Preparation method of red ginseng extracting solution, red ginseng extracting solution and cosmetic composition

Abstract

The invention discloses a preparation method of a red ginseng extracting solution, the red ginseng extracting solution and a cosmetic composition. The preparation method comprises the following steps: providing red ginseng powder; adding the red ginseng powder into a solvent, carrying out variable-temperature interactive extraction, and after the variable-temperature interactive extraction is finished, carrying out filtering separation to obtain a crude extracting solution; adding enzyme into the crude extracting solution to carry out enzymolysis treatment, and carrying out enzyme inactivation after the enzymolysis treatment is finished, so as to obtain an extracting solution after the enzymolysis treatment; phytic acid is added into the extracting solution subjected to enzymolysis treatment for adsorption treatment, and the extracting solution subjected to phytic acid treatment is obtained; and filtering and purifying the phytic acid treated extracting solution to obtain the red ginseng extracting solution. According to the preparation method, the red ginseng extracting solution is obtained through variable-temperature interaction extraction, the extraction rate of ginsenoside in red ginseng can be increased, and the stability of ginsenoside in the red ginseng extracting solution is good.

Description

Technical Field

[0001] This application belongs to the technical field of natural product extraction, and particularly relates to a preparation method of red ginseng extract, a red ginseng extract, and a cosmetic composition. Background Art

[0002] Red ginseng extract shows potential value in multiple fields. However, its full promotion in practical applications is limited by many characteristics of the extract under existing technical conditions. Currently, when preparing red ginseng extract, the content and stability of ginsenosides in the obtained red ginseng extract have become key obstacles. On the one hand, the fibrotic cell wall of red ginseng hinders the dissolution of ginsenosides, thus affecting the extraction rate of ginsenosides; on the other hand, during the extraction process and the storage period of the extract, ginsenosides have a certain degree of instability. They may degrade due to thermosensitivity, or the glycosidic bonds of the saponins may be broken under the influence of pH, light, and oxidation, resulting in hydrolysis or oxidation. This will not only cause changes in the appearance of the red ginseng extract but also lead to a decrease in the saponin content. Summary of the Invention

[0003] The embodiments of this application provide a preparation method of red ginseng extract, a red ginseng extract, and a cosmetic composition. This preparation method obtains the red ginseng extract through variable-temperature alternating extraction, which can improve the extraction rate of ginsenosides in red ginseng, and the stability of ginsenosides in the red ginseng extract is relatively good.

[0004] In a first aspect, a preparation method of red ginseng extract is provided. This preparation method includes: providing red ginseng powder; adding the red ginseng powder to a solvent for variable-temperature alternating extraction. The solvent is an aqueous solution of 1,3-propanediol with a mass percentage of 10% - 50%. After the variable-temperature alternating extraction, filtration and separation are carried out to obtain a crude extract; adding an enzyme to the crude extract for enzymatic hydrolysis treatment, and after the enzymatic hydrolysis treatment, enzyme inactivation is carried out to obtain the extract after enzymatic hydrolysis treatment; adding phytic acid to the extract after enzymatic hydrolysis treatment for adsorption treatment to obtain the extract after phytic acid treatment; carrying out filtration and purification treatment on the extract after phytic acid treatment to obtain the red ginseng extract; wherein, the variable-temperature alternating extraction includes performing multiple extractions alternately at a first temperature and a second temperature. The first temperature is 80°C - 90°C, and the second temperature is 10°C - 20°C. The extraction time for each extraction at the first temperature or the second temperature is 20 min - 30 min; the total number of extractions at the first temperature or the second temperature is 6 - 8 times, and the total time is less than or equal to 240 min; between two adjacent extractions, the extraction temperature rapidly changes between the first temperature and the second temperature, and the temperature change rate is 20°C / min - 40°C / min, and the temperature change time is 1.5 min - 4 min.

[0005] According to the present application, in the preparation of red ginseng extract, the present application adopts high-low temperature alternating extraction and implements extremely rapid temperature change. By the drastic temperature change, the cell wall of red ginseng is induced to rapidly expand or contract under the action of thermal expansion and contraction, thereby intensifying the stress, promoting the fragmentation of the cell wall, and improving the dissolution of active substances. Under the action of high-low temperature alternating extraction with rapid temperature change, the temperature in the high-temperature stage only needs to be controlled at 80°C to 90°C, and the total high-temperature extraction time is reduced. Compared with the long-term high-temperature extraction at 100°C or above used in the prior art, it can reduce the thermosensitive degradation of ginsenosides, reduce the occurrence of side reactions, and improve the extraction rate of ginsenosides in the red ginseng extract and the stability of the red ginseng extract. In addition, in the process of preparing the red ginseng extract, the present application also removes the crude polysaccharide in the extract by adding phytic acid, improving the separation and purification efficiency, and further improving the extraction rate of saponins and the stability of the red ginseng extract. In summary, the red ginseng extract with a high saponin extraction rate, high content, and good stability can be prepared according to the preparation method provided by the present application.

[0006] In some specific embodiments, providing red ginseng powder includes: pulverizing red ginseng whiskers to 10 mesh to 60 mesh, and then performing ultrasonic fragmentation treatment to obtain red ginseng powder of 150 mesh to 300 mesh.

[0007] In the above specific embodiments, the red ginseng powder after ultrasonic fragmentation treatment is further refined, thereby increasing the contact area between the red ginseng powder and the solvent during high-low temperature alternating extraction, and further improving the extraction rate of active ingredients.

[0008] In some specific embodiments, before adding phytic acid to the extract after enzymatic hydrolysis treatment for adsorption treatment, it further includes: measuring the content of crude polysaccharide in the extract after enzymatic hydrolysis treatment by the phenol-sulfuric acid method; in the step of adding phytic acid to the extract after enzymatic hydrolysis treatment for adsorption treatment, the addition amount of phytic acid is 0.1 wt% to 0.5 wt% of the content of crude polysaccharide.

[0009] In the above specific embodiments, the present application characterizes the content of crude polysaccharide in the extract, and removes the crude polysaccharide in the extract as efficiently and precisely as possible by adding a specific amount of phytic acid, and avoids introducing excessive phytic acid into the extract to increase the difficulty of subsequent separation and purification, improves the separation and purification efficiency, and improves the extraction rate of saponins. In addition, it can also reduce the operation cost in the subsequent production process, and is green and energy-saving.

[0010] In some specific embodiments, in the step of adding phytic acid to the extract after enzymatic hydrolysis treatment for adsorption treatment, the pH of the extract after adding phytic acid is 4.8 to 5.2.

[0011] In the above specific embodiments, the applicant found that on the premise of controlling the addition amount of phytic acid to be 0.1 wt% - 0.5 wt% of the content of crude polysaccharide in the extract, and simultaneously controlling the pH of the extract after adding phytic acid to be 4.8 - 5.2, the adsorption rate of saponins can be further improved. When the pH is too low: the aglycone can be protonated, resulting in a decrease in the binding force with the macroporous resin adsorbent during subsequent treatment; when the pH is too high: the hydrolysis of saponins and the competitive adsorption of impurities and macroporous resin can be promoted under alkaline conditions.

[0012] In some specific embodiments, the steps of adding red ginseng powder to a solvent for variable-temperature interactive extraction and performing filtration separation after the variable-temperature interactive extraction to obtain a crude extract include: adding red ginseng powder to a solvent for variable-temperature interactive extraction, and performing filtration separation after the variable-temperature interactive extraction to obtain a first liquid phase and a first filter residue; performing variable-temperature interactive extraction on the first filter residue to obtain a second liquid phase and a second filter residue; mixing the first liquid phase and the second liquid phase to obtain a crude extract.

[0013] In the above specific embodiments, some ginsenosides still remain in the filter residue after the first extraction. Due to the obstruction of the fibrotic cell wall of red ginseng, they were not completely dissolved during the first extraction. Re-extraction can further destroy the cell wall structure, release more saponins, and thus improve the overall extraction rate.

[0014] In some specific embodiments, the steps of adding an enzyme to the crude extract for enzymatic hydrolysis treatment, inactivating the enzyme after the enzymatic hydrolysis treatment, and obtaining the extract after enzymatic hydrolysis treatment include: adjusting the pH of the crude extract to 4.5 - 10.0, adding lipase, and performing enzymatic hydrolysis for 1 h - 2 h at a pH of 5.0 - 6.0 and a temperature of 40°C - 45°C to obtain a first enzymatic hydrolysate. Optionally, citric acid and / or arginine are used for pH adjustment; adding α-amylase and / or neutral protease to the first enzymatic hydrolysate, and performing enzymatic hydrolysis for 1 h - 3 h at a pH of 6.0 - 7.0 and a temperature of 60°C - 65°C to obtain a second enzymatic hydrolysate; heating the second enzymatic hydrolysate to 95°C - 100°C for enzyme inactivation for 0.3 h - 1 h to obtain the extract after enzymatic hydrolysis treatment.

[0015] In the above specific embodiments, the preparation method of the present application further removes colloidal particles and poorly soluble impurities in the red ginseng extract, removes macromolecular substances, and improves the stability of the red ginseng extract through the application of multiple enzymatic hydrolyses.

[0016] In some specific embodiments, the steps of filtering and purifying the extract treated with phytic acid to obtain the red ginseng extract include: adding diatomaceous earth with a mesh size of 100 to 800 to the treated extract, mixing, and then filtering with a microfiltration membrane to obtain the first purified filtrate and solid-phase impurities; adding an adsorption resin to the first purified filtrate, adsorbing at room temperature for 0.5 h to 5 h, and then filtering to obtain a solid phase containing the target product and a waste liquid phase; adding 70% propylene glycol to the solid phase containing the target product, performing desorption at 40°C to 70°C for 0.5 h to 3 h, then cooling to room temperature, and filtering with a microfiltration membrane to obtain the red ginseng extract.

[0017] In some specific embodiments, the variable-temperature interactive extraction includes using microwave-assisted heating and / or using one of liquid nitrogen, dry ice plus water, and ethylene glycol plus water to assist in cooling.

[0018] In the above specific embodiments, the present application makes the temperature change more uniform and the temperature change rate faster through microwave-assisted heating and / or using one of liquid nitrogen, dry ice plus water, and ethylene glycol plus water to assist in cooling, further eliminating the temperature gradient within the material, promoting the effect of variable-temperature interactive extraction, and thus further improving the extraction rate of ginsenosides.

[0019] In a second aspect, the present application provides a red ginseng extract prepared by the preparation method of the first aspect. Optionally, based on the total mass of the red ginseng extract, the content of ginsenosides in the red ginseng extract is 0.2% to 2%. The ginsenosides in the red ginseng extract of the present application have higher stability. After the red ginseng extract is stored at room temperature for 3 months, the change rate of the content of ginsenosides in the red ginseng extract is ≤20%. At the same time, the appearance, color, and smell of the red ginseng extract do not change after long-term storage.

[0020] In a third aspect, the present application provides a cosmetic composition, including the red ginseng extract prepared by the preparation method of the first aspect and / or the red ginseng extract of the second aspect. Optionally, based on the total mass of the cosmetic composition, the cosmetic composition includes 0.1 wt% to 10 wt% of the red ginseng extract. The cosmetic composition can effectively improve the change rate of skin water loss, skin roughness, skin smoothness, and skin gloss. Specific Embodiments

[0021] The features and exemplary embodiments of each aspect of the present application will be described in detail below. For the purpose of making the objectives, technical solutions, and advantages of the present application clearer and more understandable, the following further describes the present application in detail with reference to specific embodiments. It should be understood that the specific embodiments described herein are only intended to explain the present application, rather than limiting the present application. For those skilled in the art, the present application can be implemented without some of these specific details. The following description of the embodiments is only intended to provide a better understanding of the present application by showing examples of the present application.

[0022] For simplicity, only some numerical ranges are explicitly disclosed in this application. However, any lower limit can be combined with any upper limit to form a range not explicitly recited; and any lower limit can be combined with other lower limits to form a range not explicitly recited, and similarly any upper limit can be combined with any other upper limit to form a range not explicitly recited. In addition, although not explicitly recited, each point or single value between the endpoints of the range is included within the range. Thus, each point or single value can be used as its own lower or upper limit and combined with any other point or single value or with other lower or upper limits to form a range not explicitly recited.

[0023] The above Summary of the Invention of this application is not intended to describe every disclosed embodiment or every implementation of this application. The following description more specifically illustrates exemplary embodiments. Throughout the application, guidance is provided through a series of examples, which can be used in various combinations. In each instance, the listings are only representative groups and should not be construed as exhaustive. In addition, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include at least one of such features. In the description of this application, "a plurality of" means at least two, such as two, three, etc., unless otherwise specifically and explicitly defined.

[0024] In this article, room temperature is also referred to as normal temperature or general temperature. In this application, room temperature can represent 25 ± 5°C.

[0025] Red ginseng extract shows potential value in many fields. However, its full promotion in practical applications is limited by many characteristics of the extract under the existing technical conditions. The cell wall of red ginseng is mainly composed of cellulose, hemicellulose, lignin, and pectin. These components make the cell wall relatively strong, which hinders the dissolution of active ingredients and results in low extraction efficiency. In the prior art, high-temperature extraction is often used in an attempt to improve the extraction efficiency. However, high-temperature extraction not only has a limited effect on improving the extraction efficiency but also increases side reactions during the extraction process, resulting in changes in the appearance of the extract or a decrease in the saponin content. Currently, when preparing red ginseng extract, the content and stability of ginsenosides in the obtained red ginseng extract have become key obstacles. On the one hand, the fibrotic cell wall of red ginseng hinders the dissolution of ginsenosides, thus affecting the extraction rate of ginsenosides; on the other hand, during the extraction process and the storage period of the extract, ginsenosides have a certain degree of instability. They may degrade due to thermal sensitivity, or the glycosidic bonds of saponins may be broken under the influence of pH, light, and oxidation, resulting in hydrolysis or oxidation phenomena. This will not only cause changes in the appearance of red ginseng extract but also lead to a decrease in the saponin content.

[0026] Based on the above problems, the embodiments of the present application provide a preparation method of red ginseng extract, a red ginseng extract and a cosmetic composition. The preparation method obtains the red ginseng extract through variable-temperature interactive extraction, which can improve the extraction rate of ginsenosides in red ginseng, and moreover, the stability of ginsenosides in the red ginseng extract is relatively good.

[0027] The following provides a detailed description of the embodiments of the present application.

[0028] Preparation method of red ginseng extract

[0029] In the first aspect, a preparation method of a red ginseng extract is provided, and the preparation method includes:

[0030] S100, providing red ginseng powder;

[0031] S200, adding the red ginseng powder into a solvent for variable-temperature interactive extraction. The solvent is an aqueous solution of 1,3-propanediol with a mass percentage of 10% to 50%. After the variable-temperature interactive extraction is completed, filtration and separation are performed to obtain a crude extract.

[0032] S300, adding an enzyme to the crude extract for enzymatic hydrolysis treatment, and after the enzymatic hydrolysis treatment is completed, enzyme inactivation is performed to obtain an extract after enzymatic hydrolysis treatment.

[0033] S400, adding phytic acid to the extract after enzymatic hydrolysis treatment for adsorption treatment to obtain an extract after phytic acid treatment.

[0034] S500, performing filtration and purification treatment on the extract after phytic acid treatment to obtain a red ginseng extract.

[0035] In step S200, the variable-temperature interactive extraction includes performing multiple extractions alternately at a first temperature and a second temperature. The first temperature is 80°C to 90°C, and the second temperature is 10°C to 20°C. The extraction time for each extraction at the first temperature or the second temperature is 20 min to 30 min; the total number of extractions at the first temperature or the second temperature is 6 to 8 times, and the total time is less than or equal to 240 min. Between two adjacent extractions, the extraction temperature rapidly changes between the first temperature and the second temperature, and the temperature change rate is 20°C / min to 40°C / min, and the temperature change time is 1.5 min to 4 min.

[0036] As an example, in step S200, the first temperature can be 80°C, 81°C, 82°C, 83°C, 84°C, 85°C, 86°C, 87°C, 88°C, 89°C, 90°C or a range composed of any of the above values, and the second temperature can be 10°C, 11°C, 12°C, 13°C, 14°C, 15°C, 16°C, 17°C, 18°C, 19°C, 20°C or a range composed of any of the above values.

[0037] In step S200, the temperature change rate can be the same or different in two adjacent extractions, and the temperature change time between two adjacent extractions can be the same or different.

[0038] In step S200, the number of extractions can be 6, 7, or 8.

[0039] In step S200, the temperature change rate between two adjacent extractions is: 20°C / min to 40°C / min. For example, it can be 20°C / min, 21°C / min, 22°C / min, 23°C / min, 24°C / min, 25°C / min, 26°C / min, 27°C / min, 28°C / min, 29°C / min, 30°C / min, 31°C / min, 32°C / min, 33°C / min, 34°C / min, 35°C / min, 36°C / min, 37°C / min, 38°C / min, 39°C / min, 40°C / min, or any range composed of the above values. The temperature change time between two adjacent extractions is: 1.5 min to 4 min. For example, it can be 1.5 min, 2 min, 2.5 min, 3 min, 3.5 min, 4 min, or any range composed of the above values.

[0040] In step S200, the total extraction time at the first temperature or the second temperature can be 120 min, 140 min, 160 min, 180 min, 200 min, 220 min, 240 min, or any range composed of the above values.

[0041] In step S200, the extraction time each time at the first temperature or the second temperature can be 20 min, 21 min, 22 min, 23 min, 24 min, 25 min, 26 min, 27 min, 28 min, 29 min, 30 min, or any range composed of the above values.

[0042] As an example, the extraction time each time can be the same or different. For example, the total extraction time can be 120 min, the number of extractions n is 6, and the extraction time each time is 20 min. Or, the first extraction time is 30 min, the second extraction time is 20 min, the third extraction time is 10 min, the fourth extraction time is 30 min, the fifth extraction time is 20 min, and the sixth extraction time is 10 min. It can also be that the total extraction time is 120 min, the number of extractions n is 5, and the extraction time each time is 24 min. Or, the first extraction time is 30 min, the second extraction time is 30 min, the third extraction time is 20 min, the fourth extraction time is 20 min, and the fifth extraction time is 20 min.

[0043] According to the present application, the inventors found that in the preparation of red ginseng extract, by adopting high-low temperature alternating extraction and implementing extremely rapid temperature change, the rapid expansion or rapid contraction of the red ginseng cell wall is induced by the drastic temperature change under the action of thermal expansion and contraction, thereby intensifying the stress, promoting the fragmentation of the cell wall, and enhancing the dissolution of active substances. Under the action of high-low temperature alternating extraction with rapid temperature change, the temperature in the high-temperature stage only needs to be controlled at 80-90 °C, and the total high-temperature extraction time is reduced. Compared with the long-time high-temperature extraction at 100 °C or above used in the prior art, it can reduce the thermosensitive degradation of ginsenosides, reduce the occurrence of side reactions, reduce the loss of ginsenosides in the extract, and significantly improve the stability of the red ginseng extract and the extraction rate of ginsenosides in the extract. In addition, in the process of preparing the red ginseng extract in the present application, crude polysaccharides in the extract are removed by adding phytic acid, improving the separation and purification efficiency, and further enhancing the extraction rate of saponins and the stability of the red ginseng extract. In summary, the red ginseng extract with a high saponin extraction rate and content and good stability can be prepared according to the preparation method provided in the present application.

[0044] In some specific embodiments, providing red ginseng powder includes: after crushing red ginseng whiskers to 10 mesh to 60 mesh, for example, it can be 10 mesh, 15 mesh, 20 mesh, 25 mesh, 30 mesh, 35 mesh, 40 mesh, 45 mesh, 50 mesh, 55 mesh, 60 mesh or a range composed of any of the above values, and performing ultrasonic fragmentation treatment to obtain red ginseng powder of 150 mesh to 300 mesh, for example, it can be 100 mesh, 120 mesh, 150 mesh, 180 mesh, 200 mesh, 220 mesh, 250 mesh, 280 mesh, 300 mesh or a range composed of any of the above values.

[0045] As an example, ultrasonic fragmentation treatment can be performed for 5 min to 30 min to refine the red ginseng powder. For example, the ultrasonic treatment time can be 5 min, 10 min, 15 min, 20 min, 25 min, 30 min or a range composed of any of the above values.

[0046] In the above specific embodiments, the red ginseng powder after ultrasonic fragmentation treatment is further refined, thereby increasing the contact area between the red ginseng powder and the solvent during high-low temperature alternating extraction and further enhancing the extraction rate of active ingredients.

[0047] In some specific embodiments, before adding phytic acid to the enzymatically treated extract for adsorption treatment, it further includes: measuring the content of crude polysaccharides in the enzymatically treated extract by the phenol-sulfuric acid method; in the step of adding phytic acid to the enzymatically treated extract for adsorption treatment, the addition amount of phytic acid is 0.1 wt% to 0.5 wt% of the content of crude polysaccharides. For example, the addition amount of phytic acid can be 0.1 wt%, 0.15 wt%, 0.2 wt%, 0.25 wt%, 0.3 wt%, 0.35 wt%, 0.4 wt%, 0.45 wt%, 0.5 wt% of the content of crude polysaccharides or the range composed of any of the above values.

[0048] In the above specific embodiments, the polysaccharides in red ginseng are usually composed of monosaccharides such as glucose, arabinose, and galactose. During the extraction process, the polysaccharide components in red ginseng dissolve out. With the change of the extraction temperature, the polysaccharide molecules can aggregate to form a gel under the influence of their rheological properties; in addition, other components in red ginseng, such as proteins and tannins, can also interact with the polysaccharides to promote the formation of the gel, which is not conducive to subsequent separation and purification. In this application, by characterizing the content of crude polysaccharides in the extract, the crude polysaccharides in the extract are removed as efficiently and precisely as possible by adding a specific amount of phytic acid, and the introduction of excessive phytic acid into the extract is avoided to increase the difficulty of subsequent separation and purification, improve the separation and purification efficiency, and increase the extraction rate of saponins. In addition, it can also reduce the operation cost in the subsequent production process, and is green and energy-saving.

[0049] It should be noted that the content of crude polysaccharides in the enzymatically treated extract can be detected by the method in the entry-exit inspection and quarantine industry standard SN / T 4260-2015.

[0050] In some specific embodiments, in the step of adding phytic acid to the enzymatically treated extract for adsorption treatment, the pH of the extract after adding phytic acid is 4.8 to 5.2. For example, it can be 4.8, 4.9, 5.0, 5.1, 5.2 or the range composed of any of the above values.

[0051] In the above specific embodiments, the applicant found that on the premise of controlling the addition amount of phytic acid to be 0.1 wt% to 0.5 wt% of the content of crude polysaccharides in the extract, and simultaneously controlling the pH of the extract after adding phytic acid to be 4.8 to 5.2, the adsorption rate of saponins can be further improved. When the pH is too low: the glycoside ligand can be protonated, resulting in a decrease in the binding force with the macroporous resin adsorbent during subsequent treatment; when the pH is too high: the saponin hydrolysis and the competitive adsorption of impurities and macroporous resin can be promoted under alkaline conditions.

[0052] In some specific embodiments, in step S200, adding red ginseng powder into a solvent for variable-temperature interactive extraction, and after the variable-temperature interactive extraction is completed, performing filtration and separation to obtain a crude extract, which includes: adding red ginseng powder into a solvent for variable-temperature interactive extraction, and after the variable-temperature interactive extraction is completed, performing filtration and separation to obtain a first liquid phase and a first filter residue, and taking the first liquid phase as the crude extract.

[0053] In some specific embodiments, in step S200, adding red ginseng powder into a solvent for variable-temperature interactive extraction, and after the variable-temperature interactive extraction is completed, performing filtration and separation to obtain a crude extract, which includes:

[0054] S201, adding red ginseng powder into a solvent for variable-temperature interactive extraction, and after the variable-temperature interactive extraction is completed, performing filtration and separation to obtain a first liquid phase and a first filter residue.

[0055] S202, performing variable-temperature interactive extraction on the first filter residue to obtain a second liquid phase and a second filter residue.

[0056] S203, mixing the first liquid phase and the second liquid phase to obtain a crude extract.

[0057] In the above specific embodiments, some ginsenosides still remain in the filter residue after the initial extraction. Due to the obstruction of the fibrotic cell wall of red ginseng, they were not completely dissolved during the first extraction. Re-extraction can further break the cell wall structure, release more saponins, and thus improve the overall extraction rate.

[0058] In some specific embodiments, in step S300, adding an enzyme to the crude extract for enzymatic hydrolysis treatment, and after the enzymatic hydrolysis treatment is completed, inactivating the enzyme to obtain an extract after enzymatic hydrolysis treatment, which includes:

[0059] S301, adjusting the pH of the crude extract to 4.5 - 10.0, adding lipase, and performing enzymatic hydrolysis for 1 h - 2 h under the conditions of pH 5.0 - 6.0 and temperature 40°C - 45°C to obtain a first enzymatic hydrolysate. Optionally, citric acid and / or arginine are used for pH adjustment.

[0060] S302, adding α-amylase and / or neutral protease to the first enzymatic hydrolysate, and performing enzymatic hydrolysis for 1 h - 3 h under the conditions of pH 6.0 - 7.0 and temperature 60°C - 65°C to obtain a second enzymatic hydrolysate.

[0061] S303, heating the second enzymatic hydrolysate to 95°C - 100°C for enzyme inactivation for 0.5 h - 1 h to obtain an extract after enzymatic hydrolysis treatment.

[0062] In the above specific embodiments, the preparation method of the present application further removes colloid particles and poorly soluble impurities in the red ginseng extract, removes macromolecular substances, and improves the stability of the red ginseng extract through the application of multiple enzymatic hydrolyses.

[0063] In some specific embodiments, step S400, the step of filtering and purifying the extract treated with phytic acid to obtain the red ginseng extract includes:

[0064] S401, adding diatomaceous earth with a mesh size of 100 to 800 to the treated extract, mixing, and then filtering with a microfiltration membrane to obtain the first purified filtrate and solid-phase impurities.

[0065] S402, adding an adsorption resin to the first purified filtrate, adsorbing at room temperature for 0.5 h to 5 h, and then filtering to obtain a solid phase containing the target product and a waste liquid phase.

[0066] S403, adding 70% propylene glycol to the solid phase containing the target product, performing desorption at 40°C to 70°C for 0.5 h to 3 h, then cooling to room temperature, and filtering with a microfiltration membrane to obtain the red ginseng extract.

[0067] In some specific embodiments, the variable-temperature interactive extraction includes microwave-assisted heating.

[0068] In some specific embodiments, the variable-temperature interactive extraction includes using one of liquid nitrogen, dry ice plus water, and ethylene glycol plus water to assist in cooling.

[0069] In the above specific embodiments, the present application makes the temperature change more uniform and the temperature change speed faster through microwave-assisted heating and / or using one of liquid nitrogen, dry ice plus water, and ethylene glycol plus water to assist in cooling, further eliminating the temperature gradient inside the material, promoting the effect of variable-temperature interactive extraction, and thus further improving the extraction rate of ginsenosides.

[0070] Red ginseng extract

[0071] In a second aspect, the present application provides a red ginseng extract prepared by the preparation method of the first aspect. Optionally, based on the total mass of the red ginseng extract, the content of ginsenosides in the red ginseng extract is 0.2% to 2%. The ginsenosides in the red ginseng extract of the present application have higher stability. After the red ginseng extract is stored at room temperature for 3 months, the change rate of the content of ginsenosides in the red ginseng extract ≤ 20%. At the same time, the appearance, color, and smell of the red ginseng extract do not change after long-term storage.

[0072] It should be noted that the change rate of the content of ginsenosides in the red ginseng extract = (initial content - content after storage) / initial content × 100%.

[0073] Cosmetic composition

[0074] In a third aspect, the present application provides a cosmetic composition comprising the red ginseng extract prepared by the preparation method of the first aspect and / or the red ginseng extract of the second aspect. Optionally, based on the total mass of the cosmetic composition, the cosmetic composition comprises 0.1 wt% to 10 wt% of the red ginseng extract. This cosmetic composition can effectively improve the change rate of skin moisture loss, skin roughness, skin smoothness and skin glossiness.

[0075] Example

[0076] The following examples more specifically describe the content disclosed in the present application. These examples are only for illustrative purposes, because various modifications and variations within the scope of the present application are obvious to those skilled in the art. Unless otherwise stated, all parts, percentages and ratios reported in the following examples are based on weight, and all reagents used in the examples are commercially available or synthesized according to conventional methods and can be used directly without further treatment, and the instruments used in the examples are all commercially available.

[0077] Example 1

[0078] S100, after crushing red ginseng whiskers to 10 to 60 meshes, perform ultrasonic crushing treatment to obtain 300-mesh red ginseng powder, and add the red ginseng powder into a 30% 1,3-propanediol solvent.

[0079] S200, perform variable-temperature alternating extraction using a microwave-assisted heating device and liquid nitrogen-assisted cooling. The variable-temperature alternating extraction includes performing multiple extractions alternately at a first temperature of 85°C and a second temperature of 15°C; each extraction time is 30 min, and the total number of extractions is 6 times; quickly change the temperature between adjacent extractions, the temperature change rate is 35°C / min, and the temperature change time is 2 min; after the variable-temperature alternating extraction is completed, filter and collect the crude extract.

[0080] S300, adjust the pH of the crude extract to 5.0 using citric acid, add lipase, and enzymatically hydrolyze for 1.5 h at 45°C and pH 5.0 to obtain a first enzymatically hydrolyzed solution; add α-amylase and neutral protease to the first enzymatically hydrolyzed solution, and enzymatically hydrolyze for 2 h at 65°C and pH 6.0 to obtain a second enzymatically hydrolyzed solution; heat the second enzymatically hydrolyzed solution to 100°C and inactivate the enzyme for 30 min to obtain the enzymatically hydrolyzed extract.

[0081] S400. The phenol-sulfuric acid method was used to determine the content of crude polysaccharides in the extract after enzymatic hydrolysis. Then, under the condition of 40 °C, phytic acid was added to the extract after enzymatic hydrolysis, and the addition amount of phytic acid was 0.2 wt% of the content of crude polysaccharides in the extract after enzymatic hydrolysis. The pH of the extract after adding phytic acid was 5. After stirring and mixing evenly, it was left standing for 30 min to obtain the extract after phytic acid treatment.

[0082] S500. 600-mesh diatomaceous earth was added to the extract after phytic acid treatment, and microfiltration was used to obtain the first purified filtrate and solid impurities; 2 times the mass of red ginseng powder of D101 resin was added to the first purified filtrate, adsorbed at room temperature for 4 h, and filtered to obtain the solid phase containing the target product and the waste liquid phase; 70% propylene glycol was added to the solid phase containing the target product and desorbed at 65 °C for 2.5 h, cooled to room temperature, and filtered using a microfiltration membrane to obtain the red ginseng extract.

[0083] Examples 2 to 5

[0084] In Examples 2 to 5, the steps for preparing the red ginseng extract were similar to those in Example 1, except that some parameters in the extraction steps were changed, as shown in the corresponding items in Table 1.

[0085] Comparative examples 1 to 2

[0086] The differences between Comparative Examples 1 to 2 and Example 1 were only that in the steps of extracting red ginseng powder in Comparative Examples 1 to 2, instead of using variable-temperature interactive extraction, extraction was carried out at 85 °C for 180 min throughout and at 100 °C for 180 min throughout, respectively.

[0087] Comparative example 3

[0088] The difference between Comparative Example 3 and Example 1 was only that in Comparative Example 3, rapid temperature change was not carried out between two adjacent extractions, and the temperature change rate was only 7 °C / min, and the temperature change time was relatively long, being 10 min.

[0089] Comparative examples 4 to 5

[0090] The differences between Comparative Examples 4 to 5 and Example 1 were only that in the enzymatic hydrolysis of the crude extract in Comparative Examples 4 to 5, two-step enzymatic hydrolysis was not used, and only one-step enzymatic hydrolysis was used.

[0091] Comparative example 6

[0092] The difference between Comparative Example 6 and Example 1 was only that in Comparative Example 6, the extract was not subjected to phytic acid adsorption treatment after enzymatic hydrolysis.

[0093] Comparative examples 7 to 8

[0094] The differences between Comparative Examples 7 - 8 and Example 1 are only as follows: in the step of adding phytic acid to the extract after enzymatic hydrolysis for adsorption treatment in Comparative Examples 7 - 8, the pH of the extract after adding phytic acid was not controlled within the range of 4.8 - 5.2.

[0095] The main parameters of Examples 1 - 5 and Comparative Examples 1 - 8 are shown in Table 1.

[0096] Table 1 Process parameter table of examples and comparative examples

[0097]

[0098] Performance test

[0099] The following tests were conducted on the red ginseng extracts of Examples 1 to 5 and Comparative examples 1 to 8:

[0100] (1) For the detection of the saponin content, the vanillin - perchloric acid method in T / AHFIA 004—2018 Determination of total saponin content in foods - Spectrophotometry was used for detection.

[0101] (2) Saponin extraction rate % = mass of total saponin in the extract / mass of red ginseng powder × 100%.

[0102] (3) For the stability investigation test, the red ginseng extract was stored at room temperature in the dark for 3 months, and then samples were taken for detection. The detection items included the odor, color of the red ginseng extract, and whether the appearance was clear and transparent.

[0103] The test data of Examples 1 - 5 and Comparative Examples 1 - 8 are shown in Table 2.

[0104] Table 2 Test results of examples and comparative examples

[0105]

[0106]

[0107] It can be seen from Examples 1 to 5 and Comparative Examples 1 to 8 that in the preparation process of the red ginseng extract in Examples 1 to 5, high-low temperature alternating extraction was adopted, and extremely rapid temperature change was implemented. Through the drastic temperature change, the red ginseng cell wall was induced to rapidly expand or contract under the action of thermal expansion and contraction, thereby intensifying the stress, promoting the fragmentation of the cell wall, and improving the dissolution of active substances. During the high-low temperature alternating extraction process, the temperature in the high-temperature stage was 80-90 °C, not reaching 100 °C, and the total high-temperature extraction time was also controlled, which was beneficial to reducing the thermosensitive degradation of ginsenosides, reducing the occurrence of side reactions, and reducing the loss of ginsenosides in the extract. In addition, in Examples 1 to 5, crude polysaccharides in the extract were removed by adding phytic acid, which improved the separation and purification efficiency and the extraction rate of saponins. Therefore, the extraction rate and content of ginsenosides in the red ginseng extract prepared in Examples 1 to 5 were relatively high, and the stability was also good.

[0108] Compared with Example 1, high-low temperature alternating extraction was not adopted in Comparative Examples 1 to 2. Although high-low temperature alternating extraction was adopted in Comparative Example 3, the temperature change rate was slow. Although the stability of the red ginseng extract prepared in Comparative Examples 1 to 3 was acceptable, the extraction rate and content of ginsenosides were inferior to those in Examples 1 to 5. In Comparative Examples 4 to 5, enzymolysis with lipase, α-amylase, and / or neutral protease was not carried out, and the stability of the prepared red ginseng extract was poor. In Comparative Examples 6 to 8, phytic acid adsorption treatment was not carried out, or although phytic acid was added, the pH of the extract after phytic acid addition was not controlled within the range of 4.8-5.2, which significantly affected the extraction rate and content of ginsenosides or was not conducive to the stability of the red ginseng extract.

[0109] Preparation of the cosmetic composition of Example 6

[0110] This example provides a cosmetic composition, and the raw materials include the components shown in Table 3 in terms of mass percentage.

[0111] Table 3 Raw material formula of the cosmetic composition containing red ginseng extract

[0112]

[0113] This cosmetic composition is prepared by the following method:

[0114] Heat phase A and phase B to 85 °C respectively, stir evenly until fully dissolved or dissolved and dispersed evenly; under stirring conditions, slowly add phase B to phase A and stir to mix evenly; use a homogenizer to emulsify the A / B mixed phase into a uniform mass; stir to 50 °C, add phase C and phase D respectively, and stir until evenly mixed; slowly stir to room temperature to obtain a cosmetic composition containing red ginseng extract.

[0115] Efficacy test of the cosmetic composition:

[0116] Test instruments: Antera 3D (Miravex, Ireland), Corneometer CM825 (Courage-Khazaka, Germany), Glossymeter (Courage-Khazaka, Germany), Tewameter TM300 (Courage-Khazaka, Germany), VC20plus skin surface analysis system (Courage-Khazaka, Germany).

[0117] Subjects: A total of 5 people, aged 35 to 50 years old, meeting the volunteer inclusion criteria for subjects.

[0118] Initial visit: The subjects cleaned their faces with the cleansing products provided by the laboratory and dried them with dry paper towels. They sat quietly for 30 minutes in a constant temperature and humidity room with a temperature of 21°C and a relative humidity of 50±10%. The tester used Antera 3D to collect images of the periorbital area of the subjects' faces, and used Corneometer CM825 and Tewameter TM300 to measure the skin moisture content and transepidermal water loss of the left and right cheek areas of the subjects. The Glossymeter was used to measure the skin glossiness of the left and right cheek areas of the subjects, and the VC20plus was used to measure the roughness and smoothness of the left and right cheeks of the subjects. Each test area was tested three times, and the test data was recorded. Fourteen days after using the product, the above operations were repeated.

[0119] Evaluation of the moisturizing performance of the cosmetic composition: When the change rate of the test value of any parameter of the skin moisture content or transepidermal water loss after using the product is significantly higher than the result before use, or when the change result on the product side after using the product is significantly higher than the control side, it is determined that the product has a moisturizing effect at this test time point; otherwise, it is determined that the test product has no moisturizing effect.

[0120] Evaluation of the nourishing performance of the cosmetic composition: When the change results of the main parameters (skin smoothness SEsm, skin roughness SEr) and secondary parameters (glossiness DSC) on the test product side at any visit time point after using the product are better than those on the control side, it indicates that the test product has a nourishing effect; otherwise, it is considered that the test product has no nourishing effect.

[0121] After testing, the change rate of transepidermal water loss on the cosmetic composition side decreased by 20.64% after 14 days of using the product, while the change rate of transepidermal water loss on the blank control side decreased by 14.01% after 14 days of using the product. It can be seen that the change rate result of transepidermal water loss on the cosmetic composition side is significantly better than that on the blank control side, and the cosmetic composition of this application has good moisturizing effect.

[0122] After detection, the skin roughness SEr on the side of the cosmetic composition increased by 21.74% after 14 days of using the product, while that on the blank side decreased by 9.00%, indicating that the change rate of the skin roughness SEr on the side of the cosmetic composition was significantly better than that on the blank control side. After detection, the skin smoothness SEsm on the side of the cosmetic composition decreased by 2.64% after 14 days of using the product, while that on the blank side increased by 13.27%, indicating that the change rate of the skin smoothness SEsm on the side of the cosmetic composition was significantly better than that on the blank control side. After detection, the skin gloss DSC on the side of the cosmetic composition increased by 9.34% after 14 days of using the product, while that on the blank side increased by 8.92%, indicating that the change rate of the skin gloss DSC on the side of the test product was better than that on the blank control side. Combining the above results, it can be seen that the cosmetic composition of the present application has a good nourishing effect.

[0123] As described above, it is only the specific implementation manner of the present application, but the protection scope of the present application is not limited thereto. Any person skilled in the art within the technical scope disclosed in the present application can easily think of various equivalent modifications or substitutions, and these modifications or substitutions should be covered within the protection scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.

Claims

1. A method for preparing a red ginseng extract, characterized in that: include: Provide red ginseng powder; The red ginseng powder is added to a solvent for temperature-variable alternating extraction, wherein the solvent is an aqueous solution of 1,3-propylene glycol with a mass percentage of 10% to 50%, and after the temperature-variable alternating extraction is completed, the crude extract is separated by filtration; Adding enzyme to the crude extract for enzymolysis treatment, and deactivating the enzyme after the enzymolysis treatment to obtain an extract after enzymolysis treatment; adding phytic acid to the extract after the enzymatic hydrolysis treatment for adsorption treatment to obtain an extract after phytic acid treatment; filtering and purifying the extract after the phytic acid treatment to obtain a red ginseng extract; The variable temperature interactive extraction includes performing multiple extractions alternately at a first temperature and a second temperature, wherein the first temperature is 80°C to 90°C, and the second temperature is 10°C to 20°C; Each extraction time at the first temperature or the second temperature is 20 minutes to 30 minutes; the total number of extractions at the first temperature or the second temperature is 6 to 8 times, and the total time is less than or equal to 240 minutes; Between two adjacent extractions, the extraction temperature is rapidly changed between the first temperature and the second temperature, the temperature change rate is 20°C / min to 40°C / min, and the temperature change time is 1.5min to 4min.

2. The preparation method according to claim 1, characterized in that: The method for providing the red ginseng powder comprises: crushing the red ginseng roots to 10-60 meshes, and then performing ultrasonic crushing to obtain the red ginseng powder to 150-300 meshes.

3. The preparation method according to claim 1, characterized in that: Before adding phytic acid to the extract after the enzymatic hydrolysis treatment for adsorption treatment, the method further comprises: determining the content of crude polysaccharides in the extract after the enzymatic hydrolysis treatment by using a phenol-sulfuric acid method; In the step of adding phytic acid to the extract after the enzymatic hydrolysis treatment for adsorption treatment, the added amount of the phytic acid is 0.1wt% to 0.5wt% of the content of the crude polysaccharide.

4. The preparation method according to claim 3, characterized in that: In the step of adding phytic acid to the extract after the enzymatic hydrolysis treatment for adsorption treatment, the pH of the extract after the addition of phytic acid is 4.8 to 5.

2.

5. The preparation method according to claim 1, characterized in that: The step of adding the red ginseng powder into a solvent for temperature-variable interactive extraction, and filtering and separating to obtain a crude extract after the temperature-variable interactive extraction is completed comprises: The red ginseng powder is added to a solvent for temperature-variable alternating extraction, and after the temperature-variable alternating extraction is completed, filtering and separating to obtain a first liquid phase and a first filter residue; Performing temperature-varying alternating extraction on the first filter residue to obtain a second liquid phase and a second filter residue; The crude extract is obtained by mixing the first liquid phase and the second liquid phase.

6. The preparation method according to claim 1, characterized in that: The step of adding an enzyme to the crude extract for enzymolysis treatment, and deactivating the enzyme after the enzymolysis treatment to obtain the extract after the enzymolysis treatment comprises: Adjusting the pH of the crude extract to 4.5-10.0, adding lipase, and performing enzymolysis at a pH of 5.0-6.0 and a temperature of 40° C.-45° C. for 1 h-2 h to obtain a first enzymolysis solution, preferably, using citric acid and / or arginine for pH adjustment; Adding α-amylase and / or neutral protease to the first enzymatic hydrolyzate, performing enzymatic hydrolysis for 1 h to 3 h at a pH of 6.0 to 7.0 and a temperature of 60° C. to 65° C., to obtain a second enzymatic hydrolyzate; The second enzymatic hydrolysis solution is heated to 95° C. to 100° C. for enzyme inactivation for 0.5 h to 1 h to obtain the extract after the enzymatic hydrolysis treatment.

7. The preparation method according to claim 1, characterized in that: The step of filtering and purifying the extract after the phytic acid treatment to obtain the red ginseng extract comprises: Adding 100-800 mesh diatomaceous earth to the treated extract, mixing and filtering with a microfiltration membrane to obtain a first purified filtrate and solid impurities; Adding adsorption resin to the first purification filtrate, adsorbing at room temperature for 0.5 h to 5 h, filtering to obtain a solid phase containing the target product and a waste liquid phase; 70% propylene glycol is added to the solid phase containing the target product, and desorption is carried out at 40° C. to 70° C. for 0.5 h to 3 h, then the temperature is lowered to room temperature, and filtered using a microfiltration membrane to obtain the red ginseng extract.

8. The preparation method according to claim 1, characterized in that: The variable temperature interactive extraction includes microwave-assisted heating and / or auxiliary cooling selected from the group consisting of liquid nitrogen, dry ice plus water, and ethylene glycol plus water.

9. A red ginseng extract, characterized in that: The red ginseng extract is prepared by the preparation method according to any one of claims 1 to 8. Preferably, based on the total mass of the red ginseng extract, the content of ginsenoside in the red ginseng extract is 0.2% to 2%.

10. A cosmetic composition, characterized in that The invention comprises a red ginseng extract prepared by the preparation method according to any one of claims 1 to 8 and / or a red ginseng extract according to claim 9. Preferably, based on the total mass of the cosmetic composition, the cosmetic composition comprises 0.1 wt% to 10 wt% of the red ginseng extract.

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