A gardenia flower extract, a preparation method thereof and application thereof in anti-wrinkle skin care products

Abstract

The present application belongs to the technical field of cosmetics, and particularly relates to gardenia flower extract, a preparation method thereof and application of the gardenia flower extract in anti-wrinkle skin care products. The present application uses gardenia flowers as raw materials, and first extracts the gardenia flowers with water, filters to remove water-soluble impurities, then extracts the obtained filter residue with butanediol, and after filtering, butanediol is supplemented to prepare the gardenia flower extract. The present application uses a simple process of water and butanediol step extraction, and the operation process is simple, without complex post-treatment process, which can effectively reduce the production cost and improve the production efficiency, and the whole process uses butanediol as an organic solvent, without harmful solvent residues, and the product safety is high. The gardenia flower extract prepared by the process of the present application has excellent anti-wrinkle activity, and can be applied to skin care products as an anti-wrinkle functional component, and the anti-wrinkle effect is better than that of similar products on the market, and has good industrial application prospect and market promotion value.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, and particularly relates to a gardenia extract, its preparation method, and its application in anti-wrinkle skin care products. Background Technology

[0002] Aging is an extremely complex biological process composed of multiple stages and is irreversible, but its progress can be slowed down using modern biological techniques. There are many methods to delay aging, such as chemical drugs like dehydroepiandrosterone (DHEA), testosterone, and human growth hormone. However, long-term use of these drugs can produce uncontrollable side effects. Plant extracts, on the one hand, can, to some extent, eliminate the damage caused by peroxides to the body and enhance the body's aerobic metabolism, thereby achieving the goal of delaying aging. On the other hand, they can enhance the activity of elastase and collagenase, increasing skin elasticity and reducing wrinkles, thus delaying skin aging.

[0003] Gardenia is a traditional Chinese medicinal plant. Gardenia jasminoides The flowers of the genus *Ceratophyllum demersum* have been widely used in the cosmetics, food, and pharmaceutical industries. The *Compendium of Materia Medica* states that it "improves complexion," and its use has a long history and enormous development potential. Its main active ingredients are flavonoids, polyphenols, and iridoids, which show significant potential in anti-oxidation, anti-aging, promoting collagen synthesis, and anti-inflammation.

[0004] Existing technologies for preparing gardenia extract mainly include water extraction, alcohol extraction, and supercritical fluid extraction. Water extraction has low extraction efficiency and produces more impurities; although alcohol extraction can improve the dissolution rate of active ingredients, the risk of residual organic solvents and the desolventizing process increase production costs; supercritical fluid extraction equipment is expensive and not suitable for industrial application. Summary of the Invention

[0005] The purpose of this invention is to overcome the shortcomings of the prior art and provide a gardenia flower extract, its preparation method, and its application in anti-wrinkle skincare products. This invention employs a specific process to prepare the gardenia flower extract. First, water-soluble impurities are removed through hydrothermal extraction, followed by a secondary extraction using butylene glycol aqueous solution, effectively improving the purity and application performance of the extract's active ingredients. The gardenia flower extract obtained by this preparation method possesses excellent anti-wrinkle effects and can be widely used as a highly effective anti-wrinkle functional additive in various skincare products.

[0006] To achieve the above objectives, the technical solution adopted by the present invention includes: In a first aspect, the present invention provides a method for preparing gardenia flower extract, comprising the following steps: (1) Add water to gardenia flowers for extraction, filter, and collect the residue; (2) Add butanediol to the filter residue for extraction, filter, and collect the filtrate; (3) Add butanediol to the filtrate to obtain the gardenia extract.

[0007] This invention employs a stepwise extraction process combining water extraction for impurity removal with butylene glycol extraction, offering significant advantages over conventional water and alcohol extraction methods. First, pure water extraction removes water-soluble inorganic salts, polysaccharides, and pigments—impurities with no anti-wrinkle activity—from gardenia flowers, eliminating interfering components and enriching the anti-wrinkle active substances such as polyphenols and flavonoids. Then, butylene glycol, commonly used in skincare systems and known for its gentle and safe properties, is used to dissolve the impurity-removing residue a second time, extracting the active components. Finally, butylene glycol is added to adjust the final product. This process avoids the drawbacks of traditional single-solvent extraction, such as high impurity levels, low activity content, and easy deactivation of the extract through stratification. It fully preserves the anti-wrinkle bioactivity of the extract, resulting in a product with low irritation and good compatibility with various skincare matrices. The process is simple to operate and easy to scale up for production. It can be directly added to skincare products as an anti-wrinkle raw material without additional purification steps, balancing extraction efficiency, product safety, and industrial application advantages.

[0008] Preferably, the mass ratio of gardenia flowers to water is 1:(1-5), and the water extraction conditions are: extraction at 30-80℃ for 0.5-3 hours.

[0009] More preferably, in step (1), the mass ratio of gardenia flowers to water is 1:4, and the extraction conditions are: extraction at 40°C for 3 hours.

[0010] Experimental research revealed that limiting the water extraction ratio of gardenia flowers to water to 1:(1-5), the temperature range of 30-80℃, and the extraction time range of 0.5-3h can precisely balance the elution efficiency of water-soluble impurities with the loss of gardenia polyphenols and flavonoids, which are active anti-wrinkle substances. If the material-to-liquid ratio is too low, impurities will not dissolve sufficiently; if it is too high, the active ingredients will be easily damaged. Insufficient temperature and time will not be enough to remove inorganic salts, water-soluble polysaccharides, and other ineffective impurities. If the temperature is too high or the extraction time is too long, the active substances will be easily oxidized and deactivated. The optimal parameters of 1:4 material-to-liquid ratio with constant temperature extraction at 40℃ for 3h can filter out water-soluble impurities without skin care activity to the maximum extent while retaining the target anti-wrinkle active components completely. The process conditions are mild and controllable, which can lay the best raw material foundation for the subsequent extraction of high-activity and high-purity gardenia anti-wrinkle extract with butylene glycol.

[0011] Preferably, in step (1), the particle size of the gardenia is 40-80 mesh; the filtration mesh size is 100-500 mesh.

[0012] Preferably, in step (2), the mass ratio of gardenia to butylene glycol is 1:(1-3), the extraction conditions for butylene glycol are: extraction at 30-60℃ for 0.5-5h, and the mass concentration of butylene glycol is 30-50%.

[0013] More preferably, in step (2), the mass ratio of gardenia to butylene glycol is 1:2, the extraction conditions for butylene glycol are: extraction at 40°C for 3 hours, and the mass concentration of butylene glycol is 40%.

[0014] Experimental research revealed that limiting the process parameters to a 1:(1-3) ratio of gardenia to butylene glycol, a 30%-50% butylene glycol concentration, and extraction at 30-60℃ for 0.5-5 hours precisely matches the dissolution characteristics of gardenia polyphenols and flavonoids, which are active ingredients for anti-wrinkle activity. A lower ratio, insufficient solvent concentration, or inadequate temperature and time will result in incomplete dissolution of active substances, significantly reducing the anti-wrinkle efficacy of the extract. Excessive solvent usage, high concentration, or exceeding temperature and time limits not only increases production costs but also easily dissolves trace amounts of harmless impurities and induces oxidative degradation of active ingredients. The preferred range of this invention balances active dissolution rate with production economy. The optimal parameters of a 1:2 ratio of gardenia to butylene glycol, 40% butylene glycol, and extraction at 40℃ for 3 hours maximize the dissolution of the target anti-wrinkle active ingredients. The mild conditions throughout the process do not damage the structure of the active substances, resulting in an extract with fewer impurities, higher activity content, and better compatibility with cosmetic matrices. This provides the best extraction process for preparing high-performance gardenia anti-wrinkle extracts.

[0015] Preferably, in step (2), the filter mesh size is 100-500 mesh.

[0016] Preferably, in step (3), the mass concentration of butanediol is 30-100%, and the amount of butanediol added is such that the mass of the filtrate is 1-4 times the mass of the gardenia.

[0017] More preferably, in step (3), the mass concentration of butanediol is 40%, and the amount of butanediol added is such that the mass of the filtrate is twice the mass of the gardenia.

[0018] Experimental research revealed that step (3) with a butylene glycol concentration of 30-100% and a total system mass of 1-4 times that of gardenia flowers effectively controlled the concentration of active ingredients in the gardenia extract, as well as the viscosity and storage stability of the system. If the butylene glycol concentration was too low, the total system mass would be too large, which would reduce the solubility of the active ingredients, dilute anti-wrinkle active ingredients such as polyphenols and flavonoids, and reduce the skin care efficacy. If the butylene glycol concentration was too high or the total system mass was too small, the extract would have a high viscosity, making it difficult to blend with skin care bases such as lotions and serums, and problems such as layering and precipitation would easily occur. The optimal solution of using 40% butylene glycol to adjust to twice the mass of the raw material can maintain the appropriate content of active ingredients in the extract to ensure the anti-wrinkle effect, and also give the extract moderate fluidity and compatibility, inhibit the oxidation and inactivation of active ingredients, and allow for long-term stable storage without additional stabilizers, making it directly compatible with the formulation and production of various anti-wrinkle skin care products, taking into account both performance and product stability.

[0019] The above three-step process parameters are progressive and mutually supportive. The preceding steps reduce impurity interference and improve the extraction efficiency of the subsequent steps. The subsequent steps stabilize the active ingredients enriched in the first two steps. The synergy of the three can effectively avoid defects such as loss of activity, excessive impurities, and poor formula compatibility caused by imbalance of parameters in a single process. Finally, a highly active, highly stable gardenia extract suitable for anti-wrinkle skin care products is obtained.

[0020] Secondly, the present invention provides a gardenia extract prepared by the preparation method described above.

[0021] Thirdly, the present invention provides the application of the gardenia extract in the preparation of anti-wrinkle products.

[0022] The gardenia extract prepared by the specific process of this invention, when applied to the skin, can effectively reduce the proportion of wrinkles and significantly improve skin elasticity. It works synergistically to fade wrinkles and enhance skin elasticity, and has excellent and stable anti-wrinkle skin care effects.

[0023] Preferably, the dosage form of the product includes at least one of creams, lotions, aqueous solutions, gels, oils, powders, muds, aerosols, patches, and films.

[0024] Compared with the prior art, the beneficial effects of the present invention are as follows: (1) The preparation process of gardenia extract of the present invention is simple, the process is highly controllable, the overall process gradient is reasonable and the operation is simple. Only two extraction steps are required to complete the preparation of the extract, which greatly simplifies the traditional preparation process and reduces production energy consumption. (2) The gardenia extract prepared by the present invention has excellent skin care and anti-wrinkle effects and can be effectively applied in the field of anti-wrinkle skin care products. According to human efficacy test, the extract can effectively reduce the proportion of skin wrinkles, and at the same time significantly improve skin elasticity, improve skin laxity and aging problems, and has outstanding skin care and anti-wrinkle effects. (3) The gardenia extract prepared by this invention has high purity and good safety. The entire preparation process of the product is free of organic solvent residues such as ethanol, which completely avoids the problems of skin irritation and use risks caused by solvent residues. The product safety and performance are superior to existing similar products on the market, and its market application advantages are obvious. Detailed Implementation

[0025] To better illustrate the objectives, technical solutions, and advantages of this invention, the invention will be further described below with reference to specific embodiments. Those skilled in the art should understand that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

[0026] Unless otherwise specified, all raw materials used in the following examples and comparative examples are commercially available general-purpose materials.

[0027] Example 1 This embodiment provides a method for preparing gardenia flower extract, including the following steps: (1) Weigh 0.5 kg of dried gardenia flowers, grind them to 60 mesh, and set aside; (2) Add 2 kg of deionized water to the crushed gardenia flowers and reflux at 40°C for 3 h. After extraction, filter through 200 mesh and collect the residue for later use. (3) Add 1 kg of 40% butanediol aqueous solution to the filter residue in step (2), reflux and extract at 40°C for 3 h. After extraction, filter through 300 mesh and keep the filtrate for later use. (4) Add 40% butanediol aqueous solution to the filtrate obtained in step (3) so that the total mass of the filtrate is 1 kg, and obtain gardenia extract.

[0028] Example 2 This embodiment provides a method for preparing gardenia flower extract, including the following steps: (1) Weigh 0.5 kg of dried gardenia flowers, grind them to 80 mesh, and set aside; (2) Add 1 kg of deionized water to the crushed gardenia flowers and reflux at 70°C for 1 h. After extraction, filter through 100 mesh and collect the residue for later use. (3) Add 0.6 kg of 50% butanediol aqueous solution to the filter residue in step (2), reflux and extract at 30°C for 4 h. After extraction, filter through 200 mesh and keep the filtrate for later use. (4) Add 50% butanediol aqueous solution to the filtrate obtained in step (3) so that the total mass of the filtrate is 1 kg, and obtain gardenia extract.

[0029] Example 3 This embodiment provides a method for preparing gardenia flower extract, including the following steps: (1) Weigh 0.5 kg of dried gardenia flowers, grind them to 40 mesh, and set aside; (2) Add 2 kg of deionized water to the crushed gardenia flowers and reflux at 30°C for 3 h. After extraction, filter through 100 mesh and collect the residue for later use. (3) Add 1 kg of 40% butanediol aqueous solution to the filter residue in step (2), reflux and extract at 30°C for 3 h. After extraction, filter through 200 mesh and keep the filtrate for later use. (4) Add 100% butanediol aqueous solution to the filtrate obtained in step (3) so that the total mass of the filtrate is 1 kg, and obtain gardenia extract.

[0030] Example 4 This embodiment provides a method for preparing gardenia flower extract, including the following steps: (1) Weigh 0.5 kg of dried gardenia flowers, grind them to 40 mesh, and set aside; (2) Add 2.5 kg of deionized water to the crushed gardenia flowers and reflux at 30°C for 3 hours. After extraction, filter through a 500 mesh and collect the residue for later use. (3) Add 1.5 kg of 30% butanediol aqueous solution to the filter residue in step (2), reflux and extract at 30°C for 5 h. After extraction, filter through 500 mesh and keep the filtrate for later use. (4) Add 30% butanediol aqueous solution to the filtrate obtained in step (3) to make the total mass of the filtrate 2kg, and obtain gardenia extract.

[0031] Example 5 This embodiment provides a method for preparing gardenia flower extract, including the following steps: (1) Weigh 1 kg of dried gardenia flowers, grind them to 80 mesh, and set aside; (2) Add 1 kg of deionized water to the crushed gardenia flowers and reflux at 80°C for 0.5 h. After extraction, filter through 100 mesh and collect the residue for later use. (3) Add 1 kg of 50% butanediol aqueous solution to the filter residue in step (2), reflux and extract at 60°C for 0.5 h. After extraction, filter through 100 mesh and keep the filtrate for later use. (4) Add 100% butanediol aqueous solution to the filtrate obtained in step (3) so that the total mass of the filtrate is 1 kg, and obtain gardenia extract.

[0032] Comparative Example 1 This comparative example provides a method for preparing gardenia extract, which differs from Example 1 only in that: in step (2), 4 kg of deionized water (material-to-liquid ratio of 1:8) is added to the pulverized gardenia flowers, and the mixture is refluxed at 20°C for 3.5 h.

[0033] Comparative Example 2 This comparative example provides a method for preparing gardenia extract, which differs from Example 1 only in that: in step (2), 0.3 kg of deionized water (material-liquid ratio of 5:3) is added to the pulverized gardenia flowers, and the mixture is refluxed at 90°C for 0.3 h.

[0034] Comparative Example 3 This comparative example provides a method for preparing gardenia extract, which differs from Example 1 only in that: in step (3), the mass concentration of butylene glycol in the butylene glycol aqueous solution is 60%, and the extraction is carried out by reflux at 20°C for 5.5 h.

[0035] Comparative Example 4 This comparative example provides a method for preparing gardenia extract, which differs from Example 1 only in that: in step (3), the mass concentration of butylene glycol in the butylene glycol aqueous solution is 20%, and the extraction is carried out by reflux at 70°C for 0.3 h.

[0036] Comparative Example 5 This comparative example provides a method for preparing gardenia extract, which differs from Example 1 only in that: in step (3), an aqueous ethanol solution with a mass concentration of 40% is used instead of an aqueous butylene glycol solution.

[0037] Comparative Example 6 This comparative example provides a method for preparing gardenia extract, including the following steps: (1) Weigh 0.5 kg of dried gardenia flowers, grind them to 60 mesh, and set aside; (2) Add 7.5L of 50% ethanol aqueous solution to the crushed gardenia flowers, reflux at 80℃ for 1h, filter through 300 mesh after extraction, and keep the filtrate for later use. (3) Add 40% butanediol aqueous solution to the filtrate obtained in step (2) to make the total mass of the filtrate 1kg, and obtain gardenia extract.

[0038] Test case This test example uses gardenia extracts prepared by the methods described in Examples 1-5 and Comparative Examples 1-6 as test samples to test their anti-wrinkle efficacy. The specific methods are as follows: (1) Required equipment: facial image imaging system, skin elasticity test probe.

[0039] (2) Testing method: The test shall be conducted in accordance with T / CAB 0152-2022 "Test method for seven effects of cosmetics: anti-wrinkle, firming, moisturizing, oil control, repair, nourishing and soothing".

[0040] One hundred and twenty participants, aged 35-55 years, were randomly divided into 12 groups of 10 each. After cleansing their faces with an alkaline soap-based facial cleanser under guidance, the participants were placed in a constant temperature and humidity environment of 21±1℃ and 50±10%RH for 30 minutes to acclimatize. Baseline skin values ​​were measured before product use (D0), including the percentage of wrinkled skin area and the skin elasticity parameter R², and these values ​​were recorded. The product was used continuously for 21 days according to the instructions, and the same tests were performed again after 21 days of use (D21).

[0041] (3) Sample preparation: The samples were prepared into 2.5% (w / w) gardenia extract solutions (containing 2.5% gardenia extract and 97.5% water) for testing. Pure water was used as a solvent control.

[0042] The specific test results are shown in Table 1-2.

[0043] Table 1. Results of detection indicators before and after sample use. Table 2. Results of differences for each detection indicator Table 1-2 shows that after subjects used the test samples containing gardenia extract prepared by the process of this invention for 21 consecutive days, compared with their baseline state before product use, the proportion of skin wrinkles decreased significantly and the skin elasticity index R2 increased significantly (P < 0.05). Simultaneously, compared with the blank solvent group, the test samples significantly reduced the difference in wrinkle area proportion and increased the difference in elasticity parameter R2. The above test results confirm that the gardenia extract prepared by the specific process of this invention possesses good anti-wrinkle activity in the human body.

[0044] When the parameters of the water extraction process in Comparative Examples 1-2 and the parameters of the butanediol extraction in Comparative Examples 3-4 deviate from the preferred range of the present invention, after 21 days of human trials, the improvement in wrinkles and the increase in elasticity of the samples are significantly worse than those of the examples, and the anti-wrinkle effect is greatly reduced.

[0045] Comparative Example 5 only replaced the extraction solvent with ethanol, while the other process parameters were completely consistent with the Example. The effect of this sample in reducing wrinkles and enhancing skin elasticity was still inferior to that of Example 1. This shows that butylene glycol as the extraction solvent is a key condition for ensuring the anti-wrinkle activity of gardenia extract, and ethanol substitution will significantly weaken the efficacy of the extract.

[0046] Comparative Example 6 used commercially available general ethanol extraction technology to prepare gardenia extract. After 21 days of human trial, there was no statistically significant difference between the difference in wrinkle area ratio and the difference in skin elasticity R2 compared with the blank solvent group, proving that the gardenia extract obtained by conventional ethanol extraction does not have a significant anti-wrinkle effect.

[0047] Finally, it should be noted that the above embodiments are used to illustrate the technical solutions of the present invention and not to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A method for preparing gardenia flower extract, characterized in that, Includes the following steps: (1) Add water to gardenia flowers for extraction, filter, and collect the residue; (2) Add butanediol to the filter residue for extraction, filter, and collect the filtrate; (3) Add butanediol to the filtrate to obtain the gardenia extract.

2. The preparation method according to claim 1, characterized in that, In step (1), the mass ratio of gardenia flowers to water is 1:(1-5), and the water extraction conditions are: extraction at 30-80℃ for 0.5-3h.

3. The preparation method according to claim 2, characterized in that, In step (1), the mass ratio of gardenia flowers to water is 1:4, and the extraction conditions are: extraction at 40℃ for 3 hours.

4. The preparation method according to claim 1, characterized in that, In step (2), the mass ratio of gardenia to butylene glycol is 1:(1-3), the extraction conditions for butylene glycol are: extraction at 30-60℃ for 0.5-5h, and the mass concentration of butylene glycol is 30-50%.

5. The preparation method according to claim 4, characterized in that, In step (2), the mass ratio of gardenia to butylene glycol is 1:2, and the extraction conditions for butylene glycol are: extraction at 40℃ for 3 hours, and the mass concentration of butylene glycol is 40%.

6. The preparation method according to claim 1, characterized in that, In step (3), the mass concentration of butanediol is 30-100%, and the amount of butanediol added is such that the mass of the filtrate is 1-4 times the mass of the gardenia.

7. The preparation method according to claim 6, characterized in that, In step (3), the mass concentration of butanediol is 40%, and the amount of butanediol added is such that the mass of the filtrate is twice the mass of the gardenia.

8. A gardenia extract prepared by the method according to any one of claims 1-7.

9. The use of the gardenia extract as described in claim 8 in the preparation of anti-wrinkle products.

10. The application as described in claim 9, characterized in that, The dosage form of the product includes at least one of creams, lotions, aqueous solutions, gels, oils, powders, muds, aerosols, patches, and films.

Images