a coaxial structure. The internal phase fluid is surrounded by the external phase fluid, and the flow rates of the internal and external phase fluids can be adjusted.

[0076] The T-shaped channel has a relatively simple structure, is not prone to laminar flow, and has an adjustable manufacturing throughput.

[0077] The inner diameter of the T-shaped channel can be 0.5-2.5mm, preferably 0.5-1.6mm, more preferably 0.5-1.0mm, for example 0.72mm.

[0078] The T-channel can be a T-channel micro single channel or a T-channel micro multi channel.

[0079] When the T-channel is a T-channel micro single channel, the feed rate of the oil phase can be 15-50 mL / min.

[0080] When the T-channel is a T-channel micro-multichannel, the feed rate of the oil phase can be 30-3000 mL / min.

[0081] In Method 1, preferably, when the channel of the microfluidic device is a T-shaped channel, the oil phase enters from the vertical inlet of the T-shaped channel, the outlet of the oil phase inlet channel is connected to the water, and the outlet end face of the oil phase channel is perpendicular to the surface of the water phase, so as to ensure that the material of the oil phase is simultaneously and vertically cut off and encapsulated by the water phase at the moment it flows out of the inlet channel.

[0082] The temperature at which the oil phase enters the vertical inlet can be between 70-100°C, preferably between 80-85°C, for example 82°C.

[0083] The temperature of the aqueous phase entering the main channel can be 10-40℃ or 75℃-85℃, for example, 20℃, 30℃ or 80℃. When the aqueous phase closed container is under negative pressure, the temperature of the aqueous phase entering the main channel is preferably 75℃-85℃, for example, 80℃.

[0084] When the oil phase flows out from the outlet of the flow channel, a peristaltic pump or vacuum can be used to power the oil phase. The rotation speed of the peristaltic pump can be 50-300 rpm / min, preferably 60-160 rpm / min, for example 80 rpm / min or 100 rpm / min. After vacuuming, the pressure in the sealed container of the aqueous phase can be -(0.03-0.1) MPa, for example -0.08 MPa. This invention uses a peristaltic pump and / or vacuum pressure to power the oil phase, allowing the oil and aqueous phases to merge at a basically constant rate to form, thereby improving the throughput and preparation rate of microfluidic beads.

[0085] When a peristaltic pump is used to power the oil phase, a vibrator is generally required at the outlet of the oil phase flow channel. The vibration frequency of the vibrator can be 1-100 Hz, for example, 50 Hz.

[0086] In Method 1, the stirring speed of the aqueous phase can be 120-800 rpm / min (e.g., 260 rpm / min or 550 rpm / min) or 30-75 Hz (e.g., 65 Hz).

[0087] In Method 1, after obtaining the oily gel microbeads, a pH adjuster (such as aminomethylpropanol) can generally be added to the system to make the oily gel microbeads more uniformly dispersed.

[0088] In Method 2, the mass ratio of the oil phase to the water phase can be 1:(0.5-5.5), for example, 1:1.

[0089] In Method 2, before mixing, preferably, the oil phase and the water phase are heated to 80-85°C, for example, 82°C.

[0090] In Method 2, preferably, the oil phase is added to the aqueous phase.

[0091] In Method 2, the mixing method can be conventional in the art, such as stirring. The stirring speed can be 100-500 rpm / min, preferably 150-300 rpm / min, for example 180 rpm / min.

[0092] In Method 2, preferably, the aqueous phase and the oil phase are heated to 80-85°C respectively, and then the oil phase is added to the stirred aqueous phase and stirred until room temperature is reached.

[0093] In Method 1, the oily gel microspheres are prepared by a microfluidic device, which allows the oil phase to diffuse rapidly and uniformly into the aqueous phase to form microfluidic microspheres. This effectively avoids the formation of parallel stratified fluids between the oil phase and the aqueous phase when the oil phase flows rapidly, breaks the flow rate limitation of the oil phase, and improves the throughput and preparation rate of liposome microfluidic microspheres.

[0094] The present invention also provides a skin care product comprising the oily gel microbeads as described above.

[0095] In this invention, the types of skin care products can be conventional in the art, such as serums, gels, creams, or masks.

[0096] In this invention, the oily gel microbeads account for 10-35% of the mass of the skin care product, for example, 11%.

[0097] In this invention, the viscosity of the skin care product can be 5000-15000 mPa.s, preferably 6000-8000 mPa.s, for example 7000 mPa.s.

[0098] The present invention also provides an application of the oily gel microbeads in skin care products.

[0099] Based on common knowledge in the field, the above-mentioned preferred conditions can be combined arbitrarily to obtain various preferred embodiments of the present invention.

[0100] The reagents and raw materials used in this invention are all commercially available.

[0101] The positive and progressive effects of this invention are as follows:

[0102] (1) The oily gel microbeads prepared by this invention have good low-temperature stability, moderate uniformity and hardness, are easy to apply evenly, are easy to absorb, have strong skin adhesion, and can melt on the skin surface without the need for a special pump head to break them up.

[0103] (2) The oily gel microbeads prepared by the present invention have a novel appearance (the shape is a regular spherical shape), are visible, crystal clear, and greatly improve the sensory experience when using the product.

[0104] (3) The oily gel microbeads prepared by the present invention have a good skin feel, can better stabilize active ingredients, and provide long-lasting protection for the skin;

[0105] (4) The gel microbeads prepared by the present invention are mild and have good film-forming properties. When added to skin care products, the change in skin moisture content and transepidermal water loss are far superior to ordinary products due to their good film-forming properties. They have strong moisturizing and repairing properties. Attached Figure Description

[0106] Figure 1 Image of a peristaltic pump; Figure 1 Image 'a' is of a single-channel peristaltic pump; Figure 1 Image b is of a multi-channel peristaltic pump.

[0107] Figure 2 This is a diagram of an upright single-microchannel needle.

[0108] Figure 3 Image of the oily gel microbeads prepared in Example 3.

[0109] Figure 4 The image shows the oily gel microbeads prepared in Example 4.

[0110] Figure 5 Image of the oily gel microbeads prepared in Example 5.

[0111] Figure 6 The image shows the oily gel microspheres prepared in Example 5 after low-temperature testing.

[0112] Figure 7 The image shows the oily gel microbeads prepared for Comparative Example 1 after low-temperature testing.

[0113] Figure 8 The image shows the oily gel microspheres prepared in Comparative Example 2 after low-temperature testing. Detailed Implementation

[0114] The present invention is further illustrated below by way of embodiments, but the invention is not limited to the scope of the embodiments described herein. Experimental methods in the following embodiments that do not specify specific conditions were performed according to conventional methods and conditions, or as selected according to the product instructions.

[0115] Information on the raw materials and equipment used in Examples 1-13 and Comparative Examples 1-3 is shown in Table 1:

[0116] Table 1

[0117]

[0118]

[0119] The melt temperature of the castor oil / IPDI copolymer is 100°C. The density of the triglyceride (ethylhexanoate) is 0.95-1.0 g / cm³. 3 The viscosity is 50-200 mPa·s (25℃), and the IOB value is 0.35; the freezing point of C13-16 isoparaffins is -80℃, and the relative density is 0.77 G / CM3; the IOB value of meadowfoam seed oil is 0.16; the freezing point of caprylic / capric triglyceride is -65℃, and the IOB value is 0.3.

[0120] Example 1

[0121] Oil phase formulation A1: by weight,

[0122] Polar oils: 88 parts triglyceride (ethylhexanoate), 0.5 parts meadowfoam seed oil;

[0123] Oil phase gelling agent: 7.5 parts castor oil / IPDI copolymer;

[0124] Low pour point fats: 3 parts C13-16 isoparaffins;

[0125] Semi-solid fats: 0.5 parts bis-diglyceride polyacryl adipate-2;

[0126] Additives: 0.3 parts tocopheryl acetate and 0.2 parts fragrance;

[0127] Aqueous phase formulation C3: by weight,

[0128] 99.31985 portions of deionized water;

[0129] Thickener: 0.08 parts of acrylate / C10-30 alkanol acrylate crosspolymer;

[0130] Preservative: 0.6 parts phenoxyethanol;

[0131] Colorant: 0.00015 parts, CI 14700;

[0132] The viscosity of the aqueous phase is 20 CP.

[0133] The process steps are as follows:

[0134] Preparation of the oil phase:

[0135] (1) At room temperature, the polar oil and oil phase gelling agent in the oil phase are heated to 102°C with stirring at a stirring speed of 300 rpm / min and mixed evenly to obtain a dispersion.

[0136] (2) The above dispersion was homogenized at 102℃ for 15 min at a speed of 6000 rpm / min.

[0137] (3) After cooling the homogenized dispersion to 82°C, add the low-pour-point oil, semi-solid oil and additives from the oil phase in sequence, mix them evenly, and obtain the oil phase.

[0138] Preparation of the aqueous phase:

[0139] At room temperature, deionized water, thickener, preservative and colorant in the aqueous phase are mixed evenly to obtain the aqueous phase.

[0140] Preparation of gel microbeads (active microfluidics):

[0141] The temperature of the oil phase was controlled at 82℃, and the temperature of the aqueous phase was controlled at 30℃. Figure 1 The microfluidic device shown (using a T-shaped channel with a diameter of 0.72 mm) controls the stirring speed of the aqueous phase at 260 rpm / min, the rotation speed of the peristaltic pump in the oil phase at 80 rpm / min, and the mass ratio of the oil phase to the aqueous phase at 1:1. The oil phase enters the aqueous phase through the vertical inlet of the channel in the T-shaped structure. The outlet of the oil phase inlet channel is connected to the water and is inserted into the aqueous phase to a depth of about 0.3-1 cm. The vibration frequency of the vibrator at the oil phase outlet is 50 Hz. The outlet end face of the oil phase channel is perpendicular to the water phase channel, so that the oil phase flows uniformly into the water phase moving at a constant speed. The oil phase material is simultaneously and vertically cut off and encapsulated by the water phase at the moment it flows out of the inlet channel. After cooling and solidification, pure oily gel microbeads are prepared.

[0142] Finally, add the pH adjuster (aminomethylpropanol), stir until homogeneous, and the prepared oily gel microbeads are uniformly dispersed in the dispersion formed by the aqueous phase.

[0143] Examples 2-5, Examples 7-11 and Comparative Examples 2-3

[0144] Except for the formula and process in Table 2-4, all other operations and conditions are the same as in Example 1.

[0145] Example 6

[0146] Except for adopting the formulation and process in Table 2-4, and in the preparation of gel microspheres, except adjusting the speed of the oil phase peristaltic pump from 80 rpm / min to control the pressure in the closed container of the aqueous phase to -0.08 MPa and controlling the temperature of the aqueous phase at 80°C, all other operations and conditions are the same as in Example 1.

[0147] Example 12

[0148] Using the formulations in Tables 2-4, aqueous and oil phases were prepared according to Example 1, and oily gel microspheres were prepared according to the following preparation method:

[0149] The aqueous phase and oil phase were heated to 82°C respectively. Then the oil phase was added to the stirred aqueous phase and stirred until room temperature was reached. The stirring speed was 180 rpm / min.

[0150] Comparative Example 1

[0151] Except for the formulation and process in Table 2-4, all other operations and conditions are the same as in Example 1; in this comparative example, the timing of the addition of caprylic / capric triglyceride is the same as that of triglyceride (ethylhexanoate) in Example 1.

[0152] Figure 1 Image of a peristaltic pump; Figure 1 Image 'a' is of a single-channel peristaltic pump; Figure 1 Image b is of a multi-channel peristaltic pump. Figure 2 This is a diagram of an upright single-microchannel needle.

[0153] Table 2. Process conditions for Examples 1-12 and Comparative Examples 1-3

[0154]

[0155]

[0156] Note: In Examples 1-5, Examples 7-12 and Comparative Examples 1-3, the stirring speed of the aqueous phase is in rpm / min.

[0157] Table 3 Oil phase formulation

[0158]

[0159] Note: " / " indicates that it has not been added.

[0160] Table 4. Formulation of the aqueous phase

[0161]

[0162]

[0163] Note: (1) " / " means no addition; (2) The viscosity test conditions are: DVPlus viscometer, quantitative, 2# 200r / min, 25℃, 1min.

[0164] Effect Example

[0165] 1. The oily gel microspheres prepared in Examples 1-12 and Comparative Examples 1-3 were evaluated for relevant factors (particle size distribution, particle size uniformity, regularity, spreadability, hardness, absorption, and overall likability). The test results are shown in Table 6.

[0166] Particle size distribution: Measured using a 20cm ruler.

[0167] Particle size uniformity: The uniformity of particle size is evaluated by the experimenter by measuring the range of particle size. A++: Excellent (more than 90% within the middle particle size range), A+: Excellent (more than 80% within the middle particle size range), B: Good (more than 70% within the middle particle size range), C: Poor (more than 60% within the middle particle size range), D: Very poor (less than 60% within the middle particle size range).

[0168] Uniformity: The uniformity of the microspheres is assessed by the experimenter using the percentage of irregularities. A++: Excellent (irregularities less than 5%), A+: Excellent (irregularities less than 10%), B: Good (irregularities less than 20%), C: Poor (irregularities less than 30%), D: Very poor (irregularities greater than 40%). Note: "Irregularity" refers to the prepared microspheres having a non-spherical shape, such as an elliptical shape.

[0169] Ease of application:

[0170] Ten professionals were selected to rate the application performance. The rating criteria are as follows, and the average value is rounded to the nearest whole number.

[0171] 0-1 points: The cosmetic feels very oily and sticky when applied to the skin and is difficult to spread;

[0172] 1-2 points: The cosmetics feel slightly oily when applied to the skin, but are still relatively easy to spread;

[0173] 2-3 points: The cosmetic feels relatively smooth and easy to spread when applied to the skin, but there is still a certain stickiness.

[0174] 3-4 points: The cosmetics feel very smooth and easy to spread when applied to the skin, without any noticeable stickiness;

[0175] 4-5 points: The cosmetic feels very smooth and light when applied to the skin, with almost no stickiness, and is very easy to spread.

[0176] hardness:

[0177] Ten professionals were selected to rate the hardness of the oily gel microbeads and the resistance on the skin during application, and the average value was rounded off.

[0178] The scoring criteria are as follows:

[0179] 0-1 points: The cosmetic feels very hard and difficult to spread when applied to the skin;

[0180] 1-2 points: The cosmetic feels slightly firm when applied to the skin, but it is still relatively easy to spread.

[0181] 2-3 points: The cosmetic feels somewhat firm when applied to the skin, but it is relatively smooth and easy to spread;

[0182] 3-4 points: The cosmetic feels relatively soft when applied to the skin, with a certain degree of firmness, but it is easy to spread.

[0183] 4-5 points: The cosmetic feels very soft and smooth when applied to the skin, without any noticeable hardness, and is very easy to spread.

[0184] Absorbability: This refers to the degree to which cosmetics are absorbed by the skin, used to assess the permeability and absorbability of cosmetics. The scoring criteria are as follows:

[0185] 0-1 points: The cosmetic feels very oily after being applied to the skin and is difficult for the skin to absorb;

[0186] 1-2 points: The cosmetic feels slightly oily after being applied to the skin and takes some time to be absorbed.

[0187] 2-3 points: The cosmetics feel smooth after being applied to the skin and are easily absorbed, but it still takes some time.

[0188] 3-4 points: The cosmetics feel very smooth after being applied to the skin, are easily absorbed by the skin, and are absorbed quickly.

[0189] 4-5 points: The cosmetic feels very light and is easily absorbed after being applied to the skin, leaving almost no residue, making it very suitable for skin absorption.

[0190] Overall preference:

[0191] This refers to consumers' overall satisfaction and preference for cosmetics, typically including assessments of multiple aspects such as product texture, scent, ease of use, and efficacy. The following are the rating criteria:

[0192] 0-1 points: Consumers have no liking for this cosmetic product and may even have a strong aversion to it;

[0193] 1-2 points: Consumers have a very low level of liking for this cosmetic product and may give some negative reviews;

[0194] 2-3 points: Consumers generally have a moderate level of liking for this cosmetic product, and may have some neutral or positive reviews;

[0195] 3-4 points: Consumers have a high level of liking for this cosmetic product and may give some positive reviews;

[0196] 4-5 stars: Consumers have a very high level of liking for this cosmetic product and are likely to give it many positive reviews.

[0197] 2. Moisturizing test

[0198] Oily gel microsphere mixture: Oily gel microsphere and aqueous phase mixtures were prepared according to the preparation methods of Examples 5-7, and part of the aqueous phase was filtered off so that the mass ratio of oily gel microsphere and aqueous phase mixture was 1:1.

[0199] The above-mentioned oily gel microbead mixture was prepared into moisturizing essences according to the following formulas, and moisturizing properties were tested.

[0200] Based on a total weight of 100 parts: 22 parts oily gel microbead mixture, 69.36 parts deionized water, 0.3 parts pH100, 0.16 parts PC 2000, 0.03 parts sodium hyaluronate, 0.5 parts AM 20, 0.1 parts allantoin, 0.25 parts EZ-4U, 0.25 parts Symsave H, 4 parts 1,3-propanediol, 3 parts glycerol, and 0.05 parts disodium EDTA.

[0201] The above raw materials were mixed to prepare a moisturizing essence with a viscosity of 7000 mPa·s. The viscosity test conditions were: 25℃, No. 94 rotor, and a rotation speed of 5 rpm.

[0202] Experimental Methods: After cleaning their forearms, the subjects sat quietly for 30 minutes with their forearms exposed in a temperature and humidity controlled laboratory (temperature: 21.0±2.0℃; humidity: 50±5%). Eleven subjects were selected, and three 3cm x 3cm areas were marked on both arms. The instrument measured the initial moisture content of the skin in the marked areas and the initial transepidermal water loss. 20μL of different test samples were evenly applied to the marked areas, and instrument tests were performed 2h, 4h, and 6h after application.

[0203] Materials and instruments:

[0204] (a) Reagents and materials: facial tissues, hand sanitizer, continuous pipettes (Gilson, USA);

[0205] (b) Instruments: E / IB-053 Skin Moisture Meter CM825 (CK, Germany); E / IE-204 Moisture Loss Meter TEWL (CK, Germany); E / IB-033 Temperature and Humidity Meter ZJ1-2B (China).

[0206] Statistical methods:

[0207] Calculate the average of the initial values ​​for each test area, and then use the average to statistically analyze the differences between different product groups and the control group before and after use. Calculate the improvement rate between the test values ​​before and after use for each test area.

[0208] As shown in Table 5, the serum containing the gel microbeads of this application can significantly reduce transepidermal water loss and improve the skin's moisturizing rate, demonstrating good moisturizing ability.

[0209] Table 5. Transdermal water loss rate and moisture retention rate after 24 hours

[0210]

[0211] 3. Low-temperature stability test:

[0212] The test subject was the moisturizing essence prepared in "2. Moisturizing Test" above. The moisturizing essence was placed in a sealed container and stored at -20℃ for one month. The state of the oily gel microbeads was observed. The test results are shown in Table 6 and Figures 6-7 . Figure 6 The image shows the oily gel microspheres prepared in Comparative Example 1 after low-temperature testing. Figure 7 The image shows the oily gel microspheres prepared in Comparative Example 2 after low-temperature testing.

[0213] Table 6 Performance evaluation of the microspheres prepared in Examples 1-12 and Comparative Examples 1-3

[0214]

[0215]

[0216] Figure 3 , Figure 4 and Figure 5 Images of the oily gel microspheres prepared in Examples 3, 4, and 5, respectively. Figures 3-5 It can be seen that the oily gel microspheres prepared by this invention are in an oily microsphere state, are transparent, smooth and glossy, and exhibit a crystal-clear transparency. According to Figure 6 It can be seen that the oily gel microspheres prepared by the present invention did not change in shape and color after low-temperature stability testing, and have good low-temperature stability.

[0217] The oily gel microbeads prepared in Examples 1-12 of this invention have a melting temperature of about 37°C, which is the human body temperature. They can melt upon contact with the skin without the need for a special pump head to break them up. Because they are oily, they are easy to apply evenly and have strong skin adhesion. When added to skin care products, they have strong moisturizing and repairing properties.

[0218] Furthermore, as shown in Table 5, the oily gel microspheres prepared in Examples 1-12 of the present invention have a particle size distribution between 0.1-4 mm, good particle size uniformity and regularity, moderate hardness, good spreadability, easy absorption, high overall likability, and good low-temperature stability.

[0219] Compared to Example 1, Comparative Example 1 used caprylic / capric triglyceride instead of triglyceride (ethylhexanoate), according to Figure 7 It can be seen that the low-temperature stability test of the oily gel microbeads prepared by them was unqualified, and the microbeads broke.

[0220] Compared to Example 1, Comparative Example 2 reduced the amount of low-freezing-point oil to 2%, according to Figure 8 It can be seen that the low-temperature stability test of the oily gel microbeads prepared by them was unqualified, and the microbeads ruptured and turned white.

[0221] Comparative Example 3 used a low-freezing-point oil (i.e., C13-15 alkyl) with a freezing point of -65℃. The low-temperature stability test of the oily gel microbeads prepared by it failed, and the microbeads turned white.

Claims

1. An oily gel microbead, characterized by, The preparation method of the oil gel microbead comprises the following steps: (1) preparing an oil phase: adding a low freezing point oil and a semi-solid oil into a mixed solution formed by a polar oil and an oil phase gel agent to obtain the oil phase; (2) preparing a water phase: mixing water 95-99.9% and a thickening agent 0.01-5% uniformly to prepare the water phase, the percentages of the components in the water phase being mass percentages; (3) using the oil phase and the water phase to prepare the oil gel microbead through a microfluidic device; the mass ratio of the oil phase to the water phase is 1:(1-5.5); the oil gel microbead comprises a polar oil, an oil phase gel agent 5-20%, a low freezing point oil 3-8% and a semi-solid oil 0.2-2%, the percentages of the components in the oil phase being mass percentages; wherein the polar oil is glyceryl tri(ethylhexanoate) 70-90% and white pool rapeseed oil 0.1-5%; the oil phase gel agent is castor oil / IPDI copolymer; the low freezing point oil has a freezing point of -80℃; the low freezing point oil is C13-16 isoparaffin; the semi-solid oil is bis-diglyceryl polyacyladipate-2 or butyrospermum parkii (shea) fruit oil.

2. The oil gel microbead of claim 1, wherein the amount of the glyceryl tri(ethylhexanoate) is 72-89%; and / or, the amount of the white pool rapeseed oil is 0.2-4%.

3. The oil gel microbead of claim 2, wherein the amount of the glyceryl tri(ethylhexanoate) is 74.2%, 74.4%, 78.5%, 78.7%, 81.2%, 84.7%, 87.9% or 88%; and / or, the amount of the white pool rapeseed oil is 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5% or 4%.

4. The oil gel microbead of claim 1, wherein the amount of the oil phase gel agent is 6-18%.

5. The oil gel microbead of claim 4, wherein the amount of the oil phase gel agent is 7.5%, 8.0%, 8.5%, 9.5%, 11%, 12%, 13%, 14% or 15%.

6. The oil gel microbead of claim 1, wherein the amount of the low freezing point oil is 3%, 4%, 5%, 6%, 7% or 8%.

7. The oil gel microbead of claim 1, wherein the amount of the semi-solid oil is 0.5% or 1%.

8. The oil gel microbead of claim 1, wherein the mass ratio of the oil phase to the water phase is 1:1, 1:2, 1:3, 1:4.5 or 1:5.

5.

9. A skin care product, characterized by, It comprises the oil gel microbead according to any one of claims 1-8.

10. Use of the oil gel microbead according to any one of claims 1-8 in skin care products.

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