Preparation method of a lemon fruit extract containing eriodictyol and application thereof in soothing

Abstract

This invention belongs to the field of cosmetic technology, specifically relating to a method for preparing a lemon fruit extract containing sennaol and its application in soothing. This invention provides a method for preparing a lemon fruit extract containing sennaol, utilizing the strong penetration and dissolving power of a green solvent and the high selectivity of enzymatic reactions to achieve not only efficient extraction and conversion of sennaol but also naturally endowing the final product with excellent water solubility and chemical stability. The prepared lemon fruit extract can be directly applied to water-based formulations without complex modification or the addition of large amounts of co-solvents, maintaining potent skin-soothing activity. The entire process is gentle and safe, with no irritating organic solvents or strong acid residues, making it particularly suitable for cosmetic development targeting sensitive skin.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, specifically relating to a method for preparing lemon fruit extract containing sennaol and its application in soothing. Background Technology

[0002] Eriodictyol is a naturally occurring dihydroflavonoid compound widely found in plants such as lemons and citrus fruits. Studies have shown that eriodictyol possesses remarkable antioxidant, anti-inflammatory, and tyrosinase-inhibiting bioactivities. In the skincare field, these properties translate into significant potential for soothing and repairing, reducing skin irritation, combating photoaging, and aiding in skin whitening, making it a promising high-end functional cosmetic ingredient. However, eriodictyol faces two major bottlenecks in its cosmetic applications: firstly, its extremely poor water solubility makes it difficult to directly formulate into water-based cosmetic systems, resulting in low bioavailability; secondly, the phenolic hydroxyl groups in its molecular structure make it sensitive to environmental factors such as light, heat, and oxygen, easily degrading and inactivating during processing and storage, making it difficult to guarantee product stability.

[0003] In existing technologies, the extraction of sennaol or its aglycone precursors mostly employs organic solvent methods (such as methanol and ethanol), which pose risks of skin irritation and solvent residue, and have limited selectivity. To improve aglycone yield, vigorous strong acid hydrolysis processes are often used, which easily destroy the active structure of sennaol and generate unnecessary byproducts, and the residual acids can easily irritate the skin. Subsequent attempts to improve solubility usually rely on chemical modification or the addition of large amounts of solubilizers, which may introduce new irritants or affect the mildness of the formulation. Therefore, developing a green preparation process that can simultaneously achieve efficient extraction, targeted transformation, and naturally impart high water solubility and high stability to the product is crucial for promoting the application of this active ingredient. Summary of the Invention

[0004] In view of the above-mentioned defects or improvement needs of the existing technology, the present invention provides a method for preparing lemon fruit extract containing sennaol, which can simultaneously achieve efficient extraction, targeted conversion, and naturally endow the product with high water solubility and high stability in a green preparation, thereby promoting the application of sennaol in cosmetic products.

[0005] The objective of this invention can be achieved through the following technical solutions: The first aspect of the present invention provides a method for preparing a lemon fruit extract containing sennaol, comprising the following steps: drying and pulverizing lemon peel, adding it to an aqueous solution of a eutectic solvent for ultrasonic extraction, adding glycosidase for enzymatic hydrolysis after extraction, collecting the hydrolysis product, centrifuging, filtering, and taking the supernatant to obtain the lemon fruit extract containing sennaol.

[0006] Preferably, the aqueous solution of the eutectic solvent consists of a hydrogen bond acceptor, a hydrogen bond donor, and water.

[0007] Preferably, the hydrogen bond acceptor includes at least one of betaine, choline chloride, glycine, and L-proline.

[0008] Preferably, the hydrogen bond donor includes at least one of glycerol, urea, allantoin, panthenol, 1,3-propanediol, 1,2-propanediol, ethylene glycol, butylene glycol, 1,3-butanediol, 1,4-butanediol, arginine, lysine, proline, glycine, alanine, and malic acid.

[0009] More preferably, the hydrogen bond donor is betaine, and the hydrogen bond donor is panthenol or arginine.

[0010] Preferably, the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:(1-4).

[0011] More preferably, the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:(2-3).

[0012] More preferably, the molar ratio of panthenol to arginine is (20-40):1.

[0013] More preferably, the molar ratio of panthenol to arginine is (25-35):1.

[0014] Preferably, the total mass concentration of hydrogen bond acceptors and hydrogen bond donors in the eutectic solvent is 60%-90%.

[0015] More preferably, the total mass concentration of hydrogen bond acceptors and hydrogen bond donors in the eutectic solvent is 70%-80%.

[0016] Preferably, the ratio of lemon peel to eutectic solvent is 1g:(5-20)mL.

[0017] Preferably, the ultrasonic extraction temperature is 40-60℃, the power is 100-200W, and the time is 30-60min.

[0018] More preferably, the ultrasonic extraction temperature is 50-55℃, the power is 120-150W, and the time is 40-50min.

[0019] Preferably, the glycosidase includes at least one of β-glucosidase, α-L-rhamnosidase, and rutinase.

[0020] More preferably, the glycosidase is β-glucosidase or α-L-rhamnosidase in a concentration ratio of 1:0.5-2.

[0021] Preferably, the concentration of the enzyme in the enzymatic hydrolysis reaction in the system is 100-500 U / L, the enzymatic hydrolysis temperature is 30-50℃, and the time is 30-90 min.

[0022] More preferably, the concentration of the enzyme in the enzymatic hydrolysis reaction in the system is 200-300 U / L, the enzymatic hydrolysis temperature is 40-45℃, and the time is 40-60 min.

[0023] A second aspect of the present invention provides the use of the lemon fruit extract containing sennaol prepared by the preparation method described in the first aspect in the preparation of cosmetics.

[0024] Preferably, the cosmetic includes one or more of the following: toner, lotion, cream, mask, serum, and spray.

[0025] A third aspect of the present invention provides a cosmetic lotion comprising the following components by weight percentage: 1%-10% lemon fruit extract obtained by the preparation method described in the first aspect, 0.05%-0.5% thickener, 0.5%-5% moisturizer, 0.1%-1% antioxidant, 0.01%-0.3% pH adjuster, and the balance being deionized water.

[0026] Preferably, the thickener comprises at least one of the following: polyacrylate crosspolymer-6, carbomer, carrageenan, gellan gum, xanthan gum, microcrystalline cellulose, cellulose gum, ethyl cellulose, strychnine gum, guar gum, ammonium acryloyl dimethyl taurate / VP copolymer, acrylate copolymer, sclerotium gum, polyvinylpyrrolidone, amylopectin, and sodium polyacrylate.

[0027] Preferably, the moisturizer comprises at least one of glycerin, 1,2-butanediol, 1,4-butanediol, 1,2-hexanediol, 1,3-propanediol, 1,2-pentanediol, butylene glycol, caprylyl glycol, dipropylene glycol, tremella polysaccharide, trehalose, betaine, allantoin, hyaluronic acid, sodium hyaluronate, acetylated sodium hyaluronate, hydrolyzed sodium hyaluronate, sodium hyaluronate crosspolymer, β-glucan, budding stalk polysaccharide, and ceramide.

[0028] Preferably, the antioxidant is p-hydroxyacetophenone.

[0029] Preferably, the pH adjuster includes at least one of arginine, disodium ethylenediaminetetraacetate, tromethamine, and citric acid.

[0030] A fourth aspect of the present invention provides a method for preparing the lotion described in the third aspect, comprising the following steps: S1. Mix the thickener with deionized water and stir. Heat to 80-90℃ and homogenize at 1200-1400 rpm for 3-6 minutes to obtain pre-prepared component A. S2. Mix the humectant and antioxidant, heat to 60°C to melt, and obtain pre-prepared component B. S3. After cooling the pre-prepared component A to 60°C, add the pre-prepared component B at a speed of 200-500 rpm and stir to mix. Then cool to below 45°C, add the lemon fruit extract prepared by any one of the preparation methods described in claims 1-5, continue stirring for 5-10 min, and finally add a pH adjuster to adjust the pH. Then stop stirring, discharge the product, and obtain the toner.

[0031] The beneficial effects of this invention are: This invention provides a lemon fruit extract containing senna. The invention utilizes a natural eutectic solvent composed of betaine, panthenol, and arginine as a green extraction medium, combined with ultrasound-assisted technology to efficiently extract senna and its derivative sennagidine from lemon peel. Subsequently, β-glucosidase and α-L-rhamnosidase are used for gentle and specific enzymatic transformation, directionally converting sennagidine into the target active ingredient senna. This integrated process, through the strong penetration and dissolving power of the green solvent and the high selectivity of the enzymatic reaction, not only achieves efficient extraction and transformation of senna but also naturally endows the final product with excellent water solubility and chemical stability. The resulting lemon fruit extract can be directly applied to aqueous formulations without complex modification or the addition of large amounts of co-solvents, maintaining potent skin-soothing activity. The entire process is gentle and safe, with no irritating organic solvents or strong acid residues, making it particularly suitable for cosmetic development targeting sensitive skin. Attached Figure Description

[0032] Figure 1 The images show the redness areas on the faces of volunteers before and 7 days after use in the blank application example and application example 1 in test example 3. Detailed Implementation

[0033] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features and effects of the present invention, in conjunction with embodiments, is provided below.

[0034] Unless otherwise specified, experimental methods in the following examples are generally performed under standard conditions or as recommended by the manufacturer. All materials and reagents used are commercially available unless otherwise specified.

[0035] The lemons were purchased from Pupu Supermarket; the product name is Sichuan Lemon, and the variety is Eureka. β-glucosidase was purchased from Nanjing Jingchang Biotechnology Co., Ltd., product number 129; α-L-rhamnosidase was purchased from Nanjing Jingchang Biotechnology Co., Ltd., catalog number M15.

[0036] Example 1: Preparation method of lemon fruit extract containing sennaol (1) Preparation of eutectic solvent: Betaine, panthenol, and arginine were mixed in a molar ratio of 1:2.9:0.1 to form a mixture. 80g of the mixture was then mixed with 20g of deionized water to obtain a eutectic solvent. The molar ratio of hydrogen bond acceptors to hydrogen bond donors in this eutectic solvent was 1:3, and the total mass concentration was 80%.

[0037] (2) Preparation of lemon fruit extract: Peel the lemon peel, wash it clean, and dry it in a 50°C constant temperature oven until constant weight. Grind and pulverize it, then pass it through an 80-mesh sieve. Take 1g and add it to the eutectic solvent prepared in step (1), with a material-to-liquid ratio of 1g:15mL. Use ultrasonic extraction method with an ultrasonic temperature of 55°C, a power of 150W, and a time of 40min. Add β-glucosidase with a concentration of 100 U / L and α-L-rhamnosidase with a concentration of 200 U / L, and hydrolyze at 45°C for 60min. After collecting the enzymatic hydrolysis product, centrifuge at 10000g for 10min, take the supernatant, and filter it using a 10kDa ultrafiltration membrane to obtain lemon fruit extract containing sennaol. Name the extract as Example 1.

[0038] Example 2: Preparation method of lemon fruit extract containing sennaol (1) Preparation of eutectic solvent: Betaine, panthenol, and arginine were mixed in a molar ratio of 1:1.95:0.05 to form a mixture. 70g of the mixture was then mixed with 30g of deionized water to obtain a eutectic solvent. The molar ratio of hydrogen bond acceptors to hydrogen bond donors in this eutectic solvent was 1:2, and the total mass concentration was 70%.

[0039] (2) Preparation of lemon fruit extract: Peel the lemon peel, wash it clean, and dry it in a 50℃ constant temperature oven until constant weight. Grind and pulverize it, then pass it through an 80-mesh sieve. Take 1 g and add it to the eutectic solvent prepared in step (1), with a material-to-liquid ratio of 1 g: 10 mL. Use ultrasonic extraction method with an ultrasonic temperature of 50℃, a power of 120W, and a time of 50 min. Add β-glucosidase with a concentration of 130 U / L and α-L-rhamnosidase with a concentration of 70 U / L, and hydrolyze at 40℃ for 40 min. After collecting the enzymatic hydrolysis product, centrifuge at 10000g speed for 10 min, take the supernatant, and filter it using a 10kDa ultrafiltration membrane to obtain lemon fruit extract containing sennaol. Name the extract as Example 2.

[0040] Example 3: Preparation method of lemon fruit extract containing sennaol (1) Preparation of eutectic solvent: Betaine, panthenol, and arginine were mixed in a molar ratio of 1:3.95:0.05 to form a mixture. 90g of the mixture was then mixed with 10g of deionized water to obtain a eutectic solvent. The molar ratio of hydrogen bond acceptors to hydrogen bond donors in this eutectic solvent was 1:4, and the total mass concentration was 90%.

[0041] (2) Preparation of lemon fruit extract: Peel the lemon peel, wash it clean, and dry it in a 50℃ constant temperature oven until constant weight. Grind and pulverize the powder, then pass it through an 80-mesh sieve. Take 1 g of the powder and add it to the above-mentioned eutectic solvent at a material-to-liquid ratio of 1 g: 20 mL. Use ultrasonic extraction method with an ultrasonic temperature of 60℃, a power of 200W, and a time of 30 min. Add β-glucosidase at a concentration of 400 U / L and α-L-rhamnosidase at a concentration of 100 U / L, and hydrolyze at 50℃ for 90 min. Collect the enzymatic hydrolysis product and centrifuge at 10000g for 10 min. Take the supernatant and filter it using a 10 kDa ultrafiltration membrane to obtain lemon fruit extract containing sennaol. This extract is named Example 3.

[0042] Example 4: Preparation method of lemon fruit extract containing sennaol (1) Preparation of eutectic solvent: Betaine, panthenol, and arginine were mixed in a molar ratio of 1:0.9:0.1 to form a mixture. 60g of the mixture was then mixed with 40g of deionized water to obtain a eutectic solvent. The molar ratio of hydrogen bond acceptors to hydrogen bond donors in this eutectic solvent was 1:1, and the total mass concentration was 60%.

[0043] (2) Preparation of lemon fruit extract: Peel the lemon peel, wash it clean, and dry it in a 50℃ constant temperature oven until constant weight. Grind and pulverize the powder, then pass it through an 80-mesh sieve. Take 1 g of the powder and add it to the above-mentioned eutectic solvent at a material-to-liquid ratio of 1 g: 5 mL. Use ultrasonic extraction method at 40℃, 100W, and 60 min. Add β-glucosidase at a concentration of 30 U / L and α-L-rhamnosidase at a concentration of 70 U / L, and hydrolyze at 30℃ for 30 min. Collect the enzymatic hydrolysis product and centrifuge at 10000g for 10 min. Take the supernatant and filter it using a 10 kDa ultrafiltration membrane to obtain lemon fruit extract containing sennaol. This extract is named Example 4.

[0044] Example 5 Compared with the preparation method of Example 1, the only difference is the choice of hydrogen bond acceptor, that is, choline chloride is used instead of betaine. All other steps are exactly the same as those in Example 1.

[0045] Example 6 Compared with the preparation method of Example 1, the only difference is the choice of hydrogen bond donor, that is, 1,3-propanediol is used instead of panthenol and arginine. All other steps are exactly the same as those in Example 1.

[0046] Example 7 Compared with the preparation method of Example 1, the only difference is the choice of hydrogen bond donor, that is, panthenol is not added, and an equal amount of arginine is used to make up the missing amount. All other steps are exactly the same as those in Example 1.

[0047] Example 8 Compared with the preparation method of Example 1, the only difference is the choice of hydrogen bond donor, that is, arginine is not added, and an equal amount of panthenol is used to make up the missing amount. All other steps are exactly the same as those in Example 1.

[0048] Comparative Example 1 Compared with the preparation method of Example 1, only the molar ratio of hydrogen bond acceptor and hydrogen bond donor and the total mass concentration of hydrogen bond acceptor and hydrogen bond donor are different. The molar ratio of hydrogen bond acceptor and hydrogen bond donor is 1:0.5 (of which the molar ratio of panthenol and arginine is 2.9:0.1) and the total mass concentration of hydrogen bond acceptor and hydrogen bond donor is 50%. All other steps are exactly the same as those in Example 1.

[0049] Comparative Example 2 Compared with the preparation method of Example 1, only the molar ratio of hydrogen bond acceptor and hydrogen bond donor and the total mass concentration of hydrogen bond acceptor and hydrogen bond donor are different. The molar ratio of hydrogen bond acceptor and hydrogen bond donor is 1:5 (where the molar ratio of panthenol and arginine is 2.9:0.1) and the total mass concentration of hydrogen bond acceptor and hydrogen bond donor is 100%. All other steps are exactly the same as in Example 1.

[0050] Comparative Example 3 Compared with the preparation method of Example 1, only the ratio of lemon peel to eutectic solvent and the ultrasonic temperature, power and time are different. The ratio of lemon peel to eutectic solvent in this comparative example is 1g:3mL, the ultrasonic temperature is 30℃, the power is 80W and the time is 20min. All other steps are exactly the same as in Example 1.

[0051] Comparative Example 4 Compared with the preparation method of Example 1, only the ratio of lemon peel to eutectic solvent and the ultrasonic temperature, power and time are different. The ratio of lemon peel to eutectic solvent in this comparative example is 1g:30mL, the ultrasonic temperature is 70℃, the power is 250W and the time is 80min. All other steps are exactly the same as in Example 1.

[0052] Comparative Example 5 Compared with the preparation method of Example 1, only the enzyme concentration, enzymatic hydrolysis temperature and enzymatic hydrolysis time are different. In this comparative example, the concentrations of β-glucosidase and α-L-rhamnosidase are 20 U / L and 40 U / L, respectively, the enzymatic hydrolysis temperature is 20℃ and the time is 20 min. All other steps are exactly the same as in Example 1.

[0053] Comparative Example 6 Compared with the preparation method of Example 1, only the enzyme concentration, enzymatic hydrolysis temperature and enzymatic hydrolysis time are different. In this comparative example, the concentrations of β-glucosidase and α-L-rhamnosidase are 200 U / L and 400 U / L, respectively, the enzymatic hydrolysis temperature is 60℃ and the time is 120 min, and the rest of the steps are exactly the same as those in Example 1.

[0054] Comparative Example 7: Preparation method of lemon fruit extract containing sennaol Peel the lemon peel, wash it clean, and dry it in a 50℃ constant temperature oven until constant weight. Grind and pulverize the powder, then pass it through an 80-mesh sieve. Take 1 g of the powder and add an aqueous solution of 75% ethanol (mass percentage) at a material-to-liquid ratio of 1 g: 10 mL. Use ultrasonic extraction at 50℃, 150W, and 30 min. Collect the product, centrifuge, and take the supernatant to obtain the lemon fruit extract containing sennaol. Name the extract as Comparative Example 7.

[0055] Comparative Example 8: Preparation method of lemon fruit extract containing sennaol Peel the lemon peel, wash it clean, and dry it in a 50℃ constant temperature oven until constant weight. Grind and pulverize the powder, then pass it through an 80-mesh sieve. Take 1 g of the powder and add pure water at a ratio of 1 g to 10 mL. Use ultrasonic extraction at 50℃, 150 W, and 30 min. Collect the product, centrifuge, and take the supernatant to obtain the lemon fruit extract containing sennaol. Name the extract as Comparative Example 8.

[0056] Comparative Example 9 Compared with the preparation method of Example 1, only the material extraction is different, that is, lemon leaves are used instead of lemon peels, and the rest of the steps are exactly the same as those of Example 1.

[0057] Test Example 1: Content, stability, and water solubility of sennaol Determination of senna content: 1 mL of lemon fruit extract prepared in Examples 1-8 and Comparative Examples 1-9 was accurately measured, diluted in 9 mL of methanol, filtered through a 0.22 μm filter membrane, and the senna content in the extract was determined by high performance liquid chromatography (HPLC). A gradient concentration standard solution of senna (purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., catalog number E138993) was prepared with methanol, and a standard curve was plotted. The senna content M0 in the sample was calculated according to the standard curve formula. The chromatographic column used was a C18 column (100 mm × 2.1 mm, 3 μM), the mobile phase was 60% methanol, the flow rate was 0.5 mL / min, and the sample loading volume was 10 μL. Stability test: 5 mL of lemon fruit extract prepared in Examples 1-8 and Comparative Examples 1-9 were measured into 10 mL transparent sealed PE bottles and placed at 4℃, 25℃, and 50℃ respectively, and irradiated with a 15W light. The content of sennaol M1 was then measured on the 7th day, using the same method as for sennaol M0. The retention rate of sennaol was then calculated as: sennaol retention rate = M1 / M0 × 100%. Water solubility test: 1 mL of lemon fruit extract prepared in Examples 1-8 and Comparative Examples 1-9 was accurately measured, diluted in 9 mL of pure water, centrifuged at 10000g for 10 min, and the supernatant was collected. After filtration through a 0.22 μm filter membrane, the content of sennaol M2 in the extract was determined by high performance liquid chromatography. The detection method was the same as that for sennaol content M0. Then the water solubility of sennaol was calculated as follows: water solubility of sennaol = M2 / M0 × 100%. The results are shown in Table 1: Table 1. Conversion rate data of sennaol

[0058] According to the results in Table 1, 1) comparing the results of Examples 1-4 with those of Comparative Examples 7-8, it can be seen that the preparation method of this application is significantly better than the alcohol / water extraction method. Furthermore, the components of the eutectic solvent have a significant impact on the extraction efficiency, stability, and water solubility of sennaol. The eutectic solvent composed of betaine, panthenol, and arginine resulted in higher sennaol content, stability, and water solubility in the lemon fruit extract prepared in the examples, producing unexpected technical effects. 2) comparing the results of Examples 1-4 with those of Comparative Examples 1-2 reveals that the molar ratio of hydrogen bond acceptors to hydrogen bond donors and the total mass concentration also affect the extraction efficiency, stability, and water solubility of sennaol. The experiments in this application demonstrate the effects of hydrogen bond acceptors and hydrogen bond donors. The experiment showed good results when the molar ratio was in the range of 1:(1-4) and the total mass concentration of hydrogen bond acceptor and hydrogen bond donor was in the range of 60%-90%; 3) Comparing the results of Examples 1-4 with Comparative Examples 3-6, it can be seen that the material-liquid ratio in the preparation process, as well as the temperature, power, and time of ultrasound and the enzyme concentration, temperature, and time of enzymatic hydrolysis, all have a certain impact on the content and stability of sennaol; 4) Comparing the results of Example 1 with Comparative Example 9 shows that even for different parts of the same plant, the eutectic solvent is not universal because of the different compositions of different parts. The experiment of this invention proves that the eutectic solvent composed of betaine, panthenol, arginine and water is only suitable for the efficient extraction of sennaol from lemon fruit.

[0059] Application Example 1-10 and Comparative Application Example 1-9 The present invention provides a toner in application examples and comparative application examples, the components (mass percentage) of which are shown in Table 2; wherein, the lemon fruit extract used in application examples 1-8 are the lemon fruit extracts prepared in examples 1-8 respectively, and the lemon fruit extract used in application examples 9-10 is the lemon fruit extract prepared in example 1; the lemon fruit extract used in comparative application examples 1-9 are the lemon fruit extracts prepared in comparative examples 1-9 respectively; in addition, a blank application example is set up, the only difference between the blank application example and application example 1 is that no lemon fruit extract is added.

[0060] Table 2

[0061] The method for preparing the toner provided in Example 1 includes the following steps: (1) Mix the thickener with deionized water and stir. Heat to 85°C and homogenize at 1300 rpm for 4 min to obtain pre-prepared component A. (2) Mix the humectant and antioxidant, heat to 60°C to melt, and obtain the pre-prepared component B; (3) After cooling the pre-prepared component A to 60°C, add the pre-prepared component B at 300 rpm and stir to mix. Then cool to below 45°C and add lemon fruit extract. Continue stirring for 8 minutes. Finally, add pH adjuster to adjust pH, then stop stirring, discharge the product, and obtain the toner.

[0062] The preparation methods of the toners provided in Application Examples 2-10, Comparative Application Examples 1-9, and Blank Application Examples are consistent with those in Application Example 1. If the relevant components are not available, they can be omitted.

[0063] Test Example 2: Safety Test of Human Patch Thirty volunteers were recruited, 15 men and 15 women, aged 20-50 years. A closed patch test method was used. Equal volumes of 0.020 mL of test samples (toners prepared in Application Examples 1-10, Control Application Examples 1-9, and Blank Application Examples) were placed in a specific patch applicator. The patch was then applied to the volunteers' arms with hypoallergenic adhesive tape, and gently pressed to ensure even application to the skin. The patch was left on for 24 hours. The blank control group used distilled water, and the blank application examples used toners without lemon fruit extract. After 24 hours, the patch applicator was removed, and skin reactions were observed and recorded at 0.5 hours, 24 hours, and 48 hours. The severity of adverse skin reactions is shown in Table 3 below.

[0064] Table 3. Adverse skin reaction grades Rating levels Skin reaction 0 negative reaction 1 Suspicious reaction, only slight erythema 2 Weak positive reaction (erythema reaction): erythema, infiltration, edema, and papules may be present. 3 Strong positive reaction (herpes reaction): erythema, infiltration, edema, papules; the reaction may extend beyond the test area. 4 Extremely strong positive reaction (confluent herpes simplex reaction): obvious erythema, severe infiltration, edema, confluent herpes simplex; reaction extends beyond the test area. The results of the human skin patch test showed that the skin reactions of volunteers in the application examples 1-10, the control examples 1-9, and the blank application examples were observed after 0.5 h, 24 h, and 48 h. No adverse skin reactions were observed in any of them, and all were negative reactions. This indicates that the toner prepared by the skin care composition provided by the present invention is safe and non-irritating to human skin.

[0065] Test Example 3: Human Efficacy Trial Experimental Methods: Following the "Cosmetic Safety Technical Specifications" (2015), 120 Asian adults aged 18-60 years with self-reported skin sensitivity were selected and randomly divided into 20 groups of 6 participants each. Volunteers applied the sample to their entire face twice daily (morning and evening). The samples were toners prepared from Application Examples 1-10, Comparative Examples 1-9, and the blank application example. Data was collected on Day 0 (D0) and Day 7 (D7). After the visits, volunteers washed their faces with facial cleanser and sat quietly for 30 minutes in an air-conditioned room at 21±1℃ and 50±10% humidity. Researchers then used a Visia-7 to photograph the volunteers' faces. Image analysis was performed on the exported red area images to obtain the a* value. Skin soothing ability was represented by the a* value improvement rate; a higher a* value improvement rate indicated a better soothing effect on the skin. The formula for the a* value improvement rate is as follows: a* value improvement rate = (a* value D0 - a* value D7) / a* value D0 × 100%; In the formula: a* value D0 is the a* value on day 0; a* value D7 is the a* value on day 7; The results were averaged, as shown in Table 4. Table 4 Results of Human Efficacy Trials Group a* value improvement rate (%) Blank application example 2.07 Application Example 1 25.74 Application Example 2 23.56 Application Example 3 19.18 Application Example 4 21.35 Application Example 5 19.03 Application Example 6 16.92 Application Example 7 15.30 Application Example 8 17.26 Application Example 9 16.15 Application Example 10 28.21 Comparative Application Example 1 7.35 Comparative Application Example 2 8.14 Comparative Application Example 3 12.02 Comparative Application Example 4 10.47 Comparative Application Example 5 11.25 Comparative Application Example 6 13.68 Comparative Application Example 7 5.59 Comparative Application Example 8 3.24 Comparative Application Example 9 3.75 The results in Table 4 show that the improvement rate of a* value in Application Examples 1-10 was significantly higher than that in Comparative Application Examples 1-9, indicating that the toner containing lemon fruit extract containing sennaol obtained by the preparation method of this application has a better soothing effect.

[0066] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A method for preparing a lemon fruit extract containing sennaol, characterized in that, Includes the following steps: Lemon peel was dried, crushed, and then added to an aqueous solution of a eutectic solvent for ultrasonic extraction. After extraction, glycosidase was added for enzymatic hydrolysis. The hydrolysis product was collected, centrifuged, the supernatant was collected, and filtered to obtain the lemon fruit extract containing sennaol. The aqueous solution of the eutectic solvent is composed of a hydrogen bond acceptor, a hydrogen bond donor, and water; the hydrogen bond acceptor includes at least one of betaine, choline chloride, glycine, and L-proline; the hydrogen bond donor includes at least one of glycerol, urea, allantoin, panthenol, 1,3-propanediol, 1,2-propanediol, ethylene glycol, butylene glycol, 1,3-butanediol, 1,4-butanediol, arginine, lysine, proline, glycine, alanine, and malic acid; the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:(1-4). The ratio of lemon peel to eutectic solvent is 1g:(5-20)mL; the ultrasonic extraction temperature is 40-60℃, the power is 100-200W, and the time is 30-60min; The glycosidase includes at least one of β-glucosidase, α-L-rhamnosidase, and rutinase; the concentration of the enzyme in the enzymatic hydrolysis reaction in the system is 100-500 U / L, the enzymatic hydrolysis temperature is 30-50℃, and the time is 30-90 min.

2. The preparation method according to claim 1, characterized in that, The hydrogen bond donor is betaine, and the hydrogen bond donors are panthenol and arginine. The molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:(2-3), and the molar ratio of panthenol to arginine is (20-40):

1. The ultrasonic extraction temperature is 50-55℃, the power is 120-150W, and the time is 40-50min; The glycosidase is β-glucosidase and α-L-rhamnosidase in a concentration ratio of 1:(0.5-2); the concentration of the enzyme in the enzymatic hydrolysis reaction in the system is 200-300 U / L, the enzymatic hydrolysis temperature is 40-45℃, and the time is 40-60 min.

3. The preparation method according to claim 2, characterized in that, The molar ratio of panthenol to arginine is (25-35):

1.

4. The preparation method according to any one of claims 1-3, characterized in that, The total mass concentration of hydrogen bond acceptors and hydrogen bond donors in the eutectic solvent is 60%-90%.

5. The preparation method according to claim 4, characterized in that, The total mass concentration of hydrogen bond acceptors and hydrogen bond donors in the eutectic solvent is 70%-80%.

6. The use of the lemon fruit extract containing sennaol prepared by any one of claims 1-5 in the preparation of cosmetics.

7. The application of the lemon fruit extract containing sennaol as described in claim 6 in the preparation of cosmetics, characterized in that, The cosmetics include one or more of the following: toner, lotion, cream, mask, serum, and spray.

8. A toner, characterized in that, The toner comprises the following components by weight percentage: 1%-10% lemon fruit extract obtained by the preparation method according to any one of claims 1-5, 0.05%-0.5% thickener, 0.5%-5% moisturizer, 0.1%-1% antioxidant, 0.01%-0.3% pH adjuster, and the balance being deionized water.

9. The lotion as described in claim 8, characterized in that, The raw material is selected from at least one of (a)-(d): (a) The thickener comprises at least one of the following: polyacrylate crosspolymer-6, carbomer, carrageenan, gellan gum, xanthan gum, microcrystalline cellulose, cellulose gum, ethyl cellulose, strychnine gum, guar gum, ammonium acryloyl dimethyl taurate / VP copolymer, acrylate copolymer, sclerotium gum, polyvinylpyrrolidone, amylopectin, and sodium polyacrylate; (b) The moisturizer comprises at least one of the following: glycerin, 1,2-butanediol, 1,4-butanediol, 1,2-hexanediol, 1,3-propanediol, 1,2-pentanediol, butylene glycol, caprylyl glycol, dipropylene glycol, tremella polysaccharide, trehalose, betaine, allantoin, hyaluronic acid, sodium hyaluronate, acetylated sodium hyaluronate, hydrolyzed sodium hyaluronate, sodium hyaluronate cross-linked polymer, β-glucan, budding stalk polysaccharide, and ceramide; (c) The antioxidant is p-hydroxyacetophenone; (d) The pH adjuster includes at least one of arginine, disodium ethylenediaminetetraacetate, tromethamine, and citric acid.

10. The method for preparing the lotion as described in claim 8 or 9, characterized in that, Includes the following steps: S1. Mix the thickener with deionized water and stir. Heat to 80-90℃ and homogenize at 1200-1400 rpm for 3-6 minutes to obtain pre-prepared component A. S2. Mix the humectant and antioxidant, heat to 60°C to melt, and obtain pre-prepared component B. S3. After cooling the pre-prepared component A to 60°C, add the pre-prepared component B at a speed of 200-500 rpm and stir to mix. Then cool to below 45°C, add the lemon fruit extract prepared by any one of the preparation methods described in claims 1-5, continue stirring for 5-10 min, and finally add a pH adjuster to adjust the pH. Then stop stirring, discharge the product, and obtain the toner.

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