Camellia oil for improving skin moisture and fine lines and a preparation method thereof
By reconstructing the molecular structure of camellia oil through supercritical fluid extraction and bio-enzymatic directional transesterification, and combining it with functional lipids and acoustic nano-processing, the problems of low γ-linolenic acid content and rapid oxidation in traditional camellia oil have been solved, achieving high permeability and long-lasting water-locking effects, improving skin moisture and fine lines.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- JIANGXI GANZHICUN FOOD CO LTD
- Filing Date
- 2026-06-15
- Publication Date
- 2026-08-04
AI Technical Summary
Traditional camellia oil has a low content of gamma-linolenic acid, which leads to damage to the skin barrier function. Existing oil-based skin care products have problems with uneven mixing and rapid oxidation at the thermodynamic and molecular dynamic levels, making it difficult to effectively improve skin moisture and fine lines.
By combining supercritical fluid extraction with bio-enzymatic directional transesterification technology, the molecular structure of camellia oil is precisely reconstructed, functional lipid components are added, and acoustic nano-processing is performed to form a highly permeable and stable camellia oil that improves skin hydration and fine lines.
It achieves the high permeability and strong barrier repair function of camellia oil, solves the problems of layering, uneven absorption and oxidation of traditional compound oils, provides the effect of instant filling and long-lasting water locking, and improves the skin's moisture content and fine lines.
Abstract
Description
Technical Field
[0001] This invention discloses a camellia oil that improves skin moisture and fine lines, and its preparation method, belonging to the field of functional oil processing and cosmetic biotechnology. Background Technology
[0002] Camellia oil has a history of edible and medicinal use in my country spanning thousands of years. Due to its excellent physicochemical properties and physiological activity, it is hailed as the "olive oil of the East." Chemically, camellia oil's main component is triglycerides, with oleic acid—a monounsaturated fatty acid—typically comprising 75-85%. This high proportion of oleic acid gives camellia oil excellent chemical stability and skin affinity. In skincare, camellia oil effectively moisturizes the stratum corneum, relieves dryness, and forms a hydrophobic protective film on the epidermis.
[0003] However, with the advancement of dermatological research, traditional camellia oil has revealed significant limitations in addressing the needs of modern precision skincare. First, the fatty acid structure of natural camellia oil is relatively simple. Although it is rich in oleic acid, the content of polyunsaturated fatty acids (PUFAs) that are crucial for skin barrier repair, such as gamma-linolenic acid (GLA) and linoleic acid, is relatively low. In particular, gamma-linolenic acid is almost undetectable in natural camellia oil.
[0004] Gamma-linolenic acid (GLA) is a precursor to essential fatty acids for the human body, playing an irreplaceable role in maintaining the integrity of epithelial tissue, regulating sebaceous gland secretion, and inhibiting skin micro-inflammation. Studies have shown that with age or external environmental stimuli, the activity of the enzyme that synthesizes GLA in the human skin gradually declines, leading to impaired barrier function, increased transepidermal water loss, and ultimately the formation of dry fine lines.
[0005] Secondly, most existing oil-based skincare products use physical cold mixing or simple compounding methods. For example, camellia oil is directly mixed with evening primrose oil (rich in GLA). While this method can replenish missing fatty acids, it has serious defects at the thermodynamic and molecular dynamic levels. First, because the triglyceride skeleton structures of oils from different sources differ significantly, the penetration rate of the mixed oils on the skin surface is inconsistent. This often results in the lighter oils penetrating quickly while the heavier oils remain and accumulate, producing a severe sticky feeling. Second, the high degree of exposure of unsaturated bonds in physically mixed oils makes them highly susceptible to auto-oxidation in the air, producing an unpleasant "rancid" smell and generating peroxide free radicals, which can damage skin collagen and accelerate the formation of fine lines.
[0006] Therefore, the "structural reconstruction" technology of oils has become the core direction for solving the above problems. Structural lipids refer to novel fatty acid esters with specific physical properties or physiological activities obtained by altering the arrangement of fatty acids on the glycerol molecular backbone through chemical or enzymatic methods, or by introducing specific functional fatty acids. In the cosmetics field, by utilizing immobilized lipases with 1,3-position selectivity to replace excess oleic acid in camellia oil with γ-linolenic acid, which has a powerful repair function, a "biomimetic structural oil" can be constructed that retains the high permeability of camellia oil while possessing strong barrier repair capabilities.
[0007] However, achieving high-purity and high-stability reconstituted camellia oil requires overcoming the first technical hurdle: extracting high-quality raw material substrates. Take gamma-linolenic acid (GLA) as an example; its main sources are evening primrose and borage. Traditional processes often employ chemical solvents such as hexane for extraction. This not only carries the risk of solvent residue but also exposes the highly unstable GLA to cis-trans isomerization or polymerization during the unavoidable high temperatures of extraction and drying, reducing its bioactivity. Utilizing supercritical fluid extraction combined with precise low-temperature physical enrichment techniques presents a significant technical challenge in this field.
[0008] Furthermore, while simple lipid remodeling can improve physiological functions, synergistic effects are still needed for visual appeal and long-lasting hydration. The human sebum membrane is not solely composed of triglycerides; it also contains key components such as squalene and ceramides. Ceramides, acting as the "cement" in the "brick-and-mortar structure" of the skin's stratum corneum, are crucial for filling intercellular gaps and smoothing fine lines. Traditional plant oils often cannot perfectly miscible with solid or semi-solid ceramide-like lipids, easily leading to crystal precipitation during storage and affecting skin feel. Squalane, as a highly stable saturated alkane, provides a good smooth feel, but without special nano-sizing or shearing processes, it is difficult to form a uniform, multi-scale diffuse distribution in the lipid system, hindering precise filling of fine wrinkles and gaps.
[0009] In terms of physical processing techniques, current skincare oil preparation largely relies on conventional stirring. This macroscopic kinetic approach struggles to break down the non-covalent bonds between oil molecules, resulting in a wide oil particle size distribution. Larger oil particles remain only on the skin's surface, unable to penetrate the granular layer to exert their biochemical corrective effects. Introducing high-frequency acoustic fields and high-shear technology, using microjets generated by localized extreme pressure changes, forcibly compresses reconstructed lipids, squalane, ceramide-like lipids, and antioxidant systems to the nanoscale, represents a cutting-edge trend in enhancing product penetration and long-term stability.
[0010] In summary, the market and technology sectors urgently need a novel skincare oil solution that can address the functional deficiencies of camellia oil at the molecular structure level, simultaneously overcome the oxidation bottleneck of highly active polyunsaturated fatty acids, and achieve a closed loop of physical filling and biological repair. This invention addresses these complex industrial challenges by proposing a comprehensive process innovation that integrates "directional extraction, enzymatic reconstruction, multidimensional compounding, and acoustic conversion" to improve skin hydration and fine lines in camellia oil preparation, filling a technological gap in the high-end green skincare field. Summary of the Invention
[0011] The purpose of this invention is to provide a camellia oil that improves skin hydration and fine lines, and its preparation method. This invention obtains high-purity γ-linolenic acid through a precise raw material enrichment process, utilizes a bio-enzymatic directed transesterification technique to surgically reconstruct camellia oil molecules, and supplements this with physical synergy and acoustic nano-locking of functional lipid components.
[0012] To achieve the purpose of this invention, the technical solution adopted is as follows: A camellia oil for improving skin hydration and fine lines, comprising, by weight, the following components: 120-150 parts refined camellia oil, 35-45 parts γ-linolenic acid, 8-12 parts immobilized lipase, 20-30 parts plant-derived squalane, 5-10 parts ceramide-like lipids, and 1.5-2.5 parts natural complex antioxidants; wherein the preparation process of the γ-linolenic acid includes the following steps: S1 selects evening primrose seeds with a moisture content of 5-7%, and uses an ultra-micro pulverizer to perform closed-circuit pulverization in the active ingredient protection chamber, controlling the pulverization temperature at 15-25℃, and the material passes through a 40-60 mesh sieve to increase the contact area of supercritical extraction and prevent unsaturated fatty acids from oxidizing at high temperatures. S2 loads the pretreated material into the extraction vessel, uses CO2 as the extraction medium, sets the extraction pressure to 32~35MPa, the extraction temperature to 40~45℃, and the fluid flow rate to 25~30 L per hour; the primary product is collected through a secondary analysis system at a pressure of 6~12MPa. S3 mixes the initial product with a sodium hydroxide-ethanol mixed solution of 15-20% by weight at a weight ratio of 1:3-3.2, and reacts in a stirred tank under nitrogen protection at 60-65°C and 300-400 rpm for 2.5-3 hours. The triglycerides are completely converted into free sodium fatty acid salts in a strongly alkaline environment, laying the foundation for subsequent chain segment screening. S4 adds 10-12% (w / w) dilute sulfuric acid dropwise to the saponified system, controlling the dropping rate to lower the pH of the system to 2-3. At this point, the sodium fatty acid salt is converted into free fatty acid and precipitates on the surface. The system is then rinsed with deionized water until the washing liquid is neutral. The crude product of mixed free fatty acids is obtained by centrifugation and dehydrated under reduced pressure at 35-45℃ and a vacuum degree of -0.1 to -0.095 MPa. S5 involves compounding urea, mixed fatty acids, and ethanol in a weight ratio of 4-5:1:11-12, heating to 75-80℃ to completely dissolve the urea, cooling to 20-25℃ at a rate of 1.8-2℃ per minute, then switching to a cooling rate of 0.5-0.6℃ per minute to -12--14℃, and allowing it to stand at a constant temperature for 14-24 hours. The saturated fatty acids are physically captured by urea crystallization, and the unencapsulated mother liquor is filtered out. After the mother liquor containing urea is recycled to ethanol, it is sent to a two-stage molecular distillation apparatus. The temperature of the inner wall of the distillation chamber is set at 148~152℃, and the residual pressure of the system is controlled at an ultra-high vacuum state of 0.1~0.3 Pa. Taking advantage of the extremely small difference in the mean free path of the heavy and light components, the γ-linolenic acid fraction is accurately extracted on the condenser plate.
[0013] According to a camellia oil that improves skin hydration and fine lines, the immobilized lipase is one or more of Rhizopus oryzae lipase, Candida antarcticus lipase, and thermophilic fungal lipase.
[0014] According to a camellia oil that improves skin hydration and fine lines, the plant-derived squalane is extracted from one or more of olive, sugarcane, rice bran oil, and rapeseed oil.
[0015] According to a camellia oil that improves skin hydration and fine lines, the ceramide-like lipid is one or more of hydroxypropyl dipalmitamide, hexadecyl-PG hydroxyethylhexadecamide, and sodium stearoyl lactylate.
[0016] According to a camellia oil that improves skin hydration and fine lines, the natural complex antioxidant is one or more of the following: natural mixed tocopherols, rosemary extract, and bisabolol.
[0017] According to a camellia oil for improving skin hydration and fine lines, the preparation of the camellia oil for improving skin hydration and fine lines consists of the following steps: S7. Add refined camellia oil and γ-linolenic acid to the reactor according to the weight proportions. Turn on the vacuum pump to maintain the vacuum degree of the system at -0.09~-0.1 MPa. Stir at 150~250 rpm at 65~75℃ for 40~60 minutes. Reduce the water content of the system to below 0.05% through thermodynamic dehydration to create an anhydrous reaction environment. S8 lowers the system temperature to 55-65℃, introduces high-purity nitrogen for protection, and adds immobilized lipase; under the influence of nitrogen flow, a normal pressure transesterification reaction is carried out for 12-24 hours. Utilizing the selective catalytic function of the immobilized lipase, the γ-linolenic acid is driven to undergo a position-specific exchange with the triglyceride skeleton in refined camellia oil to construct a structural lipid intermediate. After the S9 reaction is completed, the oil is filtered while hot using a precision stainless steel filter element with a pore size of 5~10μm to recover the immobilized lipase for recycling, thus obtaining the primary filtered reconstituted oil. The primary filtered reconstituted oil is then sent to a molecular distillation apparatus for fractionation. The distillation temperature is set at 180~220℃ and the vacuum degree is 0.5~5 Pa. The free oleic acid generated in the reaction and the unreacted γ-linolenic acid are removed by utilizing the difference in the mean free path of molecules, thus obtaining the reconstituted camellia oil core matrix. S10 cools the reconstructed camellia oil core matrix to 45~50℃, and adds plant-derived squalane, ceramide-like lipids and natural complex antioxidants in parts by weight in sequence; starts the high-shear emulsification device, and circulates and shears for 20~40 minutes at a speed of 8000~12000 rpm to promote the full dissolution of ceramide-like lipids and form a molecular-level dispersed distribution in the reconstructed oil matrix; S11 transfers the compounded liquid into a high-frequency energy processing chamber, operating at a frequency of 40–60 kHz and a power density of 1.8–2.5 W / cm². 2 The material is treated under an acoustic field for 15-30 minutes. During this process, the system is circulated and cooled to maintain the material temperature at 30-35°C. The local microjets generated by acoustic cavitation effect are used to eliminate non-covalent aggregation between lipid molecules, and finally camellia oil with a median particle size of 120-180 nm and stable properties is obtained to improve skin moisture and fine lines.
[0018] (1) It achieves precise "component reconstruction" at the molecular level, breaking the limitations of traditional compound oils: This invention is not a simple physical mixing of oils, but utilizes immobilized lipases with 1,3-position selectivity to convert evening primrose oils into lipases through enzymatic transesterification technology. -Glinolenic acid (GLA) is precisely grafted onto specific sites on the triglyceride backbone of camellia oil. This reconstruction technology not only retains the advantages of camellia oil's high permeability and high skin affinity, but also endows it with powerful barrier repair functions, enabling a single oil to possess multiple physiological activities, and solving the technical pain points of traditional compound oils such as easy layering, uneven absorption, and sticky skin feel.
[0019] (2) Extremely high purity bioactive substrate extraction ensures the lower limit of product efficacy: This invention uses a precise process, combining supercritical CO2 extraction, directional saponification, and gradient temperature-controlled urea inclusion balance technology, to ensure the extraction of key components. - The purity of linolenic acid has been increased to over 85%. This process strictly controls temperature and oxygen content throughout the entire process, maximizing the preservation of the bioactivity of unsaturated fatty acids. This provides a high-quality molecular substrate for subsequent structural remodeling, ensuring the product's definitive effect in improving fine lines.
[0020] (3) A dual wrinkle-reducing mechanism of "physical filling + biological repair" is constructed: This invention integrates multiple functional components through scientific formulation. Plant-derived squalane utilizes its low surface tension properties to instantly diffuse and physically fill tiny dry lines in the skin. Reconstructed camellia oil triglycerides can release γ-linolenic acid, inhibiting micro-inflammation at the cellular level; at the same time, ceramide-like lipids synergistically repair the "brick wall structure" of the stratum corneum, lock in moisture, and alleviate fine lines caused by dehydration from the root.
[0021] (4) A multi-dimensional synergistic antioxidant system was adopted to overcome the problem of easy deterioration of highly active oils: In response to the highly oxidizable nature of γ-linolenic acid, this invention designed a composite antioxidant system composed of natural mixed tocopherols, rosemary extract, bisabolol, etc. This system utilizes the redox cascade effect to not only protect the integrity of unsaturated bonds during processing, but also improve the chemical stability of the product during shelf life and after application, ensuring that the product has no rancid odor and no irritating peroxides are generated.
[0022] (5) The introduction of acoustic field nano-locking technology has achieved excellent penetration and skin feel: Through high-frequency acoustic field treatment, the local micro-jets generated by acoustic cavitation effect are used to break down the lipid molecular aggregates in the system, so that the particle size of the final product is precisely controlled at 120~180 nm. This nanoscale dispersion distribution significantly improves the transdermal absorption efficiency of oil, so that the product can quickly penetrate into the subcutaneous layer after application, achieving a high-end skin feel experience of "oily but not greasy, and instantly absorbed". Detailed Implementation Example
[0023] Evening primrose seeds with a moisture content of 5% were selected and pulverized in a closed-circuit ultrafine pulverizer within an active ingredient protection chamber. The pulverization temperature was controlled at 15℃, and the material was passed through a 40-mesh sieve to increase the contact area for supercritical extraction and prevent the oxidation of unsaturated fatty acids at high temperatures. The pretreated material was then loaded into an extraction vessel, using CO2 as the extraction medium. The extraction pressure was set at 32 MPa, the extraction temperature at 40℃, and the fluid flow rate at 25 L / h. The initial product was collected using a secondary analytical system at a pressure of 6 MPa. The initial product was mixed with a 15% sodium hydroxide-ethanol solution at a weight ratio of 1:3 and reacted in a nitrogen-protected stirred tank at 60℃ and 300 rpm for 2.5 hours. The strong alkaline environment completely converted the triglycerides into free sodium fatty acid salts, laying the foundation for subsequent chain segment screening. A 10% dilute sulfuric acid solution was added dropwise to the saponified system, controlling the dropping rate to lower the pH of the system to 2. Sodium fatty acid salts are converted into free fatty acids and precipitate on the surface. The mixture is washed with deionized water until the washing liquid is neutral, and then centrifuged to obtain crude mixed free fatty acids. This is then subjected to decompression dehydration at 35°C and a vacuum of -0.1 MPa. Urea, mixed fatty acids, and ethanol are compounded in a weight ratio of 4:1:11, and the temperature is raised to 75°C to completely dissolve the urea. The temperature is then lowered to 20°C at a rate of 1.8°C per minute, followed by a decrease to -12°C at a rate of 0.5°C per minute. The mixture is then allowed to stand at a constant temperature for 14 hours. Urea crystallization is used to physically capture the saturated fatty acids, and the unencapsulated mother liquor is filtered out. The urea-encapsulated mother liquor is then treated with ethanol recovery and sent to a two-stage molecular distillation apparatus. The distillation chamber wall temperature is set at 148°C, and the system residual pressure is controlled at an ultra-high vacuum of 0.1 Pa. Utilizing the extremely small difference in the mean free path of the heavy and light components, the γ-linolenic acid fraction is precisely extracted on a condenser plate. Example
[0024] Evening primrose seeds with a moisture content of 6% were selected and pulverized in a closed-circuit ultrafine pulverizer within an active ingredient protection chamber. The pulverization temperature was controlled at 20°C, and the material was passed through a 50-mesh sieve to increase the contact area for supercritical extraction and prevent the oxidation of unsaturated fatty acids at high temperatures. The pretreated material was then loaded into an extraction vessel, using CO2 as the extraction medium. The extraction pressure was set at 33 MPa, the extraction temperature at 43°C, and the fluid flow rate controlled at 28 L per hour. The material was then processed through a secondary analytical system at a pressure of 9... The initial product was collected at MPa; the initial product was mixed with an 18% sodium hydroxide-ethanol solution at a weight ratio of 1:3.1, and reacted in a stirred tank under nitrogen protection at 62°C and 350 rpm for 2.7 hours; the triglycerides were completely converted into free sodium fatty acid salts in a strongly alkaline environment, laying the foundation for subsequent chain segment screening; 11% dilute sulfuric acid was added dropwise to the saponified system, and the pH of the system was controlled to drop to 2.5, at which point the sodium fatty acid salts were converted into free fatty acids and precipitated on the surface; the mixture was washed with deionized water until the washing liquid was neutral, and the crude product of mixed free fatty acids was obtained by centrifugation and subjected to reduced pressure at 40°C and -0.1 MPa. Dehydration; urea, mixed fatty acids, and ethanol were compounded in a weight ratio of 4:1:12, and the mixture was heated to 77°C to completely dissolve the urea; the temperature was then lowered to 22°C at a rate of 1.9°C per minute, followed by a decrease to -13°C at a rate of 0.5°C per minute, and allowed to stand at a constant temperature for 19 hours. The urea crystals were used to physically capture the saturated fatty acids, and the unencapsulated mother liquor was filtered off; the urea-encapsulated mother liquor was treated with ethanol recovery and then sent to a two-stage molecular distillation apparatus. The distillation chamber wall temperature was set at 150°C, and the system residual pressure was controlled at an ultra-high vacuum of 0.2 Pa; the γ-linolenic acid fraction was precisely extracted on a condenser plate by utilizing the extremely small difference in the mean free path of the heavy and light components. Example
[0025] Evening primrose seeds with a moisture content of 7% were selected and pulverized in a closed-circuit ultrafine pulverizer within an active ingredient protection chamber. The pulverization temperature was controlled at 25℃, and the material was passed through a 60-mesh sieve to increase the contact area for supercritical extraction and prevent the oxidation of unsaturated fatty acids at high temperatures. The pretreated material was then loaded into an extraction vessel, using CO2 as the extraction medium. The extraction pressure was set at 35 MPa, the extraction temperature at 45℃, and the fluid flow rate was controlled at 30 L per hour. The primary product was collected using a secondary desorption system at a pressure of 12 MPa. The primary product was mixed with a 20% sodium hydroxide-ethanol mixed solution at a weight ratio of 1:3.2 and extracted in a stirred tank under nitrogen protection at 65℃ and 400 °C. The reaction was carried out at a rotation speed of rpm for 3 hours. Triglycerides were completely converted into free sodium fatty acid salts in a strongly alkaline environment, laying the foundation for subsequent chain segment screening. 12% sulfuric acid was added dropwise to the saponified system, controlling the dropping rate to lower the pH to 3. At this point, the sodium fatty acid salts were converted into free fatty acids and precipitated on the surface. The system was washed with deionized water until the washing liquid was neutral. A crude mixed free fatty acid product was obtained by centrifugation and dehydrated under reduced pressure at 45℃ and a vacuum degree of -0.095 MPa. Urea, mixed fatty acids, and ethanol were mixed at a weight ratio of 5:1: The mixture was compounded in a 1:2 ratio and heated to 75-80℃ to completely dissolve the urea. The temperature was then lowered to 25℃ at a rate of 2℃ per minute, followed by a rate of 0.6℃ per minute to -14℃. The mixture was then left to stand at a constant temperature for 24 hours. Urea crystals were used to physically capture saturated fatty acids, and the unencapsulated mother liquor was filtered out. The mother liquor containing urea was then treated with ethanol and sent to a two-stage molecular distillation apparatus. The temperature of the inner wall of the distillation chamber was set at 152℃, and the residual pressure of the system was controlled at an ultra-high vacuum of 0.3 Pa. The γ-linolenic acid fraction was precisely extracted on the condenser plate by utilizing the extremely small difference in the mean free path of the heavy and light components. Example
[0026] Refined camellia oil and γ-linolenic acid prepared in Example 1 were added to a reaction vessel according to the specified weight proportions. A vacuum pump was turned on to maintain the system vacuum at -0.09 MPa. The mixture was stirred at 150 rpm for 40 minutes at 65°C. The water content of the system was reduced to below 0.05% through thermodynamic dehydration to create an anhydrous reaction environment. The system temperature was then lowered to 55°C, and high-purity nitrogen was introduced for protection. Immobilized lipase was added. An atmospheric pressure transesterification reaction was carried out under nitrogen flow for 12 hours. The selective catalytic function of the immobilized lipase drove the position-specific exchange of γ-linolenic acid with the triglyceride backbone in the refined camellia oil, constructing a structural lipid intermediate. After the reaction, the mixture was filtered hot using a precision stainless steel filter with a pore size of 5 μm to recover the immobilized lipase for recycling, obtaining the primary filtered reconstituted oil. The primary filtered reconstituted oil was then sent to a molecular distillation apparatus for further processing. The process involved fractionation, with distillation at 180℃ and a vacuum of 0.5 Pa. Free oleic acid and unreacted γ-linolenic acid generated during the reaction were removed using differences in the mean free path of molecules, yielding a reconstructed camellia oil core matrix. The reconstructed camellia oil core matrix was cooled to 45℃, and plant-derived squalane, ceramide-like lipids, and a natural complex antioxidant were added sequentially by weight. A high-shear emulsification device was activated, and the mixture was circulated and sheared at 8000 rpm for 20 minutes to ensure complete dissolution of the ceramide-like lipids and their molecular-level dispersion within the reconstructed oil matrix. The compounded liquid was then transferred to a high-frequency energy processing chamber and processed at a frequency of 40 kHz and a power density of 1.8 W / cm². 2 The material was treated under an acoustic field for 15 minutes. During this process, the system was circulated and cooled to maintain the material temperature at 30°C. The local microjets generated by acoustic cavitation effect were used to eliminate non-covalent aggregation between lipid molecules, and camellia oil with a median particle size of 120 nm and stable properties was finally obtained to improve skin moisture and fine lines. Example
[0027] Refined camellia oil and γ-linolenic acid prepared in Example 2 were added to a reaction vessel according to the specified weight proportions. The vacuum pump was turned on to maintain the system vacuum at -0.09 MPa. The mixture was stirred at 200 rpm for 50 minutes at 70°C. The water content of the system was reduced to below 0.05% through thermodynamic dehydration to create an anhydrous reaction environment. The system temperature was then lowered to 60°C, and high-purity nitrogen gas was introduced for protection. Immobilized lipase was added. An atmospheric pressure transesterification reaction was carried out under nitrogen flow for 18 hours. The selective catalytic function of the immobilized lipase was used to drive the position-specific exchange of γ-linolenic acid with the triglyceride skeleton in refined camellia oil to construct a structural lipid intermediate. After the reaction was completed, the mixture was filtered while hot using a precision stainless steel filter with a pore size of 7 μm. The immobilized lipase was filtered and recovered for recycling to obtain the primary filtered reconstituted oil. This oil was then sent to a molecular distillation apparatus for fractionation. The distillation temperature was set at 200℃ and the vacuum degree at 2.5 Pa. Free oleic acid and unreacted γ-linolenic acid generated during the reaction were removed using the difference in the mean free path of molecules, yielding the reconstituted camellia oil core matrix. The reconstituted camellia oil core matrix was cooled to 47℃, and plant-derived squalane, ceramide-like lipids, and natural complex antioxidants were added sequentially by weight. A high-shear emulsification device was activated, and the mixture was circulated and sheared at 10,000 rpm for 30 minutes to ensure complete dissolution of the ceramide-like lipids and their molecular-level dispersion within the reconstituted oil matrix. The compounded liquid was then transferred to a high-frequency energy processing chamber and processed at a frequency of 50 kHz and a power density of 2.2 W / cm². 2 The material was treated under an acoustic field for 25 minutes. During this process, the system was circulated and cooled to maintain the material temperature at 33°C. The local microjets generated by acoustic cavitation effect were used to eliminate non-covalent aggregation between lipid molecules, and camellia oil with a median particle size of 150nm and stable properties was finally obtained to improve skin moisture and fine lines. Example
[0028] Refined camellia oil and γ-linolenic acid prepared in Example 3 were added to a reaction vessel according to the specified weight proportions. The vacuum pump was turned on to maintain the system vacuum at -0.1 MPa. The mixture was stirred at 250 rpm for 60 minutes at 75°C. The water content of the system was reduced to below 0.05% through thermodynamic dehydration to create an anhydrous reaction environment. The system temperature was then lowered to 65°C, and high-purity nitrogen gas was introduced for protection. Immobilized lipase was added. An atmospheric pressure transesterification reaction was carried out under nitrogen gas flow for 24 hours. The selective catalytic function of the immobilized lipase was used to drive the position-specific exchange of γ-linolenic acid with the triglyceride skeleton in the refined camellia oil, constructing a structural lipid intermediate. After the reaction was completed, the mixture was filtered while hot using a precision stainless steel filter with a pore size of 10 μm to recover the immobilized lipase for recycling, obtaining the primary filtered reconstituted oil. The primary filtered reconstituted oil was sent to a molecular distillation apparatus for fractionation. The distillation temperature was set to 220°C and the vacuum degree to 5. Pa, utilizing the difference in the mean free path of molecules, removes free oleic acid and unreacted γ-linolenic acid generated in the reaction to obtain a reconstructed camellia oil core matrix. The reconstructed camellia oil core matrix is cooled to 50°C, and plant-derived squalane, ceramide-like lipids, and natural complex antioxidants are added sequentially by weight. A high-shear emulsification device is activated, and cyclic shearing is performed at 12000 rpm for 40 minutes to promote the complete dissolution of ceramide-like lipids and their molecular-level dispersion in the reconstructed oil matrix. The compounded liquid is then transferred to a high-frequency energy processing chamber and subjected to high-frequency processing at 60 kHz and a power density of 2.5 W / cm². 2 The material was treated under an acoustic field for 30 minutes. During this process, the system was circulated and cooled to maintain the material temperature at 35°C. The local microjets generated by acoustic cavitation effect were used to eliminate non-covalent aggregation between lipid molecules, and camellia oil with a median particle size of 180 nm and stable properties was finally obtained to improve skin moisture and fine lines. Example
[0029] To verify the effectiveness of the preparation processes described in Examples 4, 5, and 6 in achieving precise component reconstruction at the molecular level, and to verify their technical advantages compared to traditional compound oils, an experiment was conducted to compare performance and structure. First, carbon-13 nuclear magnetic resonance spectroscopy was used to test the fatty acid distribution at the sn-1 and sn-3 sites of the triglyceride skeleton in the finished products and compound groups obtained in Examples 4, 5, and 6. The spectral analysis results showed that, due to the absence of enzyme-catalyzed site-specific exchange in the compound oils, the effective grafting rate of gamma-linolenic acid on the glycerol skeleton was close to 0, and a large number of disordered signal peaks representing free fatty acids were present in the 175 region. In contrast, the directional substitution rates of gamma-linolenic acid at the sn-1 and sn-3 sites in the samples of Examples 4, 5, and 6 reached 20.5%, 22.8%, and 24.1%, respectively, and the signal intensity representing oleic acid at the sn-2 site remained highly stable. The test data definitively proves that the process of this invention achieves directional substitution of molecular sites through immobilized lipase. In the physical stability test, the thermodynamic stability of the four groups of samples was continuously observed in a 0°C freezer. After standing for 18 hours, the compound oil showed white crystalline precipitates at the bottom of the container due to the precipitation of ceramide-like lipids, and the overall transparency of the oil decreased by 45% due to component stratification. In contrast, the samples of Examples 4, 5, and 6 remained clear and transparent after standing in the freezer for 168 hours, and their transmittance was greater than 98.5% as measured by spectrophotometer, proving that the lipid system after molecular structure reconstruction has excellent endogenous compatibility. Next, an in vitro penetration experiment was conducted on pig skin. The penetration of Nile Red fluorescently labeled oil was observed using a confocal microscope. The average penetration depth of the compound oil was only 18.2 micrometers after 30 minutes of application, with most of the oil accumulating on the surface of the stratum corneum. The penetration depths of Examples 4, 5, and 6 reached 58.6 micrometers, 65.4 micrometers, and 68.1 micrometers, respectively, with Example 6 showing stronger deep penetration, proving that the reconstructed molecular structure can more easily penetrate the human sebum barrier. Finally, 45 subjects with facial fine lines were selected and divided into three groups for a 28-day human efficacy evaluation. Test results showed that subjects using the oil prepared in Example 5 experienced an average increase of 54.8% in the stratum corneum moisture content and an average decrease of 39.2% in transepidermal water loss. The depth of fine lines around the eyes, measured by a three-dimensional skin imaging system, decreased by an average of 28.4%. In contrast, the control subjects using the compound oil showed improvements of only 13.6%, 10.5%, and 8.2% in the corresponding indicators. Furthermore, sensory evaluation feedback showed that subjects rated the absorption speed and smoothness of Examples 4, 5, and 6 at over 9.2 points, while the compound group, due to its higher content of free unsaturated fatty acids and uneven molecular weight distribution, only scored 4.5 points for skin greasiness.In summary, the above test data, through comparison of four dimensions—molecular localization, thermodynamic stability, permeation kinetics, and human efficacy indicators—quantitatively demonstrate that Examples 4, 5, and 6, through precise structural reconstruction, have completely overcome the industrial limitations of traditional compound oils, such as weak efficacy, poor penetration, and poor compatibility. Example
[0030] To ensure the efficacy limit of the products by leveraging the high-purity bioactive substrates extracted through precise processes in Examples 4, 5, and 6, Example 8 was designed for comparative verification and analysis. First, gas chromatography-mass spectrometry was used to compare the purity and component indicators of the gamma-linolenic acid substrates prepared in Examples 1, 2, and 3 with those of commercially available evening primrose oil obtained by conventional solvent extraction. The experimental results showed that the gamma-linolenic acid content in commercially available evening primrose oil was only 9.4%, accompanied by 12.5% saturated fatty acid impurities; while the purity of gamma-linolenic acid in the active substrates prepared in Examples 1, 2, and 3 of this invention reached 88.6%, 90.4%, and 92.1%, respectively, effectively removing inactive saturated lipid chains. Meanwhile, the peroxide value was detected by chemical titration. The peroxide value of commercially available evening primrose oil was 4.25 mmol / kg, while the peroxide value of the substrates subjected to the low-temperature closed-circuit pulverization and molecular distillation processes S1 to S6 of this invention was maintained between 0.35 and 0.48 mmol / kg. The extremely low initial oxidation rate laid the molecular foundation for the stability and efficacy limit of the subsequent products.
[0031] Subsequently, a lower limit bioactivity test based on a human keratinocyte model was conducted to quantify the synergistic effect of high-purity substrates on cell barrier function. The experiment divided the test samples into a low-purity substrate group (using commercially available oil) and a high-purity substrate group (using the finished products from Examples 4, 5, and 6, respectively). The active ingredient in each group was diluted to an extremely low mass fraction of 0.05% to simulate the performance of cosmetics at low doses. The concentration of prostaglandin E2 released by cells after UV irradiation was determined by enzyme-linked immunosorbent assay (ELISA). The test data showed that the prostaglandin E2 concentration in the untreated irradiated group was 792.5 picograms per milliliter, while the concentration in the low-purity substrate group was 684.2 picograms per milliliter, indicating a very weak anti-inflammatory protective effect. In contrast, the high-purity substrate groups (Examples 4, 5, and 6) showed a very strong lower limit protection, with prostaglandin E2 concentrations sharply reduced to 205.4 picograms, 188.6 picograms, and 172.3 picograms per milliliter, respectively. This indicates that, due to the high concentration of active molecules in the substrate, the camellia oil prepared by this invention can still cross the efficacy threshold and maintain a highly efficient biological response, even under extremely low loading conditions.
[0032] Finally, a lower limit stability assessment of clinical moisturizing and fine line repair was conducted. Forty-five subjects were recruited and randomly divided into three groups. Only 0.1 ml of a small amount of oil was applied to a localized area of the subjects' faces daily. Skin parameters were monitored after 14 days of continuous use using a stratum corneum moisture analyzer and a transepidermal water loss meter. The results showed that even at extremely low doses, subjects using products from Examples 4, 5, and 6 experienced an average increase in stratum corneum moisture content of 42.4%, 46.8%, and 51.2%, respectively, and an average decrease in transepidermal water loss of 28.6%, 32.5%, and 36.4%, respectively. In contrast, the control group using traditional low-purity compound oils showed only an 8.5% increase in moisture content and less than 5% improvement in water loss at the same low dose, with no statistically significant difference in fine line depth observed in visual assessment and instrument scanning. The aforementioned closed-loop data regarding substrate purity, oxidative stability, cellular inflammatory feedback, and low-dose human testing fully demonstrates that the extremely high-purity bioactive substrates obtained by the present invention through processes S1 to S6 ensure, at the molecular level, that oil products possess an extremely high efficacy baseline in practical applications. By utilizing the unit volume load of high-concentration active molecules, the invention completely breaks through the technical limitation of rapid efficacy decay of traditional low-purity substrates after product dilution. Example
[0033] To verify the significant effect of the multidimensional synergistic antioxidant system used in Examples 4, 5, and 6 in overcoming the problem of easy deterioration of highly active oils, Example 8 was designed to conduct a comparative test on the oxidative stability of oils. The experiment included four sample groups: Experimental Group A (using the finished product prepared in Example 4), Experimental Group B (using the finished product prepared in Example 5), Experimental Group C (using the finished product prepared in Example 6), and a control group (using the reconstructed oil matrix from Example 5, but without the addition of natural composite antioxidants). First, an accelerated oxidation experiment was conducted in an oven. Following the Saab method, the four groups of samples were placed in a 60°C constant-temperature incubator for continuous aging testing. Samples were taken every 5 days to measure their peroxide value and acid value. At the initial stage of the experiment, day 0, the peroxide values of all four groups of samples were at extremely low levels, ranging from 0.32 to 0.45 mmol / kg. After 30 days of continuous high-temperature aging, the control group oil, due to its high proportion of unsaturated gamma-linolenic acid bonds and lack of protection, experienced a rapid increase in its peroxide value to 68.4 mmol / kg, accompanied by a strong rancid odor, and its color changed from golden yellow to dark brown upon visual inspection. In contrast, experimental groups A, B, and C, which incorporated a multidimensional synergistic antioxidant system composed of natural mixed tocopherols, rosemary extract, and bisabolol, showed peroxide values of only 2.15 mmol / kg, 1.82 mmol / kg, and 1.54 mmol / kg, respectively, after 30 days, far below the industry safety threshold of 10 mmol / kg. Furthermore, the oils exhibited a clean odor and no significant color shift. Next, a pressure oxidation test was conducted using a lipid oxidation induction instrument, measuring the oxidation induction time of the samples under extreme conditions of 110 degrees Celsius and an air flow rate of 20 liters per hour. The test data showed that the oxidation induction time of the control group was only 1.84 hours, demonstrating its high susceptibility to chain reactions when heated or exposed to oxygen. The oxidation induction times of experimental groups A, B, and C were extended to 16.52 hours, 18.84 hours, and 20.45 hours, respectively, with experimental group C showing an antioxidant stability that was more than 11 times higher than the control group. Calculation of the synergistic effect index revealed that the combined antioxidant was significantly more effective than the control sample with only 2.5 parts of tocopherol, demonstrating a molecular-level synergistic mechanism involving tocopherol scavenging free radicals, rosemary extract blocking chain reaction initiation, and bisabolol enhancing the system's chemical potential. Finally, gas chromatography was used to detect the retention rate of gamma-linolenic acid in the system after 30 days of high-temperature aging. The results showed that the loss of active ingredients in the control group was as high as 42.6%, while the retention rates of active ingredients in experimental groups A, B, and C were all above 98.2%. The closed-loop test data from the three dimensions of peroxide value, oxidation induction time, and residual active ingredients fully demonstrate that the multi-dimensional synergistic antioxidant system adopted in this invention successfully solves the industrial defect of easily oxidized highly active unsaturated fatty acids in reconstructed camellia oil, perfectly overcoming the problem of easily deteriorating highly active oils while ensuring the long-term shelf-life stability of the product.
[0034] Please note to all technical personnel: Although the present invention has been described according to the specific embodiments above, the inventive concept of the present invention is not limited to this invention.
Claims
1. A camellia oil that improves skin hydration and reduces fine lines, characterized in that, By weight, the camellia oil for improving skin hydration and fine lines comprises the following components: 120-150 parts refined camellia oil, 35-45 parts γ-linolenic acid, 8-12 parts immobilized lipase, 20-30 parts plant-derived squalane, 5-10 parts ceramide-like lipids, and 1.5-2.5 parts natural complex antioxidants; wherein, the preparation process of the γ-linolenic acid includes the following steps: S1 selects evening primrose seeds with a moisture content of 5-7%, and uses an ultra-micro pulverizer to perform closed-circuit pulverization in the active ingredient protection chamber, controlling the pulverization temperature at 15-25℃, and the material passes through a 40-60 mesh sieve to increase the contact area of supercritical extraction and prevent unsaturated fatty acids from oxidizing at high temperatures. S2 loads the pretreated material into the extraction vessel, uses CO2 as the extraction medium, sets the extraction pressure to 32~35 MPa, the extraction temperature to 40~45℃, and the fluid flow rate to 25~30 L per hour; the primary product is collected through a secondary analysis system at a pressure of 6~12 MPa. S3 mixes the initial product with a sodium hydroxide-ethanol mixed solution of 15-20% by weight at a weight ratio of 1:3-3.2, and reacts in a stirred tank under nitrogen protection at 60-65°C and 300-400 rpm for 2.5-3 hours. The triglycerides are completely converted into free sodium fatty acid salts in a strongly alkaline environment, laying the foundation for subsequent chain segment screening. S4 adds 10-12% (w / w) dilute sulfuric acid dropwise to the saponified system, controlling the dropping rate to lower the pH of the system to 2-3. At this point, the sodium fatty acid salt is converted into free fatty acid and precipitates on the surface. The system is then rinsed with deionized water until the washing liquid is neutral. The crude product of mixed free fatty acids is obtained by centrifugation and dehydrated under reduced pressure at 35-45℃ and a vacuum degree of -0.1 to -0.095 MPa. S5 involves compounding urea, mixed fatty acids, and ethanol in a weight ratio of 4-5:1:11-12, heating to 75-80℃ to completely dissolve the urea, cooling to 20-25℃ at a rate of 1.8-2℃ per minute, then switching to a cooling rate of 0.5-0.6℃ per minute to -12--14℃, and allowing it to stand at a constant temperature for 14-24 hours. The saturated fatty acids are physically captured by urea crystallization, and the unencapsulated mother liquor is filtered out. After the mother liquor containing urea is recycled to ethanol, it is sent to a two-stage molecular distillation apparatus. The temperature of the inner wall of the distillation chamber is set at 148~152℃, and the residual pressure of the system is controlled at an ultra-high vacuum state of 0.1~0.3 Pa. Taking advantage of the extremely small difference in the mean free path of the heavy and light components, the γ-linolenic acid fraction is accurately extracted on the condenser plate.
2. The camellia oil for improving skin moisture and fine lines as described in claim 1, characterized in that, The immobilized lipase is one or more of the following: Rhizopus niger lipase, Candida antarcticis lipase, and thermophilic fungal lipase.
3. The camellia oil for improving skin hydration and fine lines as described in claim 1, characterized in that, The plant-derived squalane is extracted from one or more of olive, sugarcane, rice bran oil, and rapeseed oil.
4. The camellia oil as described in claim 1 for improving skin moisture and fine lines, characterized in that, The ceramide-like lipid is one or more of hydroxypropyl bispalmitamide, hexadecyl-PG hydroxyethylhexadecamide, and sodium stearoyl lactylate.
5. The camellia oil for improving skin moisture and fine lines as described in claim 1, characterized in that, The natural complex antioxidant is one or more of the following: natural mixed tocopherols, rosemary extract, and bisabolol.
6. A camellia oil for improving skin moisture and fine lines as described in any one of claims 1 to 5, characterized in that, The preparation of the camellia oil that improves skin hydration and fine lines consists of the following steps: S7. Add refined camellia oil and γ-linolenic acid to the reactor according to the weight proportions. Turn on the vacuum pump to maintain the vacuum degree of the system at -0.09~-0.1 MPa. Stir at 150~250 rpm at 65~75℃ for 40~60 minutes. Reduce the water content of the system to below 0.05% through thermodynamic dehydration to create an anhydrous reaction environment. S8 lowers the system temperature to 55-65℃, introduces high-purity nitrogen for protection, and adds immobilized lipase; under the influence of nitrogen flow, a normal pressure transesterification reaction is carried out for 12-24 hours. Utilizing the selective catalytic function of the immobilized lipase, the γ-linolenic acid is driven to undergo a position-specific exchange with the triglyceride skeleton in refined camellia oil to construct a structural lipid intermediate. After the S9 reaction is completed, the oil is filtered while hot using a precision stainless steel filter element with a pore size of 5~10μm to recover the immobilized lipase for recycling, thus obtaining the primary filtered reconstituted oil. The primary filtered reconstituted oil is then sent to a molecular distillation apparatus for fractionation. The distillation temperature is set at 180~220℃ and the vacuum degree is 0.5~5 Pa. The free oleic acid generated in the reaction and the unreacted γ-linolenic acid are removed by utilizing the difference in the mean free path of molecules, thus obtaining the reconstituted camellia oil core matrix. S10 cools the reconstructed camellia oil core matrix to 45~50℃, and adds plant-derived squalane, ceramide-like lipids and natural complex antioxidants in parts by weight in sequence; starts the high-shear emulsification device, and circulates and shears for 20~40 minutes at a speed of 8000~12000 rpm to promote the full dissolution of ceramide-like lipids and form a molecular-level dispersed distribution in the reconstructed oil matrix; S11 transfers the compounded liquid into a high-frequency energy processing chamber, operating at a frequency of 40–60 kHz and a power density of 1.8–2.5 W / cm². 2 The material is treated under an acoustic field for 15-30 minutes. During this process, the system is circulated and cooled to maintain the material temperature at 30-35°C. The local microjets generated by acoustic cavitation effect are used to eliminate non-covalent aggregation between lipid molecules, and finally camellia oil with a median particle size of 120-180 nm and stable properties is obtained to improve skin moisture and fine lines.