Composition for improving solubility of ginseng fruit rare saponin as well as preparation method and application of composition

Abstract

The invention relates to a composition for improving solubility of ginseng fruit rare saponin as well as a preparation method and application of the composition, and belongs to the technical field of natural extracts. The invention provides a composition for improving solubility of ginseng fruit rare saponin, which comprises ginseng fruit rare saponin, glycyrrhizic acid and centella asiatica extract, and the weight ratio of ginseng fruit rare saponin to glycyrrhizic acid to centella asiatica extract is 1: (1.5-5): (1-3). The ginseng fruit rare saponin, the glycyrrhizic acid and the centella asiatica extract are matched to form the composition, and the obtained composition has good solubility when the pH value is equal to 5-8 and can be completely dissolved in solvents such as water. In addition, the ginseng fruit rare saponin, the glycyrrhizic acid and the centella asiatica extract are matched to form the composition, the composition further has a synergistic anti-oxidation effect, a complete anti-oxidation-anti-inflammation-repair system is constructed through different action mechanisms, the limitation of a single component is overcome, and the overall effect of cosmetics is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of natural extracts, and in particular to a composition for improving the solubility of rare saponins of ginseng fruit, and a preparation method and application thereof. Background Art

[0002] Ginseng is a perennial herb of the genus Panax in the Araliaceae family. Its main root is large, spindle-shaped or cylindrical, and its leaves are palmately compound. Ginseng fruit is the mature fruit of ginseng. Although it is not a traditional medicinal part, it contains rich active ingredients such as ginsenosides (the content is higher than that in the root), polysaccharides, amino acids, etc. Ginseng fruit saponins include Re, Rd, Rg1 and other main components. Compared with ginseng roots, ginseng fruit has a higher content of total saponins. Ginseng fruit contains saponins such as Re, Rd, and Rg1, which are conventional saponins.

[0003] The content of rare saponins in natural plants is extremely low and needs to be obtained through biotransformation, chemical degradation or physical treatment. Ginseng fruit rare saponins have stronger anti-wrinkle, ultraviolet absorption, antioxidant and other effects, and are widely used. However, ginseng fruit rare saponins are insoluble in water and oily solvents. The solubility in glycerol is less than 1%, and the solubility in butylene glycol is less than 4%. In addition, the ginseng fruit rare saponin solution prepared with glycerol or butylene glycol as a solvent is easy to precipitate once water is added, which makes the application of ginseng fruit rare saponins in various fields have certain limitations. Therefore, it is urgent to develop a method to improve the solubility of ginseng fruit rare saponins in solvents such as water to break through the limitation of the low solubility of ginseng fruit rare saponins.

[0004] Furthermore, in the field of cosmetic antioxidant technology, single antioxidants, due to their inherent limitations, are unable to meet the demand for effective anti-aging treatments, making synergistic antioxidant research a key area of ​​focus. Synergistic antioxidants enhance antioxidant efficacy by combining ingredients with different mechanisms of action. Therefore, conducting synergistic antioxidant research is crucial for overcoming the bottleneck of single ingredients and developing highly effective and stable antioxidant formulas. Summary of the Invention

[0005] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a composition for improving the solubility of rare saponins of ginseng fruit, as well as its preparation method and application, which can effectively improve the solubility of rare saponins of ginseng fruit in solvents such as water. At the same time, the combination of rare saponins of ginseng fruit with glycyrrhizic acid and Centella asiatica extract to form a composition has a more excellent antioxidant effect.

[0006] To achieve the above object, the technical solution adopted by the present invention is:

[0007] In a first aspect, the present invention provides a composition for improving the solubility of rare saponins of ginseng fruit, comprising rare saponins of ginseng fruit, glycyrrhizic acid and Centella asiatica extract, wherein the weight ratio of the rare saponins of ginseng fruit, glycyrrhizic acid and Centella asiatica extract is ginseng fruit rare saponins: glycyrrhizic acid: Centella asiatica extract = 1: (1.5-5): (1-3).

[0008] The present invention combines rare ginseng fruit saponins, glycyrrhizic acid and Centella asiatica extract into a composition. The obtained composition has good solubility at pH = 5-8, can be completely dissolved in solvents such as water, and the rare ginseng fruit saponins will not precipitate even after being left to stand for 48 hours, thereby greatly improving the solubility of the rare ginseng fruit saponins.

[0009] The main components of Centella asiatica extract are triterpenoid saponin compounds such as asiaticoside and hydroxymadecassoside. Although its molecular structure contains multiple hydroxyl groups (-OH) and glycosidic bonds, which makes it hydrophilic to a certain extent, it is still a polar macromolecular substance as a whole.

[0010] The structural characteristics of rare saponins in ginseng fruit are reduced sugar groups and increased fat solubility, and they are low-polarity compounds. The polarity of Centella asiatica extract is quite different from that of rare saponins. According to the principle of "like dissolves like", it is difficult for the two to form a stable dispersion system through intermolecular forces (such as hydrogen bonds and van der Waals forces), resulting in turbidity of the solution.

[0011] Glycyrrhizic acid is a triterpenoid saponin compound. Its molecular structure contains two glucuronic acid groups (strongly hydrophilic) and glycyrrhetinic acid aglycone (lipophilic). It has amphiphilic characteristics and can form colloidal microbes (micelles) at high concentrations, encapsulating the fat-soluble rare saponins of ginseng fruit and dissolving them in water.

[0012] In general, glycyrrhizic acid has a stronger ability to encapsulate rare saponins from ginseng fruit than Centella asiatica extract. However, glycyrrhizic acid contains carboxylic acid and glucuronic acid groups and is acidic, with an initial pH of approximately 3.0 in its aqueous solution. As the pH increases, the carboxyl and glucuronic acid groups in the glycyrrhizic acid molecule all dissociate into carboxyl groups (-COO-), significantly increasing the charge density and reducing the amphiphilicity of the molecule. This causes the original weakly stable micelle structure to disintegrate due to charge repulsion, releasing and aggregating the encapsulated rare saponins from ginseng fruit, and causing the solution to become turbid.

[0013] The combined use of Centella asiatica extract and glycyrrhizic acid can resolve the solubility issues of rare ginseng fruit saponins, likely due to a synergistic solubilization mechanism formed through intermolecular interactions between the two, resulting in a stable nanoscale dispersion system with the rare saponins. Madecassoside, the main component of Centella asiatica extract, contains multiple hydroxyl groups (-OH) and glycosidic bonds. These hydroxyl groups may form a hydrogen bond network with the hydroxyl and carboxyl groups of glycyrrhizic acid, forming a steric barrier that enhances the hydrophilicity of the micelle shell and the thickness of the hydration layer. Even with changes in pH, steric hindrance can physically prevent particle collision and aggregation, maintaining dispersion stability and reducing glycyrrhizic acid's sensitivity to pH.

[0014] As a preferred embodiment of the composition of the present invention, the weight ratio of ginseng fruit rare saponins, glycyrrhizic acid and Centella asiatica extract in the composition is ginseng fruit rare saponins: glycyrrhizic acid: Centella asiatica extract = 1: (2-4): (1.2-3).

[0015] As a preferred embodiment of the composition of the present invention, the weight ratio of the ginseng fruit rare saponins, glycyrrhizic acid and Centella asiatica extract is ginseng fruit rare saponins: glycyrrhizic acid: Centella asiatica extract = 1: (2-3): (2-3).

[0016] As a preferred embodiment of the composition of the present invention, the rare ginseng fruit saponins are primarily prepared by thermally converting a ginseng fruit extract with a citric acid solution. The rare ginseng fruit saponins in the composition of the present invention can be obtained from commercial sources or by acid conversion; it only needs to be confirmed to be rare ginseng fruit saponins.

[0017] As a preferred embodiment of the composition of the present invention, the method for preparing rare ginseng fruit saponins comprises the following steps:

[0018] (1) mixing a ginseng fruit extract solution and a citric acid solution at 87-93° C., keeping the temperature for 80-100 minutes to obtain a reaction product, adjusting the pH value of the reaction product to 9-11, decolorizing the reaction product to obtain a decolorized product, adjusting the pH value of the decolorized product to 3-4, and removing the liquid to obtain a precipitate;

[0019] (2) washing the precipitate obtained in step (1) until the pH value of the washing solution is 6-7 to obtain a washed precipitate, vacuum drying, crushing, and sieving the washed precipitate to obtain rare ginseng fruit saponins.

[0020] As a preferred embodiment of the composition of the present invention, in step (1), the mass ratio of ginseng fruit extract to solvent in the ginseng fruit extract solution is ginseng fruit extract: solvent = 1: (18-22).

[0021] As a preferred embodiment of the composition of the present invention, in step (1), the mass ratio of ginseng fruit extract to solvent in the ginseng fruit extract solution is ginseng fruit extract:solvent=1:20.

[0022] As a preferred embodiment of the composition of the present invention, the solvent in the ginseng fruit extract solution includes but is not limited to at least one of water, ethanol, butylene glycol, propylene glycol laurate, diethylene glycol butyl ether and diethoxydiglycol.

[0023] As a preferred embodiment of the composition of the present invention, in step (1), the volume ratio of the ginseng fruit extract solution to the citric acid solution is ginseng fruit extract solution: citric acid solution = 1: (0.8-1).

[0024] As a preferred embodiment of the composition of the present invention, in step (1), the volume ratio of the ginseng fruit extract solution to the citric acid solution is ginseng fruit extract solution: citric acid solution = 1:0.9.

[0025] As a preferred embodiment of the composition of the present invention, in step (1), the citric acid solution is a saturated citric acid solution.

[0026] As a preferred embodiment of the composition of the present invention, in step (1), the ginseng fruit extract solution and the citric acid solution are mixed at 90° C. and kept warm for 90 minutes to obtain a reaction product.

[0027] As a preferred embodiment of the composition of the present invention, in step (1), the reaction product is cooled to 57-63° C. and then the pH value of the reaction product is adjusted.

[0028] As a preferred embodiment of the composition of the present invention, in step (1), the reaction product is cooled to 60° C. and then the pH value of the reaction product is adjusted.

[0029] As a preferred embodiment of the composition of the present invention, in step (1), the pH value of the reaction product is adjusted to 10.

[0030] As a preferred embodiment of the composition of the present invention, in step (1), the decolorization treatment is to add a peroxide solution and stir for 0.5-2 hours, and the amount of the peroxide solution is 3-5g peroxide solution per 1g of ginseng fruit extract.

[0031] As a preferred embodiment of the composition of the present invention, in step (1), the decolorization treatment is to add a peroxide solution and stir for 1-1.5 hours, and the amount of the peroxide is 4g of peroxide solution per 1g of ginseng fruit extract.

[0032] As a preferred embodiment of the composition of the present invention, in step (1), the peroxide solution is a 30% v / v hydrogen peroxide solution.

[0033] As a preferred embodiment of the composition of the present invention, in step (2), the washing is performed at 23-27°C.

[0034] As a preferred embodiment of the composition of the present invention, in step (2), the washing is performed at 25°C.

[0035] As a preferred embodiment of the composition of the present invention, in step (2), the vacuum drying is carried out at 65-75°C.

[0036] As a preferred embodiment of the composition of the present invention, in step (2), the vacuum drying is performed at 70°C.

[0037] As a preferred embodiment of the composition of the present invention, in step (2), the sieving is through a 40-mesh sieve.

[0038] In a second aspect, the present invention provides a method for preparing the aforementioned composition for improving the solubility of rare ginseng fruit saponins. The method comprises mixing an alcoholic solution of rare ginseng fruit saponins with glycyrrhizic acid and Centella asiatica extract, filtering, and evaporating under reduced pressure to obtain a composition for improving the solubility of rare ginseng fruit saponins. The method comprises first completely dissolving the rare ginseng fruit saponins in ethanol, then adding glycyrrhizic acid and Centella asiatica extract, removing insoluble particles, and then removing the organic solvent. The resulting composition is dried to be completely soluble in a solvent such as water.

[0039] As a preferred embodiment of the preparation method of the present invention, the mass ratio of ginseng fruit rare saponins to ethanol in the ginseng fruit rare saponin alcohol solution is ginseng fruit rare saponins:ethanol = 1:(10-30). Experiments in the present invention have confirmed that ginseng fruit rare saponins have extremely high solubility in ethanol. However, to avoid precipitation due to excessive ginseng fruit rare saponins content, the ginseng fruit rare saponin content in the alcohol solution can be up to 10 wt%.

[0040] As a preferred embodiment of the preparation method of the present invention, the mass ratio of ginseng fruit rare saponins and ethanol in the ginseng fruit rare saponin alcohol solution is ginseng fruit rare saponins:ethanol=1:20.

[0041] As a preferred embodiment of the preparation method of the present invention, the ethanol is anhydrous ethanol. Since the rare saponins of ginseng fruit are insoluble in water, if ethanol containing water is used, the rare saponins of ginseng fruit may not be completely dissolved.

[0042] As a preferred embodiment of the preparation method of the present invention, the mixing is performed by heating and stirring at 40-70° C. Heating and stirring can promote the dissolution of the rare saponins of ginseng fruit, glycyrrhizic acid and Centella asiatica extract.

[0043] As a preferred embodiment of the preparation method of the present invention, the mixing is performed by heating and stirring at 60°C.

[0044] As a preferred embodiment of the preparation method of the present invention, the filtration is performed using a 600-1000 mesh filter to remove insoluble impurities that may be contained in the three components.

[0045] As a preferred embodiment of the preparation method of the present invention, the filtration is performed using an 800-1000 mesh filter.

[0046] As a preferred embodiment of the preparation method of the present invention, the reduced pressure evaporation is carried out at 40-70° C. The purpose of reduced pressure evaporation is to remove the organic solvent, avoid organic solvent residue in the composition, and thus reduce the risk of allergies.

[0047] As a preferred embodiment of the preparation method of the present invention, the reduced pressure evaporation is carried out at 60°C.

[0048] As a preferred embodiment of the preparation method of the present invention, the preparation method further includes grinding the composition for improving the solubility of rare ginseng fruit saponins into a 60-mesh powder. Grinding the composition for improving the solubility of rare ginseng fruit saponins into a finer powder can effectively improve the dissolution efficiency of the composition.

[0049] In a third aspect, the present invention provides use of the above-mentioned composition for improving the solubility of rare saponins in ginseng fruit in the preparation of cosmetics.

[0050] As a preferred implementation method of the application of the present invention, the dosage form of the cosmetic includes at least one of creams, emulsions, aqueous solutions, gels, oils, powders, block powders or solids, patches, films and freeze-dried products.

[0051] As a preferred embodiment of the application of the present invention, the weight percentage of the composition for improving the solubility of rare ginseng fruit saponins in the cosmetic is 0.01-1%.

[0052] In a fourth aspect, the present invention provides the use of the above-mentioned composition for improving the solubility of rare saponins of ginseng fruit in the preparation of antioxidant products. The present invention found through free radical scavenging experiments and statistical analysis that rare saponins of ginseng fruit, glycyrrhizic acid and Centella asiatica extract have synergistic antioxidant effects. The powerful antioxidant capacity of rare saponins of ginseng fruit combined with the collagen-promoting effect of Centella asiatica extract can synergistically fight aging from the two aspects of free radical scavenging and skin structure repair; the anti-inflammatory properties of glycyrrhizic acid can reduce the inflammatory response caused by oxidative stress, creating a good environment for rare saponins of ginseng fruit and Centella asiatica extract to exert their effects. The three work together to produce a synergistic effect, constructing a complete "antioxidant-anti-inflammatory-repair" system through different mechanisms of action, overcoming the limitations of a single ingredient and enhancing the overall efficacy of cosmetics.

[0053] As a preferred embodiment of the application of the present invention, the types of the antioxidant products include at least one of medicines, daily chemical products, health products and foods.

[0054] Compared with the prior art, the present invention has the following beneficial effects:

[0055] (1) The present invention combines rare ginseng fruit saponins, glycyrrhizic acid and Centella asiatica extract into a composition. The obtained composition has good solubility at pH = 5-8, can be completely dissolved in solvents such as water, and will not precipitate rare ginseng fruit saponins even after standing for 48 hours, which can greatly improve the solubility of rare ginseng fruit saponins.

[0056] (2) The present invention has found through free radical scavenging experiments and statistical analysis that rare ginseng fruit saponins, glycyrrhizic acid, and Centella asiatica extract have synergistic antioxidant effects. The powerful antioxidant capacity of rare ginseng fruit saponins combined with the collagen-promoting effect of Centella asiatica extract can synergistically fight aging from the two aspects of free radical scavenging and skin structure repair; the anti-inflammatory properties of glycyrrhizic acid can alleviate the inflammatory response caused by oxidative stress, creating a good environment for rare ginseng fruit saponins and Centella asiatica extract to exert their effects. The three synergistically produce a synergistic effect, constructing a complete "antioxidant-anti-inflammatory-repair" system through different mechanisms of action, overcoming the limitations of a single ingredient and enhancing the overall efficacy of cosmetics. BRIEF DESCRIPTION OF THE DRAWINGS

[0057] Figure 1 The instant dissolution performance test results of different compositions for improving the solubility of rare ginseng fruit saponins in Example 1 of the present invention;

[0058] Figure 2 The long-term stability test results of different compositions for improving the solubility of rare ginseng fruit saponins in Example 2 of the present invention are as follows;

[0059] Figure 3 This is the effect of different pH values ​​on the composition for improving the solubility of rare saponins from ginseng fruit in Effect Example 2 of the present invention;

[0060] Figure 4 IC of the rare saponins of ginseng fruit (A), glycyrrhizic acid (B), Centella asiatica extract (C), the composition obtained in Example 1 (D), the composition obtained in Example 2 (E), and the composition obtained in Example 3 (F) in Example 4 of the present invention 50 curve. DETAILED DESCRIPTION

[0061] In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.

[0062] Unless otherwise specified, other materials and reagents used in the examples can be obtained from commercial sources.

[0063] The techniques not described in detail in the following examples, comparative examples and effect examples are all commonly used techniques in the art. Please refer to "Molecular Biology Experiment Manual" (Ma Wenli, People's Military Medical Publishing House), "Molecular Biology Experiment (Second Edition)" (Zhejiang University Press), and "Cell Biology Experiment" (Yang Hongbing, Hou Lixia, Zhang Yuxi, Higher Education Press).

[0064] The ginseng fruit extract used in the following examples, comparative examples, and experimental examples was purchased from Jilin Changqing Ginseng Industry Co., Ltd. The ginseng fruit extract appears as a yellow powder with a particle size of less than 100 mesh. The heavy metal and microbial content meets the requirements of 3.3 Microbiological Indexes and 3.4 Hazardous Substance Limits in Chapter 1 of the "Technical Specifications for Safety of Cosmetics" (2015 edition). The total saponins (Rg1+Re+Rb1+Rc+Rb2+Rd) in the ginseng fruit extract were greater than 60% by HPLC. The HPLC conditions are as follows:

[0065] Chromatographic column: C18 250×4.6 mm; particle size: 5 μm, carbon loading: 11%; mobile phase: acetonitrile-0.1% v / v phosphoric acid solution gradient elution (as shown in Table 1 below); detection wavelength: 203 nm; injection volume: 10 μl; column temperature: 30°C; flow rate: 1.3 mL / min.

[0066] Prepare a mixed solution of ginsenoside reference substances Re, Rg1, Rb1, Rb2, Rc, and Rd in methanol containing 1 mg of each ginsenoside reference substance Re, Rg1, Rb1, Rb2, Rc, and Rd per 1 ml. Accurately pipette 10 μL of the solution into a liquid chromatograph for determination.

[0067] Preparation and determination of test solution: Accurately weigh approximately 25 mg of the test sample into a 10 mL volumetric flask. Add an appropriate amount of methanol, sonicate for 30 minutes to dissolve, cool, and dilute to volume. Shake well, filter, and obtain the solution. Accurately pipette 10 μL of the sample into a liquid chromatograph and determine the solution.

[0068] The content of ginsenosides was calculated based on the peak area of ​​the reference spectrum and the test sample.

[0069] Table 1 Acetonitrile-0.1% v / v phosphoric acid solution gradient elution conditions

[0070] Time / min Acetonitrile / % 0.1% v / v phosphoric acid solution / % 0 19 81 30 19 81 35 24 76 60 40 60

[0071] The CAS number of glycyrrhizic acid is 1405-86-3, purchased from Gansu Panzhi Pharmaceutical Co., Ltd. (trade name glycyrrhizic acid A). The quality specifications of glycyrrhizic acid are glycyrrhizic acid A ≥ 95% (using UV determination method), residue on ignition ≤ 0.2%, loss on drying ≤ 6%, and heavy metals and microorganisms comply with the provisions of the "Technical Specifications for Safety of Cosmetics" (2015 edition).

[0072] The INCI name of Centella asiatica extract is CENTELLA ASIATICA extract, which was purchased from Guilin Lain Biotechnology Co., Ltd. It belongs to the Centella asiatica extract total glycosides series, with a total glycoside content of >80%. The product model is GKE86, and the production batch number is GKE86-21040301. According to the Centella asiatica total glycosides content determination method, the total glycoside content of Centella asiatica is 82.18%, and the hydroxymadecassoside content is 50.98%.

[0073] Example 1

[0074] This embodiment provides a method for preparing rare saponins from ginseng fruit, the method comprising the following steps:

[0075] 1. The ginseng fruit extract was mixed with water (1:20, w:w) to prepare a ginseng fruit extract solution. The ginseng fruit extract solution and the saturated citric acid solution were mixed at 90° C. according to the ratio of adding 0.9 mL of saturated citric acid solution to every 1 mL of ginseng fruit extract solution. The mixture was kept warm for 90 minutes to obtain a reaction product.

[0076] 2. The pH value of the reaction product obtained in step 1 was adjusted to 10, and the reaction product with pH = 10 was mixed with hydrogen peroxide solution at a ratio of 4 g of 30% v / v hydrogen peroxide solution per 1 g of ginseng fruit extract, and stirred for 1 hour for decolorization to obtain a decolorized product;

[0077] 3. The decolorized product obtained in step 2 is adjusted to a pH of 4, allowed to stand until the temperature reaches 25°C, the liquid is removed to obtain a solid precipitate, and the precipitate is washed with purified water until the pH value of the washing solution reaches 6 to obtain a washed precipitate;

[0078] 4. The washed precipitate obtained in step 3 was vacuum-dried at 70°C, crushed, and passed through a 40-mesh sieve to obtain rare ginseng fruit saponins.

[0079] Effect Example 1

[0080] In order to explore the solubility properties of the rare saponins of ginseng fruit obtained in Example 1 in different solvents, the rare saponins of ginseng fruit were mixed with a solvent, heated to 70-95°C (first heated to 70°C, and if it could not be completely dissolved, continued to heat to 95°C) and stirred for 60 minutes. The solubility properties of the rare saponins of ginseng fruit in different solvents were judged by transparency. If turbidity appeared, it was judged to be insoluble. If the solution became transparent, it was judged to be dissolved. The temperature for evaluating transparency was 60°C. The results are shown in Table 2.

[0081] Table 2 Solubility test results of rare ginseng fruit saponins in different solvents

[0082]

[0083]

[0084] As shown in Table 2, the solubility of rare ginseng fruit saponins in common cosmetic raw materials such as triethylhexanoin, hydrogenated polydecene, dicaprylyl carbonate, squalane, caprylic / capric triglyceride, and glycerin is less than 1%. The solubility in diethylene glycol butyl ether and propylene glycol laurate is 1-2%. Moreover, when a solution of rare ginseng fruit saponins in diethylene glycol butyl ether or propylene glycol laurate is added to water, the rare ginseng fruit saponins precipitate in the solution, making it impossible to add rare ginseng fruit saponins as raw materials to cosmetic formulas with high water content. The solubility of rare ginseng fruit saponins in diethoxydiglycol and butylene glycol both reaches 2%, but when water is added to the rare ginseng fruit saponins solution in these two solvents, the rare ginseng fruit saponins also precipitate, making it impossible to add them to cosmetic formulas. The solubility of rare ginseng fruit saponins in anhydrous ethanol is greater than 10%. Although ethanol can be used as a solvent to prepare rare ginseng fruit saponins solutions, due to the special properties of rare ginseng fruit saponins, when the ethanol solution is added to water, the rare ginseng fruit saponins will precipitate, making it difficult to apply rare ginseng fruit saponins well in cosmetic systems with high water content. In addition, many consumers believe that alcohol-containing cosmetics are highly irritating and will damage skin keratin, making the skin sensitive, and are cautious or reject them. Therefore, using ethanol as a solvent cannot solve the problem of poor solubility of rare ginseng fruit saponins.

[0085] Examples 2-6 and Comparative Examples 1-4

[0086] Examples 2-6 and Comparative Examples 1-4 respectively provide a composition for improving the solubility of rare saponins of ginseng fruit and a preparation method thereof. The components and amounts of the composition are shown in Table 3. The preparation method comprises the following steps:

[0087] A. Mixing rare ginseng fruit saponins with anhydrous ethanol at a mass ratio of 1:20 (rare ginseng fruit saponins: anhydrous ethanol) to obtain a rare ginseng fruit saponin alcohol solution;

[0088] B. Mixing the ginseng fruit rare saponin alcohol solution obtained in step A with glycyrrhizic acid and Centella asiatica extract at 60° C., and after complete dissolution, filtering through a 1000-mesh filter to obtain a filtrate;

[0089] C. Evaporate the filtrate obtained in step B under reduced pressure at 60° C. to obtain a solid, which is ground into a powder of less than 60 mesh. The obtained powder is a composition for improving the solubility of rare saponins of ginseng fruit.

[0090] Table 3 Components and dosages of different compositions for improving the solubility of rare saponins from ginseng fruit (parts by weight)

[0091]

[0092] The compositions obtained in Example 2 and Example 6 were prepared as aqueous solutions at a mass concentration of 0.5 wt %. The average particle size was tested using a molecular weight nanoparticle size analyzer SZ-100. The average particle size of the composition obtained in Example 2 was 52.9 nm, and the average particle size of the composition obtained in Example 6 was 118.9 nm, indicating that the obtained compositions were nanoscale materials.

[0093] Example 7

[0094] Example 7 provides a composition for improving the solubility of rare saponins from ginseng fruit and a preparation method thereof. The components and amounts of the composition are the same as those in Example 2. The preparation method comprises the following steps:

[0095] A. Mixing the rare ginseng fruit saponins with anhydrous ethanol at a mass ratio of 1:10 (rare ginseng fruit saponins: anhydrous ethanol) to obtain a rare ginseng fruit saponin alcohol solution;

[0096] B. Mixing the ginseng fruit rare saponin alcohol solution obtained in step A with glycyrrhizic acid and Centella asiatica extract at 40° C., transferring the mixture to a 600-mesh filter after complete dissolution to obtain a filtrate;

[0097] C. Evaporate the filtrate obtained in step B under reduced pressure at 40° C. to obtain a solid, which is ground into a powder of less than 60 mesh. The obtained powder is a composition for improving the solubility of rare saponins of ginseng fruit.

[0098] Example 8

[0099] Example 8 provides a composition for improving the solubility of rare saponins from ginseng fruit and a preparation method thereof. The components and amounts of the composition are the same as those in Example 2. The preparation method comprises the following steps:

[0100] A. Mixing rare ginseng fruit saponins with anhydrous ethanol at a mass ratio of 1:30 (rare ginseng fruit saponins: anhydrous ethanol) to obtain a rare ginseng fruit saponin alcohol solution;

[0101] B. Mixing the ginseng fruit rare saponin alcohol solution obtained in step A with glycyrrhizic acid and Centella asiatica extract at 70° C., transferring the mixture to an 800-mesh filter after complete dissolution to obtain a filtrate;

[0102] C. Evaporate the filtrate obtained in step B under reduced pressure at 70° C. to obtain a solid, which is ground into a powder of less than 60 mesh. The obtained powder is a composition for improving the solubility of rare saponins of ginseng fruit.

[0103] Effect Example 2

[0104] 1. In order to verify the solubility of the compositions for improving the solubility of rare saponins of ginseng fruit obtained in Examples 2-6 and Comparative Examples 1-4 in water, the above compositions were respectively prepared with water to form a solution with a concentration of 0.5% by mass. After stirring for 10 minutes and standing at 25±3°C for 48 hours, the solubility of the compositions was evaluated by observing the transparency of the solutions. The results are shown in FIG. Figure 1-2 and Table 4.

[0105] Table 4 Solubility performance test results of different compositions for improving the solubility of rare saponins of ginseng fruit

[0106]

[0107]

[0108] like Figure 1 As shown in Table 4, when the solutions were just prepared, Examples 2-6, Comparative Examples 1, and 3-6 all appeared clear, while Comparative Example 2 was obviously turbid. This indicates that the combination of rare saponins from ginseng fruit and Centella asiatica extract cannot improve the immediate solubility of rare saponins from ginseng fruit, while glycyrrhizic acid can improve the immediate solubility of rare saponins from ginseng fruit.

[0109] like Figure 2 As shown in Table 4, after standing for 48 hours, comparative examples 1-2 and 4-6 respectively showed different degrees of turbidity. This shows that although glycyrrhizic acid can improve the immediate solubility of ginseng fruit rare saponins, it cannot make the ginseng fruit rare saponins stably dissolved in water. They are easily precipitated when standing for a long time at room temperature. This shows that only by combining ginseng fruit rare saponins, glycyrrhizic acid and Centella asiatica extract and within a specific ratio range can the immediate solubility and long-term stability of ginseng fruit rare saponins be improved.

[0110] 2. The pH value of cosmetics is generally set to neutral, and the composition for improving the solubility of rare ginseng fruit saponins obtained in the present invention is often acidic due to the presence of glycyrrhizic acid. Therefore, according to the method of Test 1 above, the compositions obtained in Examples 2-6 and Comparative Example 3 were prepared into 0.5% (mass percentage concentration) aqueous solutions, and the pH values ​​of the aqueous solutions were adjusted to 5.0, 6.0, 7.0 and 8.0 using sodium hydroxide solution. The instant solubility was investigated (observed after stirring for 10 minutes). The results are shown in FIG. Figure 3 and Table 5.

[0111] Table 5 Solubility test results of different compositions for improving the solubility of rare saponins of ginseng fruit at different pH values

[0112] Group Original pH pH=5.0 pH=6.0 pH=7.0 pH=8.0 Example 2 transparent transparent transparent transparent transparent Example 3 transparent transparent transparent transparent transparent Example 4 transparent transparent transparent transparent transparent Example 5 transparent transparent transparent transparent transparent Example 6 transparent transparent transparent transparent transparent Comparative Example 3 transparent turbid turbid turbid turbid

[0113] like Figure 3 As shown in Table 5, the aqueous solutions of the compositions obtained in Examples 2-6 at different pH values ​​were all transparent, while the aqueous solution of Comparative Example 3 gradually became turbid with increasing pH value, indicating that rare saponins from ginseng fruit began to precipitate. This indicates that even though Comparative Example 3 was transparent at the original pH value, once used in cosmetics, the rare saponins from ginseng fruit would precipitate when the pH value was adjusted to neutral, making it difficult to maintain the stability of the cosmetics and making it impossible to use in cosmetics.

[0114] Example 9

[0115] This embodiment provides a moisturizing lotion and a preparation method thereof. The components and amounts of the moisturizing lotion are shown in Table 6. The preparation method comprises the following steps:

[0116] (1) Add the water and disodium EDTA of phase A to an emulsifier and start stirring. Then add the pre-mixed phase B and then phase C. Turn on the heat, stir and heat to 80°C, and keep warm for 30 minutes.

[0117] (2) Add phase D to the oil phase pot, turn on the heat, stir and heat to 80°C. After confirming that the oil phase is completely dissolved, add the oil phase to the emulsification pot, turn on the emulsification pot and homogenize for 3-5 minutes;

[0118] (3) Turn on the cooling, stir and cool to 45°C, and add phase E to the emulsification pot;

[0119] (4) Add the pre-mixed phase F and phase G into the emulsifier, adjust the pH to 6.5, and continue stirring for 10-15 minutes to obtain a moisturizing lotion.

[0120] Table 6 Components and dosage of moisturizing lotion

[0121]

[0122]

[0123] Comparative Example 5

[0124] This comparative example provides a moisturizing lotion and a preparation method thereof. The components and amounts of the moisturizing lotion are similar to those in Example 9, except that the amount of the composition for improving the solubility of rare saponins of ginseng fruit obtained in Example 2 in phase F is 0, and the remaining components and amounts except water remain unchanged. The preparation method is the same as that in Example 9.

[0125] Effect Example 3

[0126] The moisturizing lotions obtained in Example 9 and Comparative Example 5 were subjected to stability tests. Specifically, the moisturizing lotions were left to stand at room temperature (25±3°C), 48°C, -15°C, and 5°C for 1 month. If the emulsions did not show demulsification, stratification, discoloration, etc., they were considered qualified. In addition, the moisturizing lotions were subjected to 8 cycle tests at -5 to 40°C. If the emulsions did not show demulsification, stratification, discoloration, etc., they were considered qualified.

[0127] The test results show that the moisturizing lotions obtained in Example 9 and Comparative Example 5 did not show demulsification, stratification, discoloration, etc. after being left standing for 1 month at room temperature, 48°C, -15°C, and 5°C, and were deemed qualified; at the same time, the moisturizing lotions obtained in Example 9 and Comparative Example 5 completed 8 cycle tests at -5 to 40°C, and did not show demulsification, stratification, discoloration, etc., and were deemed qualified, indicating that the composition for improving the solubility of rare saponins of ginseng fruit obtained in the present invention has good stability when used in cosmetics, and the rare saponins of ginseng fruit will not be precipitated due to changes in the environment, thereby reducing the stability of the cosmetics.

[0128] Effect Example 4

[0129] In order to evaluate whether the components of the composition for improving the solubility of rare ginseng fruit saponins obtained in the present invention have the effect of synergistically improving the antioxidant performance, the compositions obtained in Examples 2-4 were subjected to antioxidant tests. The specific scheme is as follows:

[0130] Prepare 0.2mmol / L DPPH solution with anhydrous ethanol, take 2mL DPPH solution and 2mL sample solution of different mass concentrations and mix them respectively. React at room temperature in the dark for 30min, measure the absorbance at 517nm (A1), then replace the DPPH solution with 2mL anhydrous ethanol, measure the absorbance at 517nm (A2), and finally replace the sample solution with 2mL distilled water (butylene glycol), measure the absorbance at 517nm (A0).

[0131] The above experiment was performed in parallel three times. 200 μL of the solution was taken into a 96-well plate using a pipette, and the absorbance at 517 nm was measured using a microplate reader.

[0132] The calculation formula of DPPH free radical scavenging rate (%) is as follows:

[0133]

[0134] The logarithm of the concentration of each sample to be tested is used as the horizontal axis, and the DPPH free radical scavenging rate of each sample to be tested is used as the vertical axis to draw a curve and obtain the IC 50 ,See Figure 4 .

[0135] Referring to the literature (Ye Linlin, Zhou Ankun. Study on the extraction of active ingredients from bamboo leaves and their synergistic antioxidant efficacy [J]. Daily Chemicals Science, 2023, 46(7): 28-33.), the Chou-Talalay model was used to evaluate the synergistic effect of each composition, and the calculation formula is as follows:

[0136]

[0137] In the formula, CI represents the combination index. When CI is less than 1, it indicates that there is a synergistic effect between the components. When CI is greater than 1, it indicates that there is an antagonistic effect between the components.

[0138] C A It is expressed as the concentration of rare ginseng fruit saponins in the composition when the free radical scavenging rate of the composition reaches 50%;

[0139] C a Expressed as IC of individual ginseng fruit rare saponins 50 ;

[0140] C B It is expressed as the concentration of glycyrrhizic acid in the composition when the free radical scavenging rate of the composition reaches 50%;

[0141] C b Expressed as IC of glycyrrhizic acid alone 50 ;

[0142] C C It is expressed as the concentration of the Centella asiatica extract in the composition when the free radical scavenging rate of the composition reaches 50%;

[0143] C c Expressed as IC of Centella asiatica extract alone 50 .

[0144] The rare saponin of ginseng fruit was marked as A, glycyrrhizic acid was marked as B, the extract of Centella asiatica was marked as C, the composition obtained in Example 2 was marked as D, the composition obtained in Example 3 was marked as E, the composition obtained in Example 4 was marked as F, and the obtained IC 50 , CI see Table 7.

[0145] Table 7 Statistical results of synergistic antioxidant effects of different compositions

[0146] Group <![CDATA[Log(IC 50 )]]> <![CDATA[IC 50 (mg / mL)]]> CI Collaboration or not Rare Ginseng Fruit Saponins 1.551 35.54 - - Glycyrrhizic acid 1.873 74.71 - - Centella asiatica extract 3.149 1410 - - Example 2 0.9157 8.236 0.109 Collaboration Example 3 1.012 10.28 0.116 Collaboration Example 4 1.201 15.88 0.166 Collaboration

[0147] like Figure 4 As shown in Table 7, the compositions obtained in Examples 2-4 provide the solubility of rare saponins from ginseng fruit, and the CI values ​​are all <1, indicating that there is a synergistic antioxidant effect between the rare saponins from ginseng fruit, glycyrrhizic acid and Centella asiatica extract in the compositions obtained in Examples 2-4.

[0148] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended 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 the technical solutions of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A composition for improving the solubility of rare saponins in ginseng fruit, characterized in that: The invention comprises rare ginseng fruit saponins, glycyrrhizic acid and centella asiatica extract, wherein the weight ratio of the rare ginseng fruit saponins, glycyrrhizic acid and centella asiatica extract is ginseng fruit rare saponins: glycyrrhizic acid: centella asiatica extract=1:(1.5-5):(1-3).

2. The composition according to claim 1, wherein The rare ginseng fruit saponin is mainly prepared by thermally converting a ginseng fruit extract and a citric acid solution.

3. The composition according to claim 2, wherein The method for preparing rare ginseng fruit saponins comprises the following steps: (1) mixing a ginseng fruit extract solution and a citric acid solution at 87-93° C., keeping the temperature for 80-100 minutes to obtain a reaction product, adjusting the pH value of the reaction product to 9-11, decolorizing the reaction product to obtain a decolorized product, adjusting the pH value of the decolorized product to 3-4, and removing the liquid to obtain a precipitate; (2) washing the precipitate obtained in step (1) until the pH value of the washing solution is 6-7 to obtain a washed precipitate, vacuum drying, crushing, and sieving the washed precipitate to obtain rare ginseng fruit saponins.

4. The composition according to claim 3, wherein Including at least one of the following (I) to (IV): (I) In step (1), the mass ratio of ginseng fruit extract to solvent in the ginseng fruit extract solution is ginseng fruit extract:solvent=1:(18-22); (II) In step (1), the volume ratio of the ginseng fruit extract solution to the citric acid solution is ginseng fruit extract solution: citric acid solution = 1: (0.8-1); (III) In step (1), the decolorization treatment is performed by adding a peroxide solution and stirring for 0.5-2 hours, wherein the amount of the peroxide solution is 3-5 g per 1 g of ginseng fruit extract; (IV) In step (2), the washing is performed at 23-27°C.

5. The method for preparing the composition according to any one of claims 1 to 4, wherein: The ginseng fruit rare saponin alcohol solution is mixed with glycyrrhizic acid and Centella asiatica extract, filtered, and evaporated under reduced pressure to obtain a composition for improving the solubility of the ginseng fruit rare saponin.

6. The preparation method according to claim 5, characterized in that: The mass ratio of ginseng fruit rare saponins and ethanol in the ginseng fruit rare saponin alcohol solution is ginseng fruit rare saponins:ethanol=1:(10-30).

7. The preparation method according to claim 5, characterized in that: The mixing is performed by heating and stirring at 40-70°C.

8. Use of the composition according to any one of claims 1 to 4 in the preparation of cosmetics.

9. The use according to claim 8, characterized in that The weight percentage of the composition for improving the solubility of the rare saponin of ginseng fruit in the cosmetic is 0.01-1%.

10. Use of the composition according to any one of claims 1 to 4 in the preparation of antioxidant products.

Images