A carrot derivative, a method for preparing the same and use thereof
The preparation of nanoscale carrot derivatives using a microchannel reactor solves the problems of extraction and dispersion of effective carrot components, enabling multifunctional skincare applications. These derivatives possess full-spectrum UV absorption, antioxidant, and moisturizing effects, and meet green and environmentally friendly requirements.
Patent Information
- Application Number
- CN202410062636.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-01-16
- Publication Date
- 2026-08-25
- Estimated Expiration
- 2044-01-16
AI Technical Summary
Existing technologies make it difficult to extract the active ingredients from carrots efficiently and at low cost. Furthermore, beta-carotene is difficult to disperse evenly and maintain its activity in skincare products. Traditional methods are costly, complex, and not environmentally friendly.
Carrot juice was heated using a microchannel reactor. By precisely controlling the reaction conditions, nanoscale carbon-based carrot derivatives were formed, retaining the active ingredients and giving them water solubility and biocompatibility.
The efficient preparation of carrot derivatives has been achieved, which have full-spectrum ultraviolet absorption, antioxidant, whitening and moisturizing functions, are suitable for a variety of skin care products, meet green and environmental protection requirements, and reduce the risk of allergies.
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Figure CN117898985B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of biotechnology, specifically relating to a carrot derivative, its preparation method, and its application. Background Technology
[0002] Carrots, a root vegetable belonging to the Apiaceae family, are renowned for their sweet taste, crisp texture, and rich nutritional value. The most notable characteristic of carrots is their high content of beta-carotene, a powerful antioxidant that can be converted into vitamin A in the body. Vitamin A accelerates skin cell renewal and repair, stimulates collagen production, thus helping to protect the skin from UV rays and free radical damage, improves pigmentation and uneven skin tone, strengthens the skin barrier, and promotes healthy skin. In addition, carrots also contain vitamin C, vitamin K, potassium, various minerals, and fiber, which can help retain moisture in the skin, reduce skin inflammation and redness, and diminish signs of aging.
[0003] Carrots are rich in antioxidants, vitamins, and other nutrients beneficial to skin health, making them a potential candidate in the skincare market. However, applying the active ingredients from carrots to skincare products faces several challenges: First, current methods for extracting active ingredients from carrots, such as water extraction, supercritical fluid extraction, and enzymatic hydrolysis, fail to meet the requirements of low-cost and high-efficiency extraction. Patent CN101779788A discloses a method for extracting carrot nutrients using supercritical CO2, which ensures high extraction efficiency and selectivity, maximizing the preservation of bioactive components. However, this method is costly, requires expensive equipment, is complex to operate, and demands stringent conditions. Secondly, β-carotene in carrots is a hydrophobic compound, making it difficult to disperse evenly in skincare products. To address this issue, patent CN112438950 A discloses a transparent aqueous dispersion of β-carotene and its preparation method. This invention directly melts β-carotene as the oil phase, increasing the β-carotene content in the aqueous dispersion. However, the melting temperature is high (180℃~200℃), and additional emulsifiers or co-emulsifiers are required. This not only makes the product prone to carbonization and aggregation but also affects the stability of subsequent formulations. Finally, ensuring the activity and stability of the active ingredients in carrots throughout the product's lifecycle is also a major challenge in its application. Summary of the Invention
[0004] The present invention aims to solve the above problems and provides a carrot derivative, its preparation method and application. The invention uses a microchannel reactor to realize the continuous preparation of carrot derivative, thereby enabling the multifunctional application of carrot derivative in skin care products.
[0005] According to the technical solution of the present invention, the preparation method of the carrot derivative includes the following steps: S1: Heating the microchannel reactor; S2: Inject carrot juice into a heated microchannel reactor, heat the reaction, and obtain the crude product; S3: The crude product is filtered, dialyzed, and freeze-dried to obtain the carrot derivative.
[0006] This invention utilizes a microchannel reactor to achieve precise control of reaction conditions (temperature, residence time, etc.). The high surface area and volume ratio within the channels promote heat and mass transfer, enabling the efficient preparation of carrot derivatives in a short time while preserving the effective components of carrots to a great extent. The prepared carrot derivatives serve as a safer, more environmentally friendly, and more skin-friendly alternative raw material, meeting the current demand for green, environmentally friendly, and natural skincare ingredients while ensuring efficacy, thus filling a market gap.
[0007] Specifically, the mixture is introduced into a microchannel reactor. Under heating conditions, the complex organic components in the carrot juice decompose into smaller molecules. Sugars and other small organic molecules begin to pyrolyze, while polysaccharides and proteins decompose into smaller compounds. Further, these smaller molecules polymerize and carbonize through various chemical reactions such as dehydration and dehydrogenation (this invention uses a microchannel reactor, which has high mass and heat transfer efficiency, allowing carrot juice to begin carbonization at relatively low temperatures), forming a carbon-based structure. As the reaction proceeds, fragments of some chemical components in the carrot, such as carotenoids, sugars, and amino acids, may be fixed on the surface of the carbon-based structure, giving it higher water solubility and biocompatibility.
[0008] Furthermore, the microchannel reactor is made of stainless steel, glass, aluminum, copper, or nickel tubes, with an inner diameter of 0.25–4 mm and a length of 3–8 m.
[0009] Furthermore, in step S1, the heating temperature is 110~160 ℃, for example, it can be 110 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, etc.
[0010] Furthermore, in step S2, the solid content of the carrot juice is 10-67%, which is a carrot aqueous solution extracted by mixing carrots and water in a certain proportion.
[0011] Furthermore, in step S2, the heating temperature is 110~160 ℃, for example, it can be 110 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, etc.; the reaction time (the residence time in the microchannel reactor) is 5~60 min; for example, it can be 5 min, 10 min, 20 min, 30 min, 40 min, 50 min, 60 min, etc.
[0012] Furthermore, in step S3, the filter head used for filtration has a pore size of 0.22 μm; the molecular weight cutoff for dialysis is 500~3500 Da; the freeze-drying temperature is -50 ℃~-70 ℃, and the time is 1~3 days.
[0013] Specifically, the filtration uses a mixed cellulose (MCE) needle filter with a pore size of 0.22 μm, and the dialysis involves placing the filtered crude product in water (such as distilled water) for dialysis.
[0014] A second aspect of the present invention provides a carrot derivative prepared by the above preparation method, wherein the carrot derivative is a brown powder.
[0015] Compared to traditional carrots, carrot derivatives are nanoscale carbon materials extracted from carrots through efficient and mild chemical reactions, exhibiting higher chemical stability and a longer shelf life. Due to their nanoscale size and surface properties, they can be designed into gentle ingredients that are easily absorbed by the skin and do not easily cause skin irritation (skin-friendly and biocompatible). Carrot derivatives can also be surface functionalized to introduce additional properties, increasing their versatility in cosmetic applications.
[0016] A third aspect of the present invention provides a skin care product comprising the above-mentioned carrot derivative.
[0017] Furthermore, the skincare products mentioned are sunscreens, whitening products, moisturizing products, anti-aging products, or soothing products.
[0018] Specifically, the C=C bond in the carbon core and the surface carbonyl group of the carrot derivative correspond to the π-π* transition and n-π* transition in the ultraviolet spectrum, respectively, giving it full-spectrum ultraviolet absorption characteristics. In particular, it has excellent absorption performance for UVA and UVB light with wavelengths of 280 to 400 nm (blocking rate of over 95% for UVA and over 90% for UVB). It can replace one or more traditional ultraviolet absorbers (such as diphenyl ketone, benzophenone, titanium dioxide, zinc oxide, ethylhexyl triazine ketone (EHT), methylene bis-benzotriazolyl tetramethylbutylphenol (MBBT), bis-ethylhexyloxyphenol methoxyphenyl triazine (BMET), butyl methoxydibenzoylmethane (BMDM), ethylhexyl methoxycinnamate (OMC), octocrylene (OCTO), etc.) in sunscreen products. The carrot derivative has a large number of phenolic hydroxyl groups on its surface functional groups, which have high stability and excellent free radical scavenging ability. It can inhibit the production of tyrosinase and the synthesis of melanocytes (the inhibition rate of tyrosinase is up to 90%, the inhibition rate of melanocyte proliferation is up to 80%, and the inhibition rate of melanocyte synthesis is up to 80%), reduce skin inflammation, thereby reducing and preventing skin pigmentation, brightening skin tone and delaying skin aging. It can be used as a whitening agent in whitening products. The carrot derivative has a variety of hydrophilic functional groups on its surface and has excellent water absorption properties. It can be used as a moisturizer in moisturizing products or replace oily ingredients in the formula to make the product feel refreshing on the skin. The carrot derivative contains β-carotene, an effective antioxidant for neutralizing free radicals (with a scavenging rate of up to 90% for DPPH free radicals, ABTS). + With a free radical scavenging capacity of 75%, a superoxide anion scavenging rate of 70%, and a hydroxyl free radical scavenging rate of 85%, β-carotene can be converted into vitamin A, promoting skin cell renewal and repair, maintaining the integrity of skin structure, and slowing down the aging process. It can be used in anti-aging products.
[0019] Furthermore, when the skincare product is a sunscreen, the carrot derivative accounts for 0.05% to 5.0% of the total mass. When the skincare product is a whitening product, the carrot derivative accounts for 0.1% to 4.0% of the total mass. When the skincare product is a moisturizing product, the carrot derivative accounts for 0.5% to 10.0% of the total mass. When the skincare product is an anti-aging product, the carrot derivative accounts for 1.0% to 5.0% of the total mass. When the skincare product is a soothing product, the carrot derivative accounts for 0.05~3.0% of the total mass.
[0020] Furthermore, the sun protection product is a sunscreen cream, sunscreen gel, sunscreen spray, or sunscreen stick; The whitening products mentioned are whitening essences, whitening masks, whitening lotions, whitening body lotions, whitening toners, or whitening oral supplements; The moisturizing products are moisturizing lotions, moisturizing serums, moisturizing sprays, moisturizing masks, moisturizing oils, moisturizing facial cleansers, or lip balms. The anti-aging products are anti-aging face creams, firming masks, anti-aging essential oils, or anti-aging eye creams; The soothing products are soothing face creams, soothing face masks, soothing sprays, or soothing eye creams.
[0021] The technical solution of the present invention has the following advantages compared with the prior art: (1) This invention is simple, efficient, environmentally friendly, safe and controllable, and enables the one-step preparation of carrot derivatives for multifunctional applications in cosmetics: The microchannel reactor enables precise control of reaction conditions (temperature and residence time, etc.), and while ensuring that the reaction phases have the same residence time, carrot derivatives can be prepared efficiently in a short time. Therefore, the energy consumption during the reaction process is low, the product has good uniformity and stable quality, and the effective components in carrots are retained to a great extent, resulting in high utilization rate; (2) Natural Source and Safety: Carrots are a widely cultivated vegetable with readily available and inexpensive natural raw materials. Further processing them for use as cosmetic ingredients without introducing additional chemicals makes them safer and gentler, suitable for all skin types, especially sensitive skin. Compared to chemically synthesized ingredients, this reduces the risk of allergies and irritation. (3) Excellent performance and multifunctional applications: Carrot derivatives have full UV absorption properties and can replace traditional UV absorbers in sunscreen products; Carrot derivatives effectively inhibit the synthesis of tyrosinase and the formation of melanocytes, and can be used as whitening agents in whitening products; Carrot derivatives contain a variety of hydrophilic functional groups on their surface, have excellent water solubility and water absorption, and can absorb moisture from the atmosphere to keep the skin moist, and can be used as moisturizers in moisturizing products; Carrot derivatives exhibit excellent free radical scavenging ability, slow down skin aging, and can be used as an active ingredient in anti-aging products; (4) Carrot derivatives, as cosmetic raw materials, meet people's current pursuit of green, environmentally friendly and natural cosmetics. Their natural source and biocompatibility make them a sustainable and environmentally friendly choice, filling the market demand for natural raw materials, while transforming low-value-added crops into high-value-added products. Attached Figure Description
[0022] Figure 1 This is a photograph of the carrot derivative prepared in Example 1 of the present invention under natural light.
[0023] Figure 2 The results of the cytotoxicity experiment of the carrot derivative prepared in Example 1 of this invention are shown.
[0024] Figure 3 The infrared spectrum of the carrot derivative prepared in Example 1 of this invention.
[0025] Figure 4 The image shows the ultraviolet transmittance curve of the carrot derivative prepared in Example 1 of this invention.
[0026] Figure 5 The inhibition rate of the carrot derivative prepared in Example 1 of this invention against tyrosinase is shown.
[0027] Figure 6 The inhibition rate of the carrot derivative prepared in Example 1 of this invention on melanocyte proliferation.
[0028] Figure 7 The inhibition rate of the carrot derivative prepared in Example 1 of this invention on melanocyte synthesis is shown.
[0029] Figure 8 This is a diagram showing the transdermal absorption behavior of the carrot derivative prepared in Example 1 of the present invention.
[0030] Figure 9 The carrot derivative prepared in Example 1 of this invention is effective against DPPH free radicals and ABTS. + Scavenging rates of free radicals, superoxide anions, and hydroxyl radicals.
[0031] Figure 10 The images show actual products of whitening essence, moisturizing essence, sunscreen lotion and anti-aging cream prepared using carrot derivatives as active ingredients, as described in Example 1 of this invention. Detailed Implementation
[0032] The present invention will be further described below with reference to the accompanying drawings and specific embodiments, so that those skilled in the art can better understand and implement the present invention. However, the embodiments described are not intended to limit the present invention.
[0033] Example 1: One-step continuous synthesis of carrot derivatives (1) After setting up the experimental setup, place the microchannel reactor in an oil bath and heat it to 120 °C; (2) Using a plunger pump, carrot juice with a solid content of 20% (obtained by mixing 20 g of carrots and 80 g of deionized water and pressing) was introduced into a microchannel reactor (inner diameter 3 mm, pipe length 4.5 m), held for 20 min, and the crude product of carrot derivative was collected. (3) The crude product was filtered through a 0.22 μm MCE needle filter, transferred to distilled water, dialyzed with a 3500 Da dialysis bag for 48 h, and then freeze-dried at -60 ℃ for 48 h to obtain carrot derivative powder.
[0034] The morphology of the carrot derivative prepared in this example is as follows: Figure 1 As shown: The freeze-dried carrot derivative is brown granules with some crystalline particles, indicating that the precursor underwent a series of complex chemical changes in the microchannel reactor to generate a stable carrot derivative.
[0035] The biotoxicity of the carrot derivative prepared in this example is as follows: Figure 2 As shown: Using 3T3 cells as the subject, the MTT assay was used to test the cytotoxicity of different concentrations of carrot derivatives. The results showed that the prepared carrot derivatives were non-toxic to cells at different concentrations and had excellent biocompatibility, and could be widely used in food, cosmetics, pharmaceuticals, health products and other fields.
[0036] The infrared spectrum of the carrot derivative obtained in this embodiment is as follows: Figure 3 As shown, 3361.78 cm -1 The strong and broad absorption peaks in the vicinity indicate the presence of OH stretching vibrations. (1656.35, 1526.25, and 1397.03 cm⁻¹) -1 The peaks at the specified locations can be attributed to the C=C stretching vibration, NH bending vibration, and CO stretching vibration, respectively. This indicates that the prepared carrot derivatives possess functional groups such as carboxyl, carbonyl, and amino groups on their surface, which endow them with excellent water solubility.
[0037] The ultraviolet transmittance curve of the carrot derivative prepared in this embodiment is as follows: Figure 4 As shown, the prepared carrot derivative was dissolved in deionized water to prepare a solution with a concentration of 2.5 mg / mL, and its ultraviolet transmittance curve was tested. As can be seen from the figure, its blocking rate for UVA is as high as 98.2%, and its blocking rate for UVB is as high as 93.5%, which is much higher than some commercial sunscreens at the same concentration. It is an excellent green ultraviolet absorber that can be used in a variety of sunscreen products.
[0038] The carrot derivative prepared in this embodiment exhibits the following inhibition rates against tyrosinase, melanocyte proliferation, and melanocyte synthesis: Figures 5-7 As shown, adding only a small amount of carrot derivatives to the formula can achieve a high inhibition rate of tyrosinase, melanocyte proliferation, and melanocyte synthesis. Melanin production is mainly regulated by tyrosinase, and the proliferation and synthesis of melanocytes directly affect skin pigmentation. Carrot derivatives can serve as an excellent active ingredient in whitening skincare products, helping to improve skin tone and reduce age spots and freckles.
[0039] The transdermal absorption behavior of the carrot derivative prepared in this embodiment is as follows: Figure 8 As shown, the cumulative penetration of carrot derivatives increases continuously over time. Combined with the infrared spectrum, the following conclusions can be drawn: Carrot derivatives possess both excellent water absorption and small molecule permeability, making them suitable for use in moisturizing products, allowing them to function on multiple levels. Besides providing the necessary moisture to surface cells and preventing moisture loss, they can also penetrate deeply to provide more comprehensive hydration to the skin, thereby improving skin's moisture, elasticity, and appearance.
[0040] The carrot derivative prepared in this embodiment exhibits the following free radical scavenging ability: Figure 9 As shown, at extremely low concentrations, carrot derivatives exhibit effects on DPPH free radicals and ABTS. + The scavenging rates of free radicals, superoxide anions, and hydroxyl radicals reached 90.7%, 76.5%, 70.8%, and 88.3%, respectively. The antioxidants in the prepared carrot derivatives scavenge various free radicals through different mechanisms, exhibiting strong antioxidant activity and making them suitable for various anti-aging products.
[0041] Example 2: Preparation of sunscreen lotion based on carrot derivatives The preparation method of the carrot derivative is the same as in Example 1. The sunscreen lotion (100 parts) was prepared according to the following mass ratio of raw materials: sunscreen agent: 1 part carrot derivative and 10 parts zinc oxide; emulsifier: 3 parts glyceryl stearate and 2 parts sorbitan stearate; moisturizer: 5 parts glycerin and 3 parts squalane; stabilizer: 1 part caprylic / capric triglyceride; film-forming agent: 10 parts polydimethylsiloxane; additive: 1.5 parts hyaluronic acid; pH adjuster: 1 part NaOH (5%); preservative: 0.25 parts paraben preservative; the remainder is distilled water.
[0042] The steps for preparing sunscreen lotion are as follows: (1) Take a 150 mL beaker, heat the oil phase components (sunscreen, moisturizer, emulsifier, stabilizer, film-forming agent) to 70 °C, and stir until homogeneous; (2) At the same time, take a 100 mL beaker, heat the aqueous phase components (distilled water, additives) to 70 °C and stir evenly; under stirring conditions, slowly inject the aqueous phase into the oil phase and stir evenly. (3) After the mixture cools to about 40 °C, add preservatives and pH adjusters, and continue to stir until homogeneous to obtain sunscreen emulsion.
[0043] Example 3: Preparation of sunscreen spray based on carrot derivatives The preparation method of the carrot derivative is the same as in Example 1. The sunscreen spray (100 parts) is prepared according to the following mass ratio of raw materials: sunscreen agent: 1 part of carrot derivative and 15 parts of zinc oxide; emulsifier: 2 parts of coconut alcohol amine; moisturizer: 10 parts of aloe vera gel and 5 parts of glycerin; pH adjuster: 0.5 parts of NaOH (5%); preservative: 0.3 parts of paraben preservative; the rest is distilled water.
[0044] The preparation steps for sunscreen spray are as follows: (1) Take a 150 mL beaker, mix the sunscreen, moisturizer and emulsifier, and stir well; (2) Gradually add distilled water to the mixture while stirring constantly to ensure that the components are fully dissolved; (3) After the mixture cools to about 40 °C, add the preservative and pH adjuster, continue stirring until homogeneous, and then filter the spray liquid to ensure a smooth texture. Finally, fill the finished product into spray bottles to obtain sunscreen spray.
[0045] Example 4: Preparation of Whitening Essence Based on Carrot Derivatives The preparation method of the carrot derivative is the same as in Example 1. The whitening essence (100 parts) was prepared according to the following mass ratio of raw materials: whitening agent: 2 parts carrot derivative and 2 parts arbutin; moisturizer: 5 parts glycerin, 3 parts sorbitol and 3 parts α-mannan; thickener: 0.3 parts xanthan gum; esterifier: 0.5 parts water-soluble jojoba oil; additives: 3 parts irritation inhibitor, 0.3 parts dipotassium glycyrrhizate and 3 parts free radical scavenger; preservative: 0.2 parts diazolidinyl urea; the remainder is distilled water.
[0046] The steps for preparing a whitening face mask are as follows: (1) Take a 150 mL beaker, and under heating conditions of 80 °C, mix distilled water and thickener, stirring constantly to ensure that the components are fully dissolved; (2) Add the whitening agent, moisturizer, esterifying agent and additives to the mixture and stir to dissolve; (3) After the mixture cools to about 45°C, add the preservative, mix evenly, and then discharge.
[0047] Example 5: Preparation of Whitening Emulsion Based on Carrot Derivatives The preparation method of the carrot derivative is the same as in Example 1. The whitening emulsion (100 parts) was prepared according to the following mass ratio of raw materials: whitening agent: 1.5 parts of carrot derivative and 2 parts of arbutin; moisturizer: 1.5 parts of hyaluronic acid, 5 parts of glycerin and 3 parts of sorbitol; emulsifier: 1 part of stearyl alcohol polyether-2 and 4 parts of glyceryl stearate; pH adjuster: 1 part of NaOH (5%); skin moisturizer: 5 parts of white oil, 3 parts of caprylic triglyceride, 4 parts of ethylhexyl palmitate and 2 parts of polydimethylsiloxane; pH adjuster; preservative: 0.2 parts of methylparaben; the remainder is distilled water.
[0048] The preparation steps for whitening lotion are as follows: (1) Take a 150 mL beaker and mix distilled water, whitening agent, moisturizer and emulsifier under heating conditions of 80 ℃, and stir evenly; (2) Gradually add the emollient to the mixture while stirring constantly to ensure that the ingredients dissolve; (3) After the mixture cools to about 40 °C, add preservatives and pH adjusters, continue to stir evenly, then filter the emulsion liquid to ensure a smooth texture and discharge the material.
[0049] Example 6: Preparation of Moisturizing Essence Based on Carrot Derivatives The preparation method of the carrot derivative is the same as in Example 1. The moisturizing essence (100 parts) is prepared according to the following mass ratio of raw materials: moisturizer: 2 parts carrot derivative, 5 parts glycerin and 3 parts sorbitol; thickener: 0.5 parts xanthan gum; esterifier: 0.2 parts jojoba wax PEG-120 ester; preservative: 0.2 parts diazoimidazole urea, and the rest is distilled water.
[0050] The steps for preparing a moisturizing serum are as follows: (1) Take a 150 mL beaker, and under heating conditions of 80 °C, mix distilled water, humectant, thickener and esterifier, stir evenly to ensure that the components are dissolved; (2) After the mixture cools to about 40°C, add the preservative, continue to stir evenly, and then discharge.
[0051] Example 7: Preparation of a moisturizing gel based on carrot derivatives The preparation method of the carrot derivative is the same as in Example 1. The moisturizing gel (100 parts) is prepared according to the following mass ratio of raw materials: Moisturizer: 2 parts carrot derivative, 5 parts glycerin, 2 parts trehalose and 0.2 parts allantoin; Thickener: 0.4 parts carbomer U20; Esterifying agent: 0.2 parts jojoba wax PEG-120 ester; Film-forming agent: 0.5 parts hydroxypropyl methylcellulose; pH adjuster: 1 part NaOH (5%); Preservative: 0.2 parts azirzolidinyl urea, and the remainder is distilled water.
[0052] The steps for preparing the moisturizing gel are as follows: (1) Take a 150 mL beaker and mix distilled water, humectant, thickener, esterifier and film-forming agent under heating conditions of 80 ℃. Stir evenly to ensure that the components are dissolved. (2) After the mixture cools to about 40 °C, add pH adjuster and preservative, continue to stir evenly, and discharge.
[0053] Example 8: Preparation of anti-aging water based on carrot derivatives The preparation method of the carrot derivative is the same as in Example 1. The anti-aging water (100 parts) is prepared according to the following mass ratio of raw materials: anti-aging agent: 1 part of carrot derivative and 1 part of collagen; moisturizer: 5 parts of glycerin and 3 parts of sorbitol; esterifying agent: 0.2 parts of jojoba wax PEG-120 ester; preservative: 0.2 parts of azirzolidinyl urea, and the rest is distilled water.
[0054] The steps for preparing anti-aging water are as follows: (1) Take a 150 mL beaker, and mix distilled water, humectant, carrot derivative and esterifier under heating conditions of 80 °C. Stir well to ensure that the components are dissolved. (2) After the mixture cools to about 40°C, add collagen and preservative, continue to stir evenly, and then discharge.
[0055] Example 9: Preparation of an anti-aging face cream based on carrot derivatives The preparation method of the carrot derivative is the same as in Example 1. The anti-aging cream (100 parts) was prepared according to the following mass ratio of raw materials: Anti-aging agent: 1 part carrot derivative and 0.5 parts collagen; Moisturizer: 5 parts glycerin and 3 parts sorbitol; Emulsifier: 3.5 parts stearyl alcohol polyether-2; Skin moisturizer: 3 parts synthetic jojoba oil; 2 parts cetearyl alcohol, 2 parts glyceryl stearate, 3 parts caprylic triglyceride, 4 parts ethylhexyl palmitate and 2 parts polydimethylsiloxane; Antioxidant: 0.5 parts tocopheryl acetate; pH adjuster: 0.2 parts triethanolamine; Thickener: 0.2 parts carbomer; Preservative: 0.2 parts methylparaben, and the remainder is distilled water.
[0056] The steps for preparing anti-aging face cream are as follows: (1) Take a 150 mL beaker, heat the oil phase components (anti-aging agent, emollient, emulsifier, antioxidant and preservative) to 80 °C, and stir evenly; (2) At the same time, take a 100 mL beaker, heat the aqueous phase components (distilled water, thickener and humectant) to 80 °C and stir evenly; under stirring conditions, slowly inject the oil phase into the aqueous phase until homogeneous; (3) After the mixture cools to about 40 °C, add the preservative and pH adjuster, and continue to stir evenly to obtain the anti-aging face cream.
[0057] Comparative Example 1: Preparation of Carrot Derivatives Based on Solvent Extraction Weigh 50.0 g of carrot, pulverize it, and add 100 mL of a mixture of petroleum ether and acetone (V:V=1:4) for extraction. After three extractions, combine the extracts and transfer them to a separatory funnel, allowing them to separate into layers. Dehydrate the upper yellow liquid with anhydrous NaSO4, and evaporate the dried extract to dryness on a rotary evaporator. Add 5 mL of petroleum ether, aspirate the extract with a dropper, and pass it through an alumina chromatography column. Elute with petroleum ether to collect the carrot derivative.
[0058] Compared with Example 1, this method requires the use of chemical solvents such as petroleum ether and acetone during the preparation process, which will harm the environment and affect the safety of subsequent products; moreover, solvent extraction can only extract a small portion of the effective components, and the extraction efficiency is low, which cannot meet the subsequent needs.
[0059] Comparative Example 2: Low-Temperature Preparation of Carrot Derivatives The preparation method was the same as in Example 1, except that the temperature of the oil bath was set to 70 °C, while other conditions remained unchanged. Carrot derivatives were collected, but the infrared spectra of the carrot derivatives prepared at this temperature were indistinguishable from those of the raw carrot juice. This is because the energy provided by the lower temperature was insufficient to break the existing chemical bonds in the carrot juice, and the reaction rate was slower and the formation efficiency was lower at low temperatures.
[0060] Comparative Example 3: High-Temperature Preparation of Carrot Derivatives The preparation method was the same as in Example 1, except that the oil bath temperature was set to 200 °C, while other conditions remained unchanged, and the carrot derivative was collected. However, the excessively high reaction temperature led to over-carbonization of the carrot juice, and some functional groups on the surface also underwent carbonization, forming large carbon aggregates, which affected the quality and consistency of the product. In addition, the carbon aggregates caused blockage of the microchannels, increasing the internal pressure of the channels and increasing operational risks.
[0061] Comparative Example 4: Sunscreen Lotion Prepared Based on Octocrylene The preparation method was the same as in Example 2, except that 1 part of carrot derivative was replaced with 1 part of octocrylene sunscreen. The SPF values and irritation of the products from Example 2 and Comparative Example 4 were evaluated using an SPF-290 sun protection factor analyzer. The sunscreen lotion prepared based on the carrot derivative had an SPF value of 38.22, while the octocrylene sunscreen had an SPF value of only 19.37. Volunteers were recruited for patch testing, and changes in the patch area were compared before and after 24 hours of use. Skin irritation scores were compiled. The irritation of the sunscreen lotion based on the carrot derivative was significantly lower than that of the octocrylene sunscreen. Compared to octocrylene, the carrot derivative has superior UV absorption properties and lower irritation.
[0062] Comparative Example 5: Whitening Essence Prepared Based on Niacinamide The preparation method was the same as in Example 4, except that 2 parts of carrot derivative were replaced with 5 parts of niacinamide whitening agent. Volunteers were recruited to evaluate the whitening efficacy. Skin L*a*b* color space data were measured using a skin colorimeter to calculate the Individual Type Angle (ITA°) and Melanin Index (MI). Comparing the ΔITA° and ΔMI of the two products, the whitening essence based on carrot derivative had higher ΔITA° and Δ|MI| than the whitening essence prepared based on niacinamide. This indicates that compared to traditional niacinamide whitening agents, carrot derivative has better whitening effects and lower irritation.
[0063] Comparative Example 6: Preparation of Moisturizing Essence Based on α-Mannan The preparation method was the same as in Example 6, except that 2 parts of carrot derivative were replaced with 2 parts of α-mannan moisturizer. Volunteers were recruited to evaluate the moisturizing efficacy. Skin hydration volume (MMV) and transepidermal water loss (TEWL) were measured using Corneometer and Tewameter instruments. The comparison showed that the moisturizing efficacy of carrot derivative was higher than that of α-mannan, and it can be used as a moisturizer in cosmetics.
[0064] Comparative Example 7: Anti-aging face cream prepared based on retinyl palmitate The preparation method is the same as in Example 9, except that 1 part of carrot derivative is replaced with 1 part of retinyl palmitate anti-aging agent. Volunteers were recruited to evaluate the anti-aging efficacy. The two anti-aging creams were compared using VISIA, specifically comparing the change rate of crow's feet area in selected regions. Compared to retinyl palmitate, the anti-aging cream using carrot derivative showed a lower change rate of crow's feet area in selected regions, indicating that the carrot derivative of this invention has superior anti-wrinkle performance in skin testing.
[0065] The performance testing methods in the above embodiments and comparative examples are as follows: (1) Cytotoxicity test (MTT method) Human breast cancer cells (MCF-7) were used in the experiment and incubated in a carbon dioxide incubator at a temperature of 37°C and a CO2 concentration of 5%. After the cells had confluently covered the culture flask walls, they were digested and passaged into 96-well plates. Cell counts were performed using a cell counting chamber to ensure a cell density of approximately 5 × 10⁶ cells per well. 3 / mL. Cells were passaged overnight in 96-well plates until adherence, then different concentrations of carrot derivative (0, 2.5, 5.0, 10.0, 25.0, 50.0, 100.0, 200.0, and 500.0 μg / mL) were added, and the plates were cultured for another 24 h. Cells were washed three times with PBS, and then 20 μL of 0.5 mg / mL MTT solution was added to each well. The plates were incubated for another 4 h. Cells were then washed three times with PBS, and 150 μL of DMSO was added to each well. The plates were vortexed at room temperature for 15 min, and then analyzed using a microplate reader. The results showed that even at a carrot derivative concentration of 500 μg / mL, cell viability was above 98%, and the MTT assay results indicated that the synthesized carrot derivative exhibited low cytotoxicity.
[0066] (2) Ultraviolet transmittance test The brown carrot derivative powder obtained in Example 1 was dissolved in deionized water to prepare a solution with a concentration of 2.5 mg / mL. The transmittance spectrum of this solution was measured using a TU-1901 UV-Vis spectrophotometer from Beijing Purkinje General Instrument Co., Ltd., and the results were as follows: Figure 4 The ultraviolet transmittance spectrum.
[0067] (3) Tests on the inhibition rate of tyrosinase, melanocyte proliferation, and melanocyte synthesis. Using mouse B16 melanocytes as test cells, this study investigated the effects of carrot derivatives on the inhibition of tyrosinase activity, melanocyte proliferation, and the correlation between their effects and the inhibition of melanin production.
[0068] ①Cultivation of B16 melanocytes B16 melanocytes were cultured in an environment of 37°C with 5% CO2 in the air, and passaged every 2 days in 10% BS medium.
[0069] ② Determine cellular tyrosinase activity Using levodopa as the substrate, the assay was performed using a modified method by Marlinez-Esparza et al. After 4 days of drug treatment, the supernatant was discarded, and the cells were washed three times with PBS (pH 7.0), centrifuged at 1000 r / m for 5 min each time. 90 μL of 1% Troton X-100 solution was added to each well to lyse the cells. After pre-warming at 37 ℃, 10 μL of 1% levodopa was added to each well, and the cells were incubated at 37 ℃ for 30 min. The absorbance was measured at 475 nm, with the blank well used as the zeroing point. The absorbance (A value) of each well was read every 10 min within 1 h at 37 ℃.
[0070] Tyrosinase activity inhibition rate = (1 - average absorbance of each concentration of A / average absorbance of the control group of A) * 100% ③ Determine the proliferative activity of melanocytes Add 3*10 B16 melanin particles 4 Cells were placed in 12-well plates at a specific density. The medium was changed on the second day, and different concentrations of drug solutions were added. The control group was treated with 0.05% (v / v) DMSO. At the end of incubation, cells were collected, stained with cone blue, and counted using a hemocytometer.
[0071] Melanocyte proliferation inhibition rate = (1-N) 各浓度组计数 / N 对照组值计数 )*100% ④ Determine melanin content Melanin content was determined using a modified method by Hosoi et al. B16 melanocytes were analyzed at a concentration of 1*10-1. 5 The samples were cultured at high density in 6-well plates. After 24 h, the medium was changed, and different concentrations of the drug were added. After 72 h, the samples were washed twice with PBS, air-dried, and dissolved in 200 μL of 1 M NaOH (containing 1% DMSO). After heating to 80 °C for 1 h and cooling, the absorbance value was read at 475 nm using an ELISA reader.
[0072] Melanin inhibition rate = [1 - (absorbance value of drug well / cell density of drug well) / (absorbance value of control well / cell density of control well)] * 100% (4) Skin penetration test Fresh pigskin was used, with subcutaneous fat removed but the dermis retained to simulate human skin. Physiological saline was added to the absorption chamber of a Franz diffusion tank as the receiving solution, and a 1 mg / mL sample solution was prepared as the diffusion solution and placed in the diffusion chamber. The treated pigskin was placed between the diffusion and receiving chambers using stainless steel horseshoe clamps. The temperature was set at 37 ℃ and the rotation speed at 500 r / min. Every 2 hours, 1 mL of diffusion solution was transferred from the diffusion chamber, and 1 mL of clean diffusion solution was added simultaneously. The fluorescence intensity of the diffusion solution at the maximum excitation wavelength was measured using a fluorescence spectrophotometer, and the permeation accumulation of the sample was calculated.
[0073] (5) Free radical scavenging rate test ①DPPH free radical scavenging performance test Add 4 mL of standard phosphate buffer solution (pH 6.88) and 4 mL of 0.1777 mmol / L DPPH solution to a 10 mL test tube, and mix well. Then add the sample solution to be tested, and add distilled water to bring the volume to 10.0 mL, and mix thoroughly. Measure the absorbance at 520 nm after 10 min. Repeat the measurement three times for each sample group and take the average value. The scavenging rate of DPPH free radicals can be calculated using the following formula:
[0074] In the formula:A 1 represents the absorbance value of the test sample. A 2 is the absorbance value of the control sample (without DPPH). A 3 is the absorbance value of the control (excluding the sample).
[0075] ②ABTS + Free radical scavenging performance test By measuring ABTS + The antioxidant activity of carrot derivatives was evaluated by assessing their free radical scavenging ability, with gallic acid and ascorbic acid used as positive controls. ABTS + Preparation of free radical stock solution: First, prepare a 0.140 mol / L potassium persulfate aqueous solution. Then, add 1.76 mL of the potassium persulfate aqueous solution to 100 mL of a 0.384 mg / mL ABTS aqueous solution and react in the dark for 12–16 h. ABTS + Preparation of free radical assay solution: Dilute ABTS with phosphate buffer solution (pH=7.4) before testing. + The absorbance of the free radical stock solution to A734 was 0.70 ± 0.02. Before testing, samples of carrot derivatives at concentrations of 1.0, 2.0, 3.0, 4.0, and 5.0 mg / mL were prepared. 3.9 mL of ABTS was used as the test solution. + Add the solution to 0.1 mL of the test sample solution, mix well, let stand for 10 min, and measure the absorbance at a wavelength of 734 nm, denoted as A1; take 3.9 mL of ABTS + Add the solution to 0.1 mL of deionized water, mix well, let stand for 6 min, and measure the absorbance at a wavelength of 734 nm, denoted as A0. Calculate ABTS. + The clearance rate can be calculated using the following formula:
[0076] In the formula: A1 is the absorbance value of the sample, and A0 is the absorbance value of the control (ABTS solution without the sample).
[0077] ③ Test of superoxide anion scavenging ability a. Determination of the activity of the test substance. Add 2.8 mL of Tris-HCl-EDTA buffer (pH 8.2) to a 4 mL centrifuge tube, then add 0.1 mL of the test substance and 0.1 mL of 45 mmol / L pyrogallol solution. Measure the absorbance at 340 nm and record it as A0; measure the absorbance at 30 min and record it as A. 30 The measurement at 40 mm is recorded as A. 40 ; b. Blank determination. Add 2.8 mL of Tris-HCl-EDTA buffer, 0.1 mL of pyrogallol solution, and 0.1 mL of water to a 4 mL centrifuge tube. Measure the absorbance at 340 nm as B0; measure again after 30 min and record as B. 30 ; Record 40 minutes as B 40 ; c. Results Analysis. The scavenging rate of the test substance for superoxide anions can be calculated using the following formula.
[0078] Where: η2 is the scavenging rate of the test substance for superoxide anions, %; Initial absorbance of blank solutions B0 and A0 and test solution; B 30 A 30 The absorbance of the blank solution and the test solution at 30 min.
[0079] ④ Determination of hydroxyl radical scavenging ability a. Test Procedure: Add 0.5 mL of 0.4 mmol / L crystal violet, 1.4 mL of 0.2 mol / L PBS solution (pH 7.4), 0.5 mL of 1 mmol / L FeSO4 solution, and 0.1 mL of the sample to a 5 mL centrifuge tube, and finally add 0.5 mL of 6% H2O2 solution. After standing for 1 h, measure the absorbance (A) at 584 nm. The absorbance when distilled water is used instead of the sample is taken as CK1, and the absorbance when distilled water is used instead of both the sample and H2O2 is taken as CK2.
[0080] b. Results Analysis: The scavenging rate of the test substance for superoxide anions can be calculated using the following formula:
[0081] (6) SPF-290 sun protection factor analyzer test a. Sample preparation: Using a dedicated syringe, draw up the sample using either a pressure method or an extraction method, and apply it evenly to the polymethyl methacrylate (PMMA) surface in dots or strips. Then, use a finger wearing a latex medical finger cot to spread the sample, ensuring a uniform surface. The actual sample amount applied to each plate should be 1.8-2.2 mg / cm³. 2 between.
[0082] b. Measurement: According to the instrument instructions, use a quartz plate with a load strip and a polymethyl methacrylate plate for instrument calibration and blank calibration during measurement. Then, place the sample coated according to the above steps at room temperature (20~30 ℃) and 40%~60% relative humidity for 20 min before measuring it on the SPF meter. Each sample should have no less than 4 measurement points.
[0083] (7) Human patch test Select an area not exceeding 50 mm 2 A qualified spot test apparatus with a depth of approximately 1 mm is required. Place the test substance into the small chamber of the spot test apparatus, using approximately 0.020 g to 0.025 g or 0.020 mL to 0.025 mL, or a sample of the same size and depth as the chamber. When the test substance is the original cosmetic product, the control well should be a blank control (without any substance). When the test substance is a diluted cosmetic product, the control well should contain the diluted form of that cosmetic. Apply the spot test apparatus containing the test substance to the back or flexor side of the forearm of the subject using hypoallergenic adhesive tape, gently pressing with the fingertips or palm to ensure even application to the skin, and leave for 24 hours.
[0084] (8) Skin colorimeter and skin melanin analyzer tests Staff shall apply the test sample to the corresponding test area according to the random table, and the smear area shall be no less than 6 cm². 2 The sample volume was (2.0 ± 0.1) mg / cm³. 2 Or (2.0 ± 0.1) L / cm 2 The interval between each test area should be no less than 1.0 cm. The back is the preferred test site, but non-exposed areas such as the thighs and upper arms can also be selected. The area of each blackened test area should be no less than 0.5 cm². 2 The samples should be located within each smear area. At each visit, use a skin colorimeter to measure the L*, a*, and b* values of each test area. Test each area three times, record and calculate the ITA° value. The higher the ITA° value, the lighter the skin tone, and vice versa.
[0085]
[0086] At each visit time, the MI value of each test area was measured using a skin melanin analyzer. Each test area was tested three times and the results were recorded. The smaller the MI value, the lower the skin melanin content, and vice versa.
[0087] (9) MMV and TEWL tests Each group of test substances and test sites were randomly numbered to determine the control order of the test substances and test sites. Before the experiment, subjects were required to wash the inside of their forearms with clean water. After washing, measurement marks were made on the inside of the subjects' forearms. In this experiment, two test areas were marked on each forearm, and one test substance was applied to each area. The areas were spaced 1 cm apart, and each test area was 5 cm * 5 cm. The sample amount was 0.2 g. After the subjects sat quietly in a constant environment for 30 minutes, the blank value of the test sites was measured using a Corneometer. Five points were measured in each area in a fixed order, and the average value was obtained. Then, a designated person was responsible for applying the sample and starting the timer. According to the experimental design, the change in MMV value was measured at each time period. The change in MMV value for each time period was obtained by subtracting the blank value from the average value of each test. Dividing the blank value again gave the growth rate of MMV value. The calculation formula is as follows: Hydration growth rate = (MMV) t -MMV0) / MMV0*100% The transepidermal water loss (TEWL) value of the stratum corneum of the skin was tested before and after the use of cosmetics. The lower the TEWL value of the skin, the better the skin barrier function, and vice versa.
[0088] (10) Measurement of skin wrinkles First, calibrate the instrument according to basic operating requirements. Before the experiment, the subject needs to clean the test area with a uniform mild detergent, and mark a symmetrical 3 cm * 3 cm square test area on the test area, numbering each area. Test areas and blank controls are randomly assigned. A siloxane membrane is prepared using siloxane liquid to obtain inverse replicas of skin wrinkles in the test and blank control areas on the subject's skin. Using an image analysis instrument, a beam of light of a specific wavelength is shone onto the membrane. Then, a CCD camera lens collects the light signals from different parts of the membrane. Through photoelectric and digital processing, a three-dimensional image of the skin is obtained, which is then analyzed using specialized software to obtain the skin roughness parameters of the test and blank control areas on the subject's skin. Referring to the German Industrial Standard (Deutsche Industrie Normen, DIN), skin roughness R: the height between the highest peak and the lowest valley in the measurement segment; maximum roughness R... m : Height between adjacent peaks and valleys; Average roughness R: Average skin roughness of 5 measurement segments; Smoothing depth R: The area between the contour lines on both sides of the midline and the midline is equal when a midline is drawn through the skin surface contour to divide the contour into two parts. Smoothing depth is the height between the peak and the midline; Results analysis: The effects of anti-aging active ingredients on skin aging were evaluated based on the changes in skin roughness, maximum roughness, average roughness, smoothness depth, and arithmetic mean roughness in the test area and blank control area of the subjects.
[0089] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.
Claims
1. A method for preparing a carrot derivative, characterized in that, Includes the following steps, S1: Heating the microchannel reactor; S2: Pass carrot juice into a heated microchannel reactor and heat it to react, obtaining the crude product; S3: The crude product is filtered, dialyzed, and freeze-dried to obtain the carrot derivative; The microchannel reactor is made of stainless steel, glass, aluminum, copper, or nickel tubes, with an inner diameter of 0.25–4 mm and a length of 3–8 m. In step S1, the heating temperature is 110~160 ℃; In step S2, the heating reaction temperature is 110~160 ℃, and the reaction time is 5~60 min; In step S3, the filter head used for filtration has a pore size of 0.22 μm; the molecular weight cutoff for dialysis is 500~3500 Da; the freeze-drying temperature is -50 ℃~-70 ℃, and the time is 1~3 days.
2. A carrot derivative prepared by the preparation method according to claim 1.
3. A skincare product, characterized in that, It includes the carrot derivative as described in claim 2.
4. The skincare product as described in claim 3, characterized in that, The skincare products mentioned are sunscreens, whitening products, moisturizing products, anti-aging products, or soothing products.
5. The skincare product as described in claim 4, characterized in that, When the skincare product is a sunscreen, the carrot derivative accounts for 0.05% to 5.0% of the total mass. When the skincare product is a whitening product, the carrot derivative accounts for 0.1% to 4.0% of the total mass. When the skincare product is a moisturizing product, the carrot derivative accounts for 0.5% to 10.0% of the total mass. When the skincare product is an anti-aging product, the carrot derivative accounts for 1.0% to 5.0% of the total mass. When the skincare product is a soothing product, the carrot derivative accounts for 0.05~3.0% of the total mass.
6. The skincare product as described in claim 4 or 5, characterized in that, The sun protection product is a sunscreen cream, sunscreen gel, sunscreen spray, or sunscreen stick; The whitening products mentioned are whitening essence, whitening mask, whitening lotion, whitening body lotion or whitening toner; The moisturizing products are moisturizing lotions, moisturizing serums, moisturizing sprays, moisturizing masks, moisturizing oils, moisturizing facial cleansers, or lip balms. The anti-aging products are anti-aging face creams, firming masks, anti-aging essential oils, or anti-aging eye creams; The soothing products are soothing face creams, soothing face masks, soothing sprays, soothing serums, or soothing eye creams.
Citation Information
Patent Citations
Method for extracting nutrient components of carrot through CO2 supercritical extraction
CN101779788A