An oat whole ingredient extract, its extraction process and application in multifunctional cosmetics, pickering emulsion

Abstract

The application belongs to the technical field of cosmetics, and particularly relates to an oat whole-component extract, an extraction process thereof, application of the oat whole-component extract in multifunctional cosmetics, and Pickering emulsion. The extraction process comprises the following steps: first, performing subcritical extraction on oat kernel fine powder to obtain oat oil and residues; second, mixing the residues with a buffer solution, performing ultrasonic-microwave assisted extraction, filtering, collecting an extract and filter residues; third, performing carboxylation reaction of the extract with CO2, then performing reaction with 3-diethylaminopropylamine, and finally performing reaction with hexanol to obtain oat alkaloids; and finally, performing extraction of the filter residues in water, and performing enzymatic hydrolysis using cellulase to obtain oat beta-glucan. The extraction process is green and environmentally friendly, and solves the problems of single component, high solvent residue and high energy consumption in the prior art. The extract exhibits significant multifunctional synergistic effect in cosmetics, and has industrialization potential.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, specifically relating to an extract of all oat components, its extraction process, its application in multifunctional cosmetics, and Pickering lotion. Background Technology

[0002] Oats are one of the world's eight major grain crops, rich in nutrients and containing a variety of functional components, including minerals, protein, vitamins, and dietary fiber. Their protein content is as high as 16%, making them one of the grains with the highest protein content. This protein contains 18 amino acids, eight of which are essential amino acids for the human body, and the content of lysine and tryptophan is significantly higher than in other grains. Oats also contain various functional components, such as antioxidants like glutathione, polyphenols, phytosterols, and vitamins, as well as protein, unsaturated lipids, polyphenols, alkaloids, saponins, and beta-glucan.

[0003] Oat oil is rich in 95% high-quality fatty acids, mainly palmitic acid, oleic acid, and linoleic acid. It also contains polyphenols, sterols, and endogenous vitamin E precursors, among other antioxidants, which can scavenge free radicals and delay aging. Therefore, oat oil is frequently used in cosmetics. Currently, the main methods for extracting vegetable oils domestically and internationally are pressing and solvent extraction. Solvent extraction includes traditional solvent extraction and supercritical fluid extraction. Pressing, due to its high temperature, easily leads to oil oxidation and deterioration; traditional solvent extraction suffers from high solvent residue; and supercritical fluid extraction has a small production scale, hindering industrialization.

[0004] β-glucan is a short-chain glucan with a relatively small molecular weight. It can enhance the body's immunity, nourish the skin, and restore its elasticity. When added to cosmetics, it has skin-nourishing, anti-aging, and other effects. Industrially, β-glucan is mainly prepared by grinding wheat bran, sieving, removing impurities, and then directly extracting the β-glucan. Extraction methods mainly include chemical and enzymatic methods. Enzymatic extraction primarily extracts water-soluble β-glucan, while water-insoluble β-glucan is discarded as waste, resulting in its loss. It also consumes a large amount of water, leading to significant wastewater treatment. Chemical extraction mainly uses solvent methods such as alkaline extraction, alcohol precipitation, and salting out to improve the purity of β-glucan.

[0005] For example, Chinese invention patent publication number CN110204630A discloses a method for preparing oat beta-glucan and its application. The method includes the following steps: S1, oat bran is put into hot water, extracted at high temperature and then filtered; S2, the filtrate obtained in step S1 is added to alumina for directional impurity removal and then filtered; S3, the pH of the filtrate obtained in step S2 is adjusted to the isoelectric point, then activated carbon is added for heat preservation and then filtered; S4, the filtrate obtained in step S3 is added to polyacrylamide, stirred and complexed and then filtered; S5, the supernatant obtained in step S4 is desalted and deacidified to obtain the product. However, this preparation method requires the separation of grain bran first, which greatly increases the labor intensity. Moreover, a large amount of organic solvent polyacrylamide needs to be added during the extraction process, which is costly and not conducive to large-scale industrial production.

[0006] Oat alkaloids have excellent antioxidant, anti-allergic and anti-itch effects. Compared with oat beta-glucan and oat peptides (the main components in traditional oat extracts), they are more likely to penetrate the epidermis and enter the dermis, thereby exerting antihistamine and anti-allergic effects.

[0007] In modern cosmetics, oats are typically added as single ingredients (such as beta-glucan moisturizers, oat alkaloid antioxidants, or oat oil skin conditioners), resulting in limited efficacy. Therefore, there is an urgent need in the field to provide an extract utilizing all the components of oats, enabling cosmetics to simultaneously possess anti-inflammatory, repair, and barrier-rebuilding functions. Summary of the Invention

[0008] This invention addresses the problems existing in the prior art by providing an extract of all oat components, its extraction process, and its application in multifunctional cosmetics, specifically Pickering lotion.

[0009] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0010] An extraction process for an extract of all components of oats includes the following steps:

[0011] (1) First, the fine powder of oat kernels is subjected to subcritical extraction to obtain oat oil and residue;

[0012] (2) The residue is then mixed with buffer solution and subjected to ultrasonic-microwave assisted extraction, filtered, and the extract and filter residue are collected.

[0013] (3) The extract obtained in step (2) is reacted with CO2 to undergo a carboxylation reaction, then with 3-diethylaminopropylamine, and finally with hexanol to obtain oat alkaloids;

[0014] (4) Finally, the filter residue obtained in step (2) is extracted in water and then hydrolyzed with cellulase to obtain oat β-glucan.

[0015] Preferably, the D of the oat kernel powder described in step (1) 50 =10-20 μm.

[0016] Preferably, the mass-to-volume ratio of the oat kernel powder to the extractant in step (1) is 1 g: 1-4 mL, and the extractant is butane or propane.

[0017] Preferably, the extraction temperature in step (1) is 30-40℃, the extraction pressure is 3-5 MPa, and the extraction time is 1-3 h.

[0018] Preferably, the oat oil in step (1) contains 35-45% oleic acid.

[0019] Preferably, the buffer solution in step (2) is a mixture of ethanol and phosphate with a volume ratio of 0.2-0.3:1, and the pH of the buffer solution is 7-7.8.

[0020] Preferably, the mass-to-volume ratio of the residue to the buffer solution in step (2) is 1 g: 5-15 mL.

[0021] Preferably, in step (2), the ultrasonic frequency of the ultrasound-microwave is 20-40 kHz, the microwave frequency is 2400-2500 MHz, and the power of the ultrasound-microwave is 200-400 W.

[0022] Preferably, the extraction temperature in step (2) is 45-65℃ and the extraction time is 20-30 min.

[0023] Preferably, the carboxylation reaction process in step (3) includes: reacting the extract with CO2 at a molar ratio of 1:1-3 at 2-4 MPa and at 45-55°C for 1-3 h to generate carboxylated products.

[0024] Preferably, the reaction process with 3-diethylaminopropylamine in step (3) includes: reacting the carboxylation product, 3-diethylaminopropylamine, DCC and DMAP in a molar ratio of 1:1-1.5:1.4-1.6:0.1 at 50-70°C for 3-5 h to generate the amidation product.

[0025] Preferably, the reaction with hexanol in step (3) includes: reacting the amidation product, hexanol and sulfuric acid in a molar volume ratio of 1 mol: 2.5-3.5 mol: 0.1-1.0 mL at 60-80 °C for 1-3 h.

[0026] Preferably, the temperature of the water in step (4) is 80-95°C, and the extraction time is 20-40 min.

[0027] Preferably, the mass ratio of filter residue to cellulase in step (4) is 1:0.05-0.1.

[0028] Preferably, the enzymatic hydrolysis temperature in step (4) is 45-60℃ and the enzymatic hydrolysis time is 60-100 min.

[0029] The present invention also provides an extract obtained by the above extraction process, wherein the extract comprises oat oil, oat alkaloids and oat β-glucan in a mass ratio of 4-6:1:3-5.

[0030] The present invention also provides a Pickering emulsion comprising the above-described extract and nano-silica.

[0031] Preferably, the average particle size of the Pickering emulsion is 100-200 nm.

[0032] The present invention also provides the application of the above-mentioned extract in the preparation of cosmetics with anti-inflammatory, moisturizing and barrier repair functions.

[0033] Preferably, the amount of the extract added to the cosmetic is 0.5-5 wt%.

[0034] Compared with the prior art, the present invention has the following beneficial effects:

[0035] (1) This invention provides an extract of all oat components. Through green process design, synergistic extraction of all components and precise reaction control, it solves the problems of single component, high solvent residue and high energy consumption in the prior art. The extract shows a significant multifunctional synergistic effect in cosmetics and has industrialization potential.

[0036] (2) The present invention also provides the application of the extract of the whole oat components in Pickering lotion, and further expands the stability and transdermal efficiency of oat active ingredients, which is in line with the development trend of high efficiency, safety and sustainability in the cosmetics industry. Detailed Implementation

[0037] It is worth noting that all raw materials used in this invention are commercially available products. Specifically, the following are included: ethanol (95% by volume); potassium dihydrogen phosphate (0.01-0.1 mol / L); sulfuric acid (50% by volume); methanol (15% by volume); hexanol (90% by volume); jojoba oil (purchased from Henry Lamote Oils & Fats Ltd.); cellulase (purchased from Cangzhou Xiasheng Enzyme Biotechnology Co., Ltd.); commercially available oat oil (purchased from Jiangxi Wanlv Natural Flavors Co., Ltd.); oat alkaloid standard (99% purity) (purchased from Aladdin Scientific); DMEM culture medium (purchased from Solarbio Science & Technology Co., Ltd.); HaCaT cells (purchased from Yaji Biotechnology Co., Ltd.); and the Human IL-1α ELISA Kit (purchased from R&D Systems).

[0038] DCC stands for N,N'-dicyclohexylcarbodiimide; DMPA stands for dimethylolpropionic acid; EDC stands for 1-ethyl-(3-dimethylaminopropyl)carbodiimide; and HOBt stands for 1-hydroxybenzotriazole.

[0039] Example 1

[0040] An extract of all oat components, composed of oat oil, oat alkaloids, and oat β-glucan in a mass ratio of 5:1:4. The extraction process for this extract is as follows:

[0041] (1) Extraction of oat oil: D 50 Oat kernel powder with a particle size of 15 μm was subjected to subcritical extraction (the conditions for subcritical extraction were: butane as the extractant, a mass-to-volume ratio of oat kernel powder to extractant of 1 g:2 mL, an extraction temperature of 35℃, an extraction pressure of 4 MPa, and an extraction time of 1 h). The extractant was then recovered by rotary evaporation under reduced pressure to obtain oat oil and residue. The yield of oat oil was 10% (GC-MS showed that the linoleic acid content in the oat oil was 38.2%).

[0042] (2) Extraction of oat alkaloids: The residue was mixed with an ethanol / phosphate buffer solution of pH=7.4 (ethanol / phosphate volume ratio of 0.25:1) at a mass-volume ratio of 1 g:10 mL, and ultrasonic-microwave assisted extraction was performed (the assisted extraction conditions were: ultrasonic frequency of 40 kHZ, microwave frequency of 2480 MHZ, power of 300 W, temperature of 50℃, and time of 30 min). The mixture was filtered to obtain the extract and filter residue for later use.

[0043] HPLC analysis of the extract revealed that the total amount of avenanthramides (i.e., phenolamides in oats) reached 2.1%, indicating that the extract contained hydroxy-o-aminobenzoic acid. The extract was subjected to a Kolbe-Schmitt reaction (molar ratio of extract to CO2:1:3, reaction pressure: 2 MPa, reaction temperature: 50℃, reaction time: 2 h) to obtain the carboxylated product, o-carboxyphenoxy derivative. Then, it was subjected to an amidation reaction with 3-diethylaminopropylamine under DCC / DMAP catalysis (molar ratio of carboxylated product, 3-diethylaminopropylamine, DCC, and DMAP: 1:1.2:1.5:0.1, reaction temperature: 60℃, reaction time: 4 h) to obtain the amidated product, N-(3-diethylaminopropylamine)-o-carboxybenzamide. Finally, it was subjected to an esterification reaction with hexanol under sulfuric acid catalysis (molar volume ratio of N-(3-diethylaminopropylamine)-o-carboxybenzamide, hexanol, and sulfuric acid: 1 mol:3 mol:0.1-0.5 mL, reaction temperature: 70℃, reaction time: 2 h) to obtain oat alkaloids with a yield of 2% and a purity of 90%.

[0044] (3) Extraction of oat β-glucan: After soaking the filter residue from step (2) in water at 90℃ for 30 min, add cellulase to the water at a mass ratio of filter residue to cellulase of 1:0.05, and enzymatically hydrolyze at 50℃ for 60 min to obtain β-glucan with a molecular weight of 200 KDa (yield of 8% and purity of 90%).

[0045] Example 2

[0046] An extract of all oat components, composed of oat oil, oat alkaloids, and oat β-glucan in a mass ratio of 4:1:3. The extraction process of this extract is as follows:

[0047] (1) Extraction of oat oil: D 50 Oat kernel powder with a particle size of 10 μm was subjected to subcritical extraction (the conditions for subcritical extraction were: propane as the extractant, a mass-to-volume ratio of oat kernel powder to extractant of 1 g: 3 mL, an extraction temperature of 30℃, an extraction pressure of 3 MPa, and an extraction time of 2 h). The extractant was then recovered by rotary evaporation under reduced pressure to obtain oat oil and residue. The yield of oat oil was 16.5% (GC-MS showed that the linoleic acid content in the oat oil was 35%).

[0048] (2) Extraction of oat alkaloids: The residue was mixed with an ethanol / phosphate buffer solution of pH=7.0 (ethanol / phosphate volume ratio of 0.2:1) at a mass-volume ratio of 1 g:10 mL, and ultrasonic-microwave assisted extraction was performed (the assisted extraction conditions were: ultrasonic frequency of 28 kHZ, microwave frequency of 2450 MHZ, power of 200 W, temperature of 45℃, and time of 30 min). The mixture was filtered to obtain the extract and filter residue for later use.

[0049] HPLC analysis of the extract revealed that the total amount of avenanthramides (i.e., phenolamides in oats) reached 1.5%, indicating that the extract contained hydroxy-o-aminobenzoic acid. The extract was then subjected to a Kolbe-Schmitt reaction (molar ratio of extract to CO2:1.2, reaction pressure: 2 MPa, reaction temperature: 50℃, reaction time: 2 h) to obtain the carboxylated product, o-carboxyphenoxy derivative. This was then subjected to an amidation reaction with 3-diethylaminopropylamine under DCC / DMAP catalysis (molar ratio of o-carboxyphenoxy derivative, 3-diethylaminopropylamine, DCC, and DMAP: 1:1.2:1.5:0.1, reaction temperature: 60℃, reaction time: 4 h) to obtain the amidated product, N-(3-diethylaminopropyl)-o-carboxybenzamide. Finally, it was subjected to an esterification reaction with hexanol under sulfuric acid catalysis (molar volume ratio of N-(3-diethylaminopropyl)-o-carboxybenzamide, hexanol, and sulfuric acid: 1 mol:3 mol:0.1 mL, reaction temperature: 70℃, reaction time: 2 h). (h) to obtain oat alkaloids with a yield of 1.8% and a purity of 92%.

[0050] (3) Extraction of oat β-glucan: After soaking the filter residue from step (2) in water at 80°C for 40 min, add cellulase to the water at a mass ratio of filter residue to cellulase of 1:0.05, and enzymatically hydrolyze at 50°C for 90 min to obtain β-glucan with a molecular weight of 180 KDa (yield of 7% and purity of 82%).

[0051] Example 3

[0052] An extract of all oat components, composed of oat oil, oat alkaloids, and oat β-glucan in a mass ratio of 6:1:5. The extraction process for this extract is as follows:

[0053] (1) Extraction of oat oil: D 50Subcritical extraction was performed on oat kernel powder with a particle size of 20 μm (the conditions for subcritical extraction were: propane as the extractant, a mass-to-volume ratio of oat kernel powder to extractant of 1 g: 4 mL, an extraction temperature of 40℃, an extraction pressure of 5 MPa, and an extraction time of 3 h). The extractant was then recovered by rotary evaporation under reduced pressure to obtain oat oil and residue. The yield of oat oil was 18% (GC-MS showed that the linoleic acid content in the oat oil was 45%).

[0054] (2) Extraction of oat alkaloids: The residue was mixed with an ethanol / phosphate buffer solution at pH 7.8 (ethanol / phosphate volume ratio of 0.3:1) at a mass-volume ratio of 1 g:10 mL, and extracted with ultrasound-microwave assisted extraction (the assisted extraction conditions were: ultrasound frequency of 28 kHZ, microwave frequency of 2450 MHZ, power of 400 W, temperature of 65℃, and time of 20 min). The mixture was filtered to obtain the extract and filter residue for later use.

[0055] HPLC analysis of the extract revealed that the total amount of avenanthramides (i.e., phenolamides in oats) reached 1.8%, indicating that the extract contained hydroxy-o-aminobenzoic acid. The extract was subjected to a Kolbe-Schmitt reaction (molar ratio of extract to CO2:1.2, reaction pressure: 2 MPa, reaction temperature: 50℃, reaction time: 2 h) to obtain the carboxylated product, o-carboxyphenoxy derivative. Then, it was subjected to an amidation reaction with 3-diethylaminopropylamine under DCC / DMAP catalysis (molar ratio of o-carboxyphenoxy derivative, 3-diethylaminopropylamine, DCC, and DMAP: 1:1.3:1.6:0.1, reaction temperature: 60℃, reaction time: 4 h) to obtain the amidated product, N-(3-diethylaminopropyl)-o-carboxybenzamide. Finally, it was subjected to an esterification reaction with hexanol under sulfuric acid catalysis (molar volume ratio of N-(3-diethylaminopropyl)-o-carboxybenzamide, hexanol, and sulfuric acid: 1 mol:3 mol:0.1 mL, reaction temperature: 70℃, reaction time: 2 h) to obtain oat alkaloids. The yield of oat alkaloids was 2%, and the purity was 90%.

[0056] (3) Extraction of oat β-glucan: After soaking the filter residue from step (2) in water at 95°C for 20 min, add cellulase to the water at a mass ratio of 1:0.1 between the filter residue and cellulase, and enzymatically hydrolyze at 50°C for 100 min to obtain β-glucan with a molecular weight of 250 KDa (yield of 7% and purity of 88%).

[0057] Comparative Example 1

[0058] Compared with Example 3, the only difference is that the ethanol / phosphate buffer in step (2) is replaced with distilled water to obtain oat alkaloids with a yield of 0.7% and a purity of 70%.

[0059] Comparative Example 2

[0060] Compared with Example 3, the only difference is that the catalyst DCC / DMAP in step (2) is replaced with EDC / HOBt, and step (2) is as follows:

[0061] Extraction of oat alkaloids: The residue was mixed with an ethanol / phosphate buffer solution at pH 7.8 (ethanol / phosphate volume ratio of 0.3:1) at a mass-volume ratio of 1 g:10 mL. Ultrasonic-microwave assisted extraction was performed (extraction conditions: ultrasonic frequency of 28 kHz, microwave frequency of 2450 MHz, power of 400 W, temperature of 65℃, and time of 20 min). The mixture was filtered to obtain the extract and filter residue for later use.

[0062] HPLC analysis of the extract revealed that the total amount of avenanthramides (i.e., phenolamides in oats) reached 1.2%, indicating that the extract contained hydroxy-o-aminobenzoic acid. The extract was subjected to a Kolbe-Schmitt reaction (molar ratio of extract to CO2:1.2, reaction pressure: 2 MPa, reaction temperature: 50℃, reaction time: 2 h) to obtain the carboxylated product, o-carboxyphenoxy derivative. This was then subjected to an amidation reaction with 3-diethylaminopropylamine under EDC / HOBt catalysis (molar ratio of o-carboxyphenoxy derivative, 3-diethylaminopropylamine, EDC, and HOBt: 1:1.3:1.5:0.2, reaction temperature: 60℃, reaction time: 8 h) to obtain the amidated product, N-(3-diethylaminopropylamine)-o-carboxybenzamide. Finally, it was subjected to an esterification reaction with hexanol under sulfuric acid catalysis (molar volume ratio of N-(3-diethylaminopropylamine)-o-carboxybenzamide, hexanol, and sulfuric acid: 1 mol:3 mol:0.1 mL, reaction temperature: 70℃, reaction time: 2 h). h), oat alkaloids were obtained with a yield of 1% and a purity of 80%.

[0063] Comparative Example 3

[0064] Compared with Example 3, the only difference is that hexanol in step (2) is replaced with methanol to obtain oat alkaloids. The yield of oat alkaloids is 1.5% and the purity is 85%.

[0065] Comparative Example 4

[0066] Compared to Example 3, the only difference is that it is an extract of all oat components, which consists of oat oil, oat alkaloids and oat β-glucan in a mass ratio of 2:3:4.

[0067] Test Example 1

[0068] Anti-inflammatory and repair tests were performed on the oat extracts prepared in Examples 1-3 and Comparative Examples 1-4, respectively, to detect the IL-1α inhibition rate and the increase in Claudin-1 expression.

[0069] The experiment is as follows:

[0070] 1. Sample preparation: The oat extracts prepared in Examples 1-3 and Comparative Examples 1-4 were dissolved in PBS to prepare test samples with a concentration of 0.5 mg / mL.

[0071] 2. Experimental Methods:

[0072] 5 × 10 HaCaT cells 4 Cells / wells were seeded in 6-well plates and cultured for 24 h, then replaced with serum-free DMEM medium and cultured for 2 h. An inflammation model was established by adding lipopolysaccharide (LPS) (1 μg / mL) to the medium for 6 h of stimulation.

[0073] The test sample (0.5 mg / mL), the positive control drug dexamethasone (1 μM), and single oat β-glucan (0.5 mg / mL) were added and treated for 24 h, respectively, and normal HaCaT cells (without any drugs added) were used as blank control group.

[0074] The IL-1α content was detected by ELISA (Human IL-1α ELISA Kit), and the IL-1α inhibition rate was calculated. The Claudin-1 expression level was detected by Western blotting with Anti-Claudin-1 as antibody and GAPDH as internal control, and the fold increase in Claudin-1 expression level was calculated.

[0075] The formula for calculating the IL-1α inhibition rate is as follows:

[0076] IL-1α inhibition rate (%) = (1 - IL-1α concentration in experimental group ÷ IL-1α concentration in blank control group) × 100%.

[0077] The formula for calculating the fold increase in Claudin-1 expression is as follows:

[0078] The fold increase in Claudin-1 expression level = normalized expression level in the experimental group ÷ normalized expression level in the blank control group.

[0079] The experimental results are shown in Table 1. As can be seen from Table 1, the extracts prepared in Examples 1-3 of this invention significantly improved the inhibition rate of inflammatory factor IL-1α and the expression level of Claudin-1 through the synergistic effect of all components, and enhanced the expression of tight junction proteins. They have both anti-inflammatory and repair effects, which are superior to traditional single components and comparative examples 1-4.

[0080] Table 1. IL-1α inhibition rate and Claudin-1 expression enhancement

[0081]

[0082] Note: * indicates p<0.05 compared with the positive control group.

[0083] Test Example 2

[0084] The oat extracts prepared in Examples 1-3 and Comparative Examples 1-4 were used to prepare Pickering emulsions. The preparation method was as follows: olive oil (10 g), oat extract (2 g), and deionized water (87.5 g) were mixed in a 40°C water bath for 10 min, and then stirred at 10000 r / min for 30 min using a high-speed stirrer to form a crude emulsion. Then, 0.5 g of 20 nm nano-silica was added to the crude emulsion, and stirring was continued at 5000 r / min for 10 min to ensure uniform dispersion. Finally, the emulsion was transferred to an ultrasonic cell disruptor and ultrasonically treated at 300 W for 20 min, with the water bath temperature controlled at 40°C, to obtain the final Pickering emulsion. The average particle size of the Pickering emulsions prepared from the extracts of Examples 1-3 was 100-200 nm.

[0085] The prepared Pickering emulsion was subjected to a permeation experiment. The experimental method was as follows: a Franz diffusion cell was used for transdermal permeation experiment. Fresh pigskin was used as the permeation barrier. The Pickering emulsion was evenly applied to the surface of the pigskin. The acceptor phase of the diffusion cell was physiological saline. Under constant temperature of 37℃, samples were taken from the acceptor phase at 1 h, 6 h and 24 h. The total content of key components (oat alkaloids, oat β-glucan and oat oil) in the oat whole component extract was determined by high performance liquid chromatography, and the transdermal permeation amount was calculated.

[0086] The experimental results are shown in Table 2. As can be seen from Table 2, the cumulative permeation amount in 24 h of Examples 1-3 (48-52 μg / cm²) was significantly higher than that of the comparative examples (30-38 μg / cm²).

[0087] Table 2 Transdermal Penetration

[0088]

[0089] Test Example 3

[0090] The oat extracts prepared in Examples 1-3 and Comparative Examples 1-4 were used to prepare soothing and repairing creams. The preparation method was as follows: by mass percentage, 3% oat extract, 2% ceramide EOP, 5% jojoba oil, 0.5% zinc gluconate, 0.2% carbomer 940, 0.8% phenoxyethanol (preservative), and the balance being water were mixed to obtain the soothing and repairing cream.

[0091] Human trials of the soothing and repairing cream were conducted. The experimental method involved recruiting 70 healthy subjects aged 18-45 years with mild skin sensitivity symptoms (such as redness and dryness) and randomly dividing them into 7 groups of 10 subjects each. After cleansing their faces morning and evening, subjects applied 0.4 ± 0.1 g of the corresponding group's soothing and repairing cream evenly to the sensitive areas of their cheeks for 28 consecutive days. Epidermal water loss (TEWL, g / h / m³) was measured before and after 28 days of use using a CK-200 Cutometer. 2 The erythema index was measured using a colorimeter (CR-400), and the epidermal moisture loss rate (%) and the erythema index reduction rate (%) were further calculated. During the experiment, subjects were required to maintain their daily skincare routine and avoid using other functional skincare products and sun exposure.

[0092] The formula for calculating the epidermal moisture loss rate (%) is as follows:

[0093] Epidermal moisture loss rate (%) = (W1 - W2) ÷ W1 × 100%

[0094] W1 represents the TEWL value before using the product; W2 represents the TEWL value after using the product for 28 days. A higher epidermal moisture loss rate indicates a greater reduction in transdermal moisture loss, resulting in a better repair effect.

[0095] The formula for calculating the erythema index reduction rate (%) is as follows:

[0096] Erythema index reduction rate (%) = (C1 - C2) ÷ C1 × 100%

[0097] Wherein, C1 represents the chromaticity value before the product was used; C2 represents the chromaticity value after 28 days of using the product.

[0098] The experimental results are shown in Table 3. Table 3 shows that the soothing and repairing creams prepared in Examples 1-3 are significantly effective in improving skin barrier function and relieving inflammation. Compared with Example 3, Comparative Example 1 suffered from insufficient extraction of active ingredients due to buffer replacement; Comparative Example 2 had its component activity affected by catalyst changes; Comparative Example 3 had alcohol replacement due to esterification reaction; and Comparative Example 4 had changes in the proportion of extract components, all resulting in lower rates of epidermal moisture loss and erythema index reduction. Therefore, the extraction process and component proportions of Examples 1-3 are more conducive to the soothing and repairing creams exerting their moisturizing and anti-inflammatory effects.

[0099] Table 3. Test results of epidermal moisture loss rate and erythema index decrease rate.

[0100]

[0101] Test Example 4

[0102] The antioxidant effects of the oat oils prepared in Examples 1-3 were first tested. The experimental methods are as follows: Approximately 50 mL of the oat oils prepared in Examples 1-3 were placed in brown glass bottles, sealed, protected from light, and stored in a 45°C incubator for 30 days. The peroxide value was then measured (using the titration method according to GB5009.227-2016). Commercially available oat oil served as the blank control group, and commercially available oat oil with a final concentration of 0.1% vitamin E served as the positive control group. Three replicates were set for each group.

[0103] The peroxide value data of oat oil are shown in Table 4. Compared with the blank control group and the positive control group, the peroxide value of oat oil in Examples 1-3 is higher, indicating that the oat oil in Examples 1-3 has good antioxidant properties.

[0104] Table 4 Peroxide value of oat oil

[0105]

[0106] Accelerated oxidation experiments were then conducted on the oat alkaloid extracts prepared in Examples 1-3 and Comparative Examples 1-3, respectively. The specific methods are as follows: The extracts were placed in a 45℃ incubator for accelerated oxidation for 30 days, with three parallel samples in each group. On day 31, 0.5 g of the extract was weighed and placed in a stoppered Erlenmeyer flask, 10 mL of 70% methanol was added, and the mixture was ultrasonically extracted for 30 min in an ultrasonic bath (power 200 W, temperature 25℃). After extraction, the sample was transferred to a centrifuge tube and centrifuged at 10000 r / min for 10 min. The supernatant was then filtered through a 0.45 μm filter membrane, and the filtrate was used as the test sample. The oat alkaloid content in the filtrate was detected by HPLC, and the alkaloid retention rate was further calculated.

[0107] The HPLC detection conditions are as follows:

[0108] 1. Chromatographic conditions: C18 column (4.6 mm × 250 mm, 5 μm); mobile phase: acetonitrile-0.1% phosphoric acid aqueous solution (v / v = 15:85); flow rate: 1.0 mL / min; column temperature: 30℃; detection wavelength: 265 nm; injection volume: 10 μL.

[0109] 2. Standard Curve Construction: Accurately weigh an appropriate amount of oat alkaloid standard and prepare a series of standard solutions with concentrations of 1, 5, 10, 20, and 50 μg / mL using 70% methanol. Inject and detect the solutions under the chromatographic conditions described above. Plot a standard curve with peak area (Y) on the ordinate and concentration (X, μg / mL) on the abscissa. The linear correlation coefficient R² should be ≥ 0.999.

[0110] 3. System suitability: Inject a standard solution with a concentration of 10 μg / mL, record the chromatogram, and ensure that the theoretical plate number calculated based on the oat alkaloid peak is not less than 5000, and the resolution between adjacent peaks is greater than 1.5.

[0111] The formula for calculating the alkaloid retention rate is as follows:

[0112] Alkaloid retention rate (%) = (Peak area of ​​alkaloids after accelerated experiment ÷ Peak area of ​​alkaloids at the beginning) × 100%

[0113] The data results of alkaloid retention rate are shown in Table 5. Compared with Comparative Examples 1-4, the alkaloid content retention rate of the extracts in Examples 1-3 is higher, indicating that the extracts have better stability.

[0114] Table 5. Alkaloid retention rate in extracts

[0115]

[0116] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, and is not intended to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions made by those skilled in the art to the technical solution of the present invention do not depart from the essence and scope of the technical solution of the present invention.

Claims

1. An extract of all oat components, characterized in that, The extract comprises oat oil, oat alkaloids, and oat β-glucan in a mass ratio of 4-6:1:3-5. The extraction process of the extract includes the following steps: (1) First, the fine powder of oat kernels is subjected to subcritical extraction to obtain the oat oil and residue; (2) The residue is then mixed with buffer solution and subjected to ultrasonic-microwave assisted extraction, filtered, and the extract and filter residue are collected. (3) The extract obtained in step (2) is reacted with CO2 to undergo a carboxylation reaction, then with 3-diethylaminopropylamine, and finally with hexanol to obtain the oat alkaloids; (4) Finally, the filter residue obtained in step (2) is extracted in water and then hydrolyzed with cellulase to obtain the oat β-glucan; In step (1), the extractant is butane or propane, the extraction temperature is 30-40℃, the extraction pressure is 3-5 MPa, and the extraction time is 1-3 h; the mass-volume ratio of the oat kernel powder to the extractant is 1 g: 1-4 mL. In step (2), the buffer solution is a mixture of ethanol and phosphate with a volume ratio of 0.2-0.3:1, and the pH of the buffer solution is 7-7.8; In step (3), the carboxylation reaction includes: reacting the extract with CO2 at a molar ratio of 1:1-3 at 45-55℃ for 1-3 h at 2-4 MPa to generate the carboxylated product; the reaction with 3-diethylaminopropylamine includes: reacting the carboxylated product, 3-diethylaminopropylamine, DCC and DMAP at a molar ratio of 1:1-1.5:1.4-1.6:0.1 at 50-70℃ for 3-5 h to generate the amidated product; the reaction with hexanol includes: reacting the amidated product, hexanol and sulfuric acid at a molar volume ratio of 1 mol:2.5-3.5 mol:0.1-0.5 mL at 60-80℃ for 1-3 h.

2. The extract according to claim 1, characterized in that, In step (1), the D of the fine oat kernel powder 50 =10-20μm; the oleic acid content in the oat oil is 35-45%.

3. The extract according to claim 1, characterized in that, The mass-to-volume ratio of the residue to the buffer solution in step (2) is 1 g: 5-15 mL.

4. The extract according to claim 1, characterized in that, In step (2), the ultrasonic frequency of the ultrasound-microwave is 20-40 kHz, the microwave frequency of the ultrasound-microwave is 2400-2500 MHz, and the power of the ultrasound-microwave is 200-400 W; the extraction temperature is 45-65℃, and the extraction time is 20-30 min.

5. The extract according to claim 1, characterized in that, In step (4), the water temperature is 80-95℃, the extraction time is 20-40 min, the mass ratio of the filter residue to cellulase is 1:0.05-0.1, the enzymatic hydrolysis temperature is 45-60℃, and the enzymatic hydrolysis time is 60-100 min.

6. A Pickering emulsion, characterized in that, Includes the extract and nano-silica as described in any one of claims 1-5.

7. The use of the extract as described in any one of claims 1-5 in the preparation of cosmetics having anti-inflammatory, moisturizing and barrier repair functions.

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