A herbal composition, its extraction method and use

Abstract

The application discloses a herbal composition and an extraction method and application thereof. The herbal composition is prepared from raw materials in the following proportions by weight: wild chrysanthemum 4-8 parts, Andrographis paniculata 1-4 parts, pachouli 4-8 parts, and perilla 8-12 parts. The composition has significant soothing, antioxidant and anti-inflammatory effects and can block the occurrence of eczema from the root. The extraction method of the herbal composition combines ultrasonic extraction and supercritical CO2 extraction, and a pretreatment agent is added in the process, so that the extraction rate of water-soluble and oil-soluble active ingredients is improved, and the medicinal effect of the herbal composition is enhanced.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, and more specifically, to a herbal composition, its extraction method, and its application. Background Technology

[0002] Atopic dermatitis (AD) is a common chronic inflammatory skin disease in clinical practice, mainly referring to an allergic inflammatory skin disease caused by a variety of internal and external factors. It commonly occurs in newborns and can spread to childhood and adulthood. Eczema has a marked tendency to ooze, mainly manifested as polymorphic skin lesions such as erythema, papules, and vesicles, accompanied by intense itching and a tendency to recur, severely affecting the patient's normal life.

[0003] Currently, there are many skincare products on the market for treating infantile eczema. Many popular brands use ingredients like calendula and oatmeal as their main soothing components. While each product has its own unique features, ingredients, and effects, none truly and effectively solves the problem of infantile eczema. Most products only moisturize, and the moisturizing effect is short-lived, with negligible soothing and repairing effects. Their effectiveness fails to meet consumers' needs for a solution to infantile eczema. Products with good soothing and repairing effects often contain various hormones, which can have significant negative effects on a baby's growth with long-term use, such as poor compliance, significant side effects, and the potential for skin burning and other adverse reactions, causing irreversible damage to the infant's skin and affecting the overall treatment outcome of eczema. Clearly, current products on the market do not meet consumer needs, and there is still a need to develop and produce a new product that can truly solve the problem of infantile eczema.

[0004] Eczema is clinically characterized by intense itching and inflammatory eczematous lesions. Its pathogenesis involves skin inflammation and recurrent itching caused by damage to the skin barrier and an imbalance in the immune response. In Traditional Chinese Medicine (TCM), eczema is called "wet sores" or "impacting sores." Infantile eczema is often referred to as "fetal sores" or "milk rash." The *Zhu Bing Yuan Hou Lun* states, "Impacting sores are caused by wind-heat in the heart, manifesting on the skin." It also states, "Dampness and heat combine to cause sores on the head, face, and body." In TCM, the main causes of eczema are wind, dampness, and heat; therefore, treatment should focus on dispelling wind, eliminating dampness, and clearing heat to remove the underlying cause.

[0005] In view of this, the present invention is proposed. Summary of the Invention

[0006] The purpose of this invention is to provide a herbal composition, its extraction method, and its application. This herbal composition has antioxidant, anti-inflammatory, and moisturizing effects, and has a soothing effect on eczema. This invention also provides an extraction method for this herbal composition, which, with its improved extraction method, can maximize the extraction of active ingredients, thereby enhancing the medicinal effect of the composition. This invention further provides a moisturizing cream containing this herbal composition, which provides long-lasting soothing relief for eczema while minimizing side effects, and can effectively relieve skin pain and itching caused by eczema and diaper rash in infants.

[0007] This invention is implemented as follows:

[0008] In a first aspect, the present invention provides a herbal composition prepared from raw materials comprising the following parts by weight: 4-8 parts of wild chrysanthemum, 1-4 parts of andrographis paniculata, 4-8 parts of patchouli, and 8-12 parts of perilla.

[0009] The inventors discovered that an extract made from a combination of wild chrysanthemum, andrographis paniculata, patchouli, and perilla has significant soothing, antioxidant, and antibacterial effects, which can prevent the occurrence of eczema from the root.

[0010] By combining wild chrysanthemum and andrographis paniculata, the release of inflammatory mediators can be inhibited, the inflammatory response caused by eczema can be regulated, and the generation of cellular oxygen free radicals can be suppressed, while increasing CAT and SOD levels. By combining patchouli and perilla, the body's immunity can be regulated, the normal balance between Th1 and Th2 cellular immune states can be restored, and inflammatory cellular factors such as interleukin-6 (IL-6), interleukin-1β (IL-1β), and TNF-α can be suppressed, thereby repairing damaged skin tissue and relieving eczema symptoms.

[0011] This invention combines wild chrysanthemum, andrographis paniculata, patchouli, and perilla, which helps promote the synthesis of fibrin and maintain the moisturizing environment of the skin epidermis. At the same time, all four Chinese medicinal herbs are mild and low-irritant plants, which are unlikely to cause secondary damage to the patient's skin lesions.

[0012] From the perspective of medicinal properties, Andrographis paniculata and Chrysanthemum indicum have a bitter taste and can effectively clear heat and eliminate dampness. From the perspective of meridian tropism, many modern scholars believe that spleen deficiency leading to internal damp-heat, combined with external wind-evil attacking the internal damp-heat, resulting in accumulation in the skin, is the main cause of eczema. Patchouli and Perilla frutescens, which enter the spleen meridian, can eliminate spleen dampness and alleviate symptoms. Therefore, the combined use of these four Chinese medicinal herbs aligns with the traditional Chinese medicine treatment of "dispelling wind, eliminating dampness, and clearing heat," effectively addressing the root cause of eczema. Modern pharmacological research shows that the synergistic combination of Chrysanthemum indicum extract and Andrographis paniculata extract helps inhibit the release of inflammatory mediators, regulate the inflammatory response caused by eczema, and inhibit the generation of cellular free radicals. The synergistic combination of Patchouli extract and Perilla frutescens extract helps regulate the body's immunity, inhibit cellular inflammatory factors, thereby repairing damaged skin tissue and relieving eczema symptoms. By adding wild chrysanthemum extract, andrographis paniculata extract, patchouli extract, and perilla extract in a synergistic compound, it is beneficial to promote the synthesis of fibrin and maintain the moisturizing environment of the skin epidermis, which can effectively target the pathogenesis of eczema and block its occurrence.

[0013] Meanwhile, wild chrysanthemum, andrographis paniculata, patchouli, and perilla, as traditional Chinese medicinal herbs from Lingnan, have a long history of application in the field of traditional Chinese medicine. They are processed into Chinese herbal medicines, medicinal wines, and other preparations, widely used in clinical practice and as household medicines, and have not shown any obvious serious adverse reactions or toxic side effects. Therefore, they are all considered relatively safe drugs. Furthermore, they have important applications in both traditional Chinese medicine and food, reflecting the concept of "medicine and food sharing the same origin." Therefore, a skin composition made from these four Chinese medicinal herbs can be used to treat eczema with a high safety profile.

[0014] Secondly, the present invention provides a method for extracting the above-mentioned herbal composition, comprising the following steps:

[0015] (1) Wash the fresh plants and then mix them with the pretreatment solution to make pulp;

[0016] (2) The slurry is subjected to ultrasonic treatment and filtered to obtain pretreated plant residue and filtrate;

[0017] (3) The pretreated plant residue is subjected to a first freeze-drying to obtain dried plant powder; the filtrate is subjected to a second freeze-drying to obtain a first composition;

[0018] (4) The dried plant powder was subjected to supercritical CO2 extraction, and the pressure was reduced and the mixture was collected to obtain the second composition;

[0019] (5) Mix the first composition and the second composition to obtain the herbal composition.

[0020] This invention combines ultrasonic extraction and supercritical CO2 extraction of fresh plants, improving the extraction rates of both water-soluble and oil-soluble active ingredients. The water-soluble active ingredients include flavonoids, phenolic acids, organic acid salts, tannins, and polysaccharides, which possess anti-inflammatory, antibacterial, antioxidant, and wound-healing properties. The oil-soluble active ingredients include diterpenoid lactones, patchouli alcohol, patchouli ketone, β-patchoulene, perillaldehyde, limonene, linalool, camphor, borneol, eucalyptol, and cypermethrin, which have heat-clearing, detoxifying, blood-cooling, swelling-reducing, wind-dispelling, dampness-resolving, and cold-relieving effects. The method provided by this invention maximizes the extraction rate of these substances, enhancing the medicinal efficacy of the herbal composition.

[0021] In some embodiments, the fresh plants, calculated by weight, include: 4-8 parts wild chrysanthemum, 1-4 parts andrographis paniculata, 4-8 parts patchouli, and 8-12 parts perilla.

[0022] In some embodiments, the pretreatment solution comprises the following components by weight percentage: 5%–8% sodium phosphate, 2%–4% urea, 1%–3% trisodium ascorbate palmitate phosphate, and the balance being water.

[0023] The pretreatment solution provided by this invention contains sodium phosphate, urea, and trisodium ascorbate palmitate phosphate. On the one hand, the combination of these three substances can improve the leaching rate of water-soluble active ingredients during ultrasonic treatment. For example, sodium phosphate can chelate calcium ions, thereby destroying the cell wall structure and promoting the release of contents. At the same time, it drives the leakage of cell contents through the effect of osmotic pressure difference. Trisodium ascorbate palmitate phosphate, as a surfactant, can increase the wetting of plant powder and promote the penetration of aqueous solution. It can also chelate calcium ions and destroy cell structure. Urea can break hydrogen bonds and promote the separation of active substances from plant tissues and their dissolution into the aqueous phase. On the other hand, the three substances remaining on the plant powder after filtration can increase the damage of ice crystals to cells during freeze-drying, thereby improving the extraction rate of active ingredients during supercritical CO2 extraction. For example, the salting-out effect of sodium phosphate during freezing causes cell dehydration and shrinkage, leading to leakage of contents. Urea can break hydrogen bond structures and dissolve liposomes, causing organelle rupture.

[0024] In some embodiments, the ultrasonic treatment has a power of 200-600W, a frequency of 20-40kHz, and a duration of 30-60min.

[0025] In some embodiments, the conditions for the first freeze-drying are as follows: pre-cooling to -60 to -80°C at a rate of -2 to -5°C / min, followed by drying at -20 to -10°C, wherein the vacuum degree of the drying is 20 to 50 Pa, and the time is 12 to 24 hours.

[0026] This invention uses a relatively low cooling rate to freeze the pretreated plant residue, which is conducive to the formation of large, needle-shaped ice crystals. Combined with the use of a higher drying temperature to pierce cell membranes and organelles, it improves the extraction rate of subsequent supercritical CO2 extraction.

[0027] In some embodiments, the conditions for the second freeze-drying are as follows: pre-cooling to -60~-80°C, and then drying at -20~-10°C, wherein the vacuum degree of the drying is 20~50 Pa, and the time is 12~24 h.

[0028] In some embodiments, the supercritical CO2 extraction is performed at an extraction pressure of 15-25 MPa, an extraction temperature of 35-45°C, an extraction time of 170-200 min, and a supercritical CO2 flow rate of 55-65 kg / h. The mixing ratio of the dried plant powder and supercritical CO2 is 1 g: 1-2 mL. This invention uses relatively low extraction pressure and temperature, which helps to reduce the loss of volatile active ingredients.

[0029] In some embodiments, the pressure reduction is carried out in two stages in two separators connected in series. The first stage reduces the pressure to 5-10 MPa, and the second stage reduces it to 4-6 MPa, with the temperature of the second separator maintained at 5-15°C. This invention employs a two-stage pressure reduction and limits the temperature of the second separator, which helps to reduce the loss of volatile active ingredients.

[0030] In some embodiments, the collection refers to collecting the extract obtained from the second separation vessel as a second composition. Since components of different polarities and molecular weights precipitate under different pressures and temperatures, this design aims to precisely enrich the target active ingredient and reduce the contamination of large molecular impurities. The extract from the first separation vessel is mainly a dense paste with relatively few active ingredients. To increase the concentration of active ingredients in the extract and improve efficacy, this invention collects only the extract from the second separation vessel.

[0031] Thirdly, the present invention provides a soothing moisturizing cream comprising the following components by weight percentage: 2%-5% of the herbal composition of any of the above embodiments, 0.25%-0.35% of the skin conditioning agent, 8%-12% of the emollient, 9.5%-11.5% of the moisturizer, 1.85%-2.25% of the emulsifier, 0.28%-0.36% of the thickener, a pH adjuster for adjusting the pH value to 6.0-7.0, and the balance being water.

[0032] In some embodiments, the skin conditioning agent is selected from one or more of nitrofurazone, niacinamide, and camellia seed oil; preferably, the skin conditioning agent is composed of nitrofurazone, niacinamide, and camellia seed oil in a mass ratio of (0.1~0.13):(0.05~0.1):(0.1~0.12); more preferably, the skin conditioning agent is composed of nitrofurazone, niacinamide, and camellia seed oil in a mass ratio of 0.1:0.05:0.1; by adopting the above technical solution, the synergistic compounding of nitrofurazone, niacinamide, and camellia seed oil in a specific ratio is beneficial to soothe inflammatory response, promote rapid repair of skin lesions, and at the same time has a synergistic effect on the antibacterial effect of the moisturizing cream.

[0033] In some embodiments, the emollient is selected from one or more of dioctyl ether, cetearyl alcohol, behenol, rice bran wax, polydimethylsiloxane, cetyl ethylhexanoate, and diethoxyethyl succinate. Preferably, the emollient is composed of dioctyl ether, cetearyl alcohol, and behenol in a mass ratio of (3-4):(2-3):(1-2); more preferably, the emollient is composed of dioctyl ether, cetearyl alcohol, and behenol in a mass ratio of 3.5:2.5:1.5. By adopting the above technical solution, using one or more of the above substances as emollients, it is beneficial to relieve the inflammatory symptoms of eczema and the skin pain and itching caused by diaper rash in infants, and promote the repair and regeneration of the damaged areas.

[0034] In some embodiments, the moisturizer is selected from one or more of butylene glycol, sodium hyaluronate, 1,2-pentanediol, 1,2-hexanediol, and ethylhexylglycerin; preferably, the moisturizer is a mixture of materials in the following mass ratio: 2-3 kg of butylene glycol, 1-2 kg of sodium hyaluronate, 2-4 kg of 1,2-pentanediol, 1-3 kg of 1,2-hexanediol, and 1-2 kg of ethylhexylglycerin; more preferably, the moisturizer is a mixture of materials in the following mass ratio: 2.2 kg of butylene glycol, 1.5 kg of sodium hyaluronate, 3 kg of 1,2-pentanediol, 1.8 kg of 1,2-hexanediol, and 1.5 kg of ethylhexylglycerin. By adopting the above technical solution, using one or more substances as moisturizers, it is beneficial to increase the skin's moisture content, improve dry skin conditions, and soothe inflammatory responses.

[0035] In some embodiments, the emulsifier is selected from one or more of cetearyl alcohol, olive oil ester, and cetearyl glucoside; preferably, the emulsifier is a mixture of materials in the following mass ratio: 1-2 kg of cetearyl alcohol and 0.5-1.5 kg of olive oil ester; more preferably, the emulsifier is a mixture of materials in the following mass ratio: 1.5 kg of cetearyl alcohol and 0.7 kg of olive oil ester. By adopting the above technical solution, using one or more of the above substances as emulsifiers, it is beneficial to ensure that multiple active ingredients are mixed evenly and maintain a stable state; at the same time, it is also beneficial to allow the moisturizing cream to have better contact with the skin, penetrate the skin more easily, and promote the absorption of active ingredients.

[0036] In some embodiments, the thickener is selected from one or more of Sphingomonas fermentation product extract and acrylate / C10-30 alkanol acrylate cross-linked polymers; preferably, the thickener is a mixture of materials in the following mass ratio: 3-5 kg ​​of Sphingomonas fermentation product extract and 2-3 kg of acrylate / C10-30 alkanol acrylate cross-linked polymer; more preferably, the thickener is a mixture of materials in the following mass ratio: 4.5 kg of Sphingomonas fermentation product extract and 2.5 kg of acrylate / C10-30 alkanol acrylate cross-linked polymer.

[0037] In some embodiments, the pH adjuster is a hydrochloric acid solution and / or a sodium hydroxide solution; preferably, the concentration of the hydrochloric acid solution or sodium hydroxide solution is 1 mol / L.

[0038] In some implementations, the pH value is adjusted to 6.3 to 6.7.

[0039] Fourthly, the present invention provides a method for preparing the soothing moisturizing cream in any of the above embodiments, comprising the following steps:

[0040] (1) Preparation of oil phase: Mix emulsifier, emollient and skin conditioner and heat to 80-85℃ to melt, stir evenly, and use as oil phase, keep warm for later use;

[0041] (2) Preparation of aqueous phase: Mix the humectant, thickener and distilled water, homogenize with a homogenizer until there are no particles, heat to 80-85℃ and homogenize again to obtain the aqueous phase, and keep it warm for later use.

[0042] (3) Preparation of moisturizing cream: Pour the oil phase into the aqueous phase, homogenize at 7000-8000 rpm for 3 minutes, stir and cool to 40-45℃, add the herbal composition and stir evenly, then add pH adjuster to adjust pH to 6.0-7.0, continue to homogenize at 40-45℃ for 1-3 minutes to obtain moisturizing cream.

[0043] The moisturizing cream provided by this invention uses easily absorbed oils and pure natural extracts, and contains no pigments, preservatives, fragrances, fluorescent agents, hormones and alcohol, thus ensuring the safety, non-toxicity, stability and effectiveness of the baby eczema moisturizing cream in terms of product excipients.

[0044] The present invention has the following beneficial effects:

[0045] (1) The present invention provides a herbal composition that has significant soothing, antioxidant and anti-inflammatory effects and can block the occurrence of eczema from the root.

[0046] (2) The present invention provides an extraction method for herbal composition, which combines ultrasonic extraction and supercritical CO2 extraction, and adds a pretreatment agent during the process to improve the extraction rate of water-soluble and oil-soluble active ingredients, thereby enhancing the medicinal effect of the herbal composition. Attached Figure Description

[0047] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0048] Figure 1 The images show photographs of the back skin and pathological sections of the skin tissue of mice in Example 1, the positive control group, the blank control group, and the model group in Test Example 4. Detailed Implementation

[0049] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0050] In the description of the embodiments of this application, the technical terms "first" and "second" are used only to distinguish different objects and should not be construed as indicating or implying relative importance or implicitly indicating the number, specific order, or primary and secondary relationship of the indicated technical features.

[0051] The term "embodiment" in this document means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The appearance of this phrase in various places in the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment that is mutually exclusive with other embodiments.

[0052] In the embodiments of this application, the term "or / and" is only a description of the relationship between related objects, indicating that there can be three kinds of relationships. For example, A or / and B can represent three situations: A exists alone, A and B exist at the same time, and B exists alone.

[0053] Additionally, the character " / " in this article generally indicates that the objects before and after it are in an "or" relationship.

[0054] In the embodiments of this application, "multiple" means two or more (including two), similarly, "multiple groups" means two or more (including two groups), and "multiple layers" means two or more (including two layers), unless otherwise explicitly specified and limited.

[0055] In the embodiments of this application, "at least one" means one or more.

[0056] Those skilled in the art can understand the specific meaning of the above terms in the embodiments of this application according to the specific circumstances.

[0057] The features and performance of the present invention will be further described in detail below with reference to embodiments.

[0058] Example 1

[0059] This embodiment provides a herbal composition prepared from the following raw materials in parts by weight: 4 parts wild chrysanthemum, 2 parts andrographis paniculata, 6 parts patchouli, and 9 parts perilla.

[0060] The extraction method of the above-mentioned herbal composition includes the following steps:

[0061] (1) Wash fresh wild chrysanthemum, andrographis paniculata, patchouli and perilla with clean water, centrifuge and dehydrate, then mix with pretreatment liquid at a ratio of 1g:2mL according to the formula to obtain plant pulp;

[0062] The pretreatment solution comprises the following components by mass percentage: 6% sodium phosphate, 3% urea, 2% trisodium ascorbate palmitate phosphate, and the remainder is water.

[0063] (2) The plant pulp was subjected to ultrasonic treatment and then filtered to obtain pretreated plant residue and filtrate;

[0064] The ultrasonic treatment has a power of 500W, a frequency of 25kHz, and is performed intermittently, with a 4-second on and 3-second off cycle, for a total duration of 40 minutes.

[0065] (3) The pretreated plant residue was pre-cooled to -70℃ at -3℃ / min and then dried at -10℃ with a vacuum of 25Pa for 16h to obtain dried plant powder; the filtrate was pre-cooled to -60℃ and then dried at -10℃ with a vacuum of 25Pa for 12h to obtain the first composition.

[0066] (4) Place the dried plant powder in a supercritical CO2 extractor. The extraction temperature is 40℃, the extraction pressure is 20MPa, the supercritical CO2 flow rate is 60kg / h, the mixing ratio of dried plant powder and supercritical CO2 is 1g:2mL, and the extraction time is 180min. After the extraction is completed, open the separation vessel. The fluid passes through the first separation vessel and then flows into the second separation vessel. Collect the residue in the second separation vessel as the second composition. The pressure of the first separation vessel is 10MPa, and the temperature is not controlled. The pressure of the second separation vessel is 5MPa, and the temperature is 10℃.

[0067] (5) Mix the first composition and the second composition to obtain the herbal composition.

[0068] Example 2

[0069] The difference from Example 1 is that the first drying conditions in step (3) are as follows: the pretreated plant residue is placed in liquid nitrogen at -196°C for rapid freezing, and then dried at -20°C for 24 hours with a vacuum of 25 Pa to obtain dried plant powder.

[0070] Example 3

[0071] This embodiment provides a herbal composition prepared from the following raw materials in parts by weight: 8 parts wild chrysanthemum, 1 part andrographis paniculata, 7 parts patchouli, and 8 parts perilla.

[0072] The extraction method of the above-mentioned herbal composition includes the following steps:

[0073] (1) Wash fresh wild chrysanthemum, andrographis paniculata, patchouli and perilla with clean water, centrifuge and dehydrate, then mix with pretreatment liquid at a ratio of 1g:1.5mL according to the formula to obtain plant pulp;

[0074] The pretreatment solution comprises the following components by mass percentage: 5% sodium phosphate, 2% urea, 1% trisodium ascorbate palmitate phosphate, and the remainder is water.

[0075] (2) The plant pulp was subjected to ultrasonic treatment and then filtered to obtain pretreated plant residue and filtrate;

[0076] The ultrasonic treatment has a power of 200W, a frequency of 20kHz, and is performed intermittently, with a 4-second on and 3-second off cycle, for a total duration of 30 minutes.

[0077] (3) The pretreated plant residue was pre-cooled to -60℃ at -2℃ / min and then dried at -20℃ with a vacuum of 25Pa for 16h to obtain dried plant powder; the filtrate was pre-cooled to -60℃ and then dried at -10℃ with a vacuum of 20Pa for 24h to obtain the first composition.

[0078] (4) Place the dried plant powder in a CO2 supercritical extractor. The extraction temperature is 45℃, the extraction pressure is 15MPa, the supercritical CO2 flow rate is 65kg / h, the mixing ratio of dried plant powder and supercritical CO2 is 1g:2mL, and the extraction time is 170min. After the extraction is completed, open the separation vessel. The fluid passes through the first separation vessel and then flows into the second separation vessel. Collect the residue in the second separation vessel as the second composition. The pressure of the first separation vessel is 6MPa, and the temperature is not controlled. The pressure of the second separation vessel is 5MPa, and the temperature is 5℃.

[0079] (5) Mix the first composition and the second composition to obtain the herbal composition.

[0080] Example 4

[0081] This embodiment provides a herbal composition prepared from the following raw materials in parts by weight: 7 parts wild chrysanthemum, 4 parts andrographis paniculata, 8 parts patchouli, and 11 parts perilla.

[0082] The extraction method of the above-mentioned herbal composition includes the following steps:

[0083] (1) Wash fresh wild chrysanthemum, andrographis paniculata, patchouli and perilla with clean water, centrifuge and dehydrate, then mix with pretreatment liquid at a ratio of 1g:2.5mL according to the formula to obtain plant pulp;

[0084] The pretreatment solution comprises the following components by mass percentage: 8% sodium phosphate, 4% urea, 3% trisodium ascorbate palmitate phosphate, and the remainder is water.

[0085] (2) The plant pulp was subjected to ultrasonic treatment and then filtered to obtain pretreated plant residue and filtrate;

[0086] The ultrasonic treatment has a power of 600W, a frequency of 40kHz, and is performed intermittently, with a 4-second on and 3-second off cycle, for a total duration of 60 minutes.

[0087] (3) The pretreated plant residue was pre-cooled to -80℃ at -5℃ / min and then dried at -20℃ with a vacuum of 40Pa for 12h to obtain dried plant powder; the filtrate was pre-cooled to -60℃ and then dried at -10℃ with a vacuum of 20Pa for 24h to obtain the first composition.

[0088] (4) Place the dried plant powder in a CO2 supercritical extractor. The extraction temperature is 35℃, the extraction pressure is 25MPa, the supercritical CO2 flow rate is 55kg / h, the mixing ratio of dried plant powder and supercritical CO2 is 1g:1mL, and the extraction time is 200min. After the extraction is completed, open the separation vessel. The fluid passes through the first separation vessel and then flows into the second separation vessel. Collect the residue in the second separation vessel as the second composition. The pressure of the first separation vessel is 10MPa, and the temperature is not controlled. The pressure of the second separation vessel is 5MPa, and the temperature is 15℃.

[0089] (5) Mix the first composition and the second composition to obtain the herbal composition.

[0090] Example 5

[0091] The difference from Example 1 is that in step (1), fresh wild chrysanthemum, andrographis paniculata, patchouli and perilla are washed with clean water, centrifuged and dehydrated, and then mixed with 5wt% ethanol aqueous solution at a ratio of 1g:2.5mL to obtain plant pulp, which is then subjected to subsequent ultrasonic treatment.

[0092] Example 6

[0093] The difference from Example 1 is that in step (1), fresh wild chrysanthemum, andrographis paniculata, patchouli and perilla are washed with clean water, centrifuged and dehydrated, and then mixed with 8wt% urea aqueous solution at a ratio of 1g:2.5mL to obtain plant pulp, which is then subjected to subsequent ultrasonic treatment.

[0094] Example 7

[0095] The difference from Example 1 is that in step (1), fresh wild chrysanthemum, andrographis paniculata, patchouli and perilla are washed with clean water, centrifuged and dehydrated, and then mixed with 8wt% sodium phosphate aqueous solution at a ratio of 1g:2.5mL to obtain plant pulp, which is then subjected to subsequent ultrasonic treatment.

[0096] Example 8

[0097] The difference from Example 1 is that in step (1), fresh wild chrysanthemum, andrographis paniculata, patchouli and perilla are washed with clean water, centrifuged and dehydrated, and then mixed with 3wt% sodium dodecyl sulfate at a ratio of 1g:2.5mL to obtain plant pulp, which is then subjected to subsequent ultrasonic treatment.

[0098] Example 9

[0099] This embodiment provides a herbal composition prepared from the following raw materials in parts by weight: 7 parts wild chrysanthemum, 4 parts andrographis paniculata, 8 parts patchouli, and 11 parts perilla.

[0100] The extraction method of the above-mentioned herbal composition includes the following steps:

[0101] (1) Wash fresh wild chrysanthemum, andrographis paniculata, patchouli and perilla with clean water, and then pulverize them at low temperature to obtain plant powder; the low temperature pulverization is carried out by pre-freezing at -60℃, drying at -20℃, vacuum degree of 25Pa, time of 12h, and finally crushing at room temperature.

[0102] (2) Place the plant powder in a CO2 supercritical extractor, with an extraction temperature of 40℃, an extraction pressure of 25MPa, a supercritical CO2 flow rate of 60kg / h, a mixing ratio of 1g:2mL for the dried plant powder and supercritical CO2, and an extraction time of 200min. After the extraction is completed, open the separation vessel, and the fluid passes through the first separation vessel and then flows into the second separation vessel. Collect the residue in the second separation vessel as the second composition. The pressure in the first separation vessel is 10MPa, and the temperature is not controlled. The pressure in the second separation vessel is 5MPa, and the temperature is 15℃. Collect the extract from the second separation vessel as the herbal composition.

[0103] Example 10

[0104] The difference from Example 1 is that the second composition is used as the herbal composition.

[0105] Example 11

[0106] The difference from Example 1 is that the first composition is used as the herbal composition.

[0107] Example 12

[0108] This embodiment provides a herbal composition prepared from the following raw materials in parts by weight: 7 parts wild chrysanthemum, 4 parts andrographis paniculata, 8 parts patchouli, and 11 parts perilla.

[0109] The extraction method of the above-mentioned herbal composition is based on Example 9, wherein the plant powder remaining after supercritical CO2 extraction is subjected to ultrasonic extraction to obtain an extract, and the extract obtained by freeze-drying the extract is combined with the extract from the second separation vessel to obtain the herbal composition. The ultrasonic extraction includes: dispersing the plant powder in a pretreatment solution, subjecting it to ultrasonic treatment, and obtaining the extract by pressure filtration; the pretreatment solution includes the following components by mass percentage: 6% sodium phosphate, 3% urea, 2% trisodium ascorbate palmitate phosphate, and the balance being water; the ultrasonic treatment power is 500W, the frequency is 25kHz, and it is performed intermittently, with a 4s on and 3s off cycle, for a total time of 40min.

[0110] Test Example 1: In vitro antioxidant effect of herbal composition

[0111] Each herbal composition solution with a concentration of 100 mg / L was taken and tested using a DPPH free radical scavenging ability test kit (purchased from Nanjing Jiancheng) according to the kit instructions. Control tube solutions, test tube solutions, and blank tube solutions were prepared separately (as shown in Table 1 below), mixed well, and incubated at room temperature (25℃) in the dark for 30 min. After centrifugation at 400 rpm for 5 min, 800 µL was transferred to a cuvette, zeroed with anhydrous ethanol, and the absorbance value of each tube was measured at 517 nm. Vitamin C was used as a positive control in this experiment. The DPPH free radical scavenging rate of each sample was calculated using the following formula: DPPH free radical scavenging rate (%) = [1 - (A...] 测定管 -A 对照管 )÷A 空白管 ]×100%, where A 测定管 To measure the absorbance of the tube, A 对照管 A is the absorbance of the control tube. 空白管 The absorbance values ​​are for the blank tubes. The average DPPH free radical scavenging rates of the herbal compositions in each embodiment are shown in Table 2.

[0112] Table 1

[0113]

[0114] Table 2

[0115]

[0116] In comparison with the model control group, * indicates a significant difference (p < 0.05), and ** indicates a highly significant difference (p < 0.01). Statistical analysis was performed using SPSS software. Independent sample t-tests were used to compare the DPPH free radical scavenging rates of the experimental samples, positive control, and negative control. All statistical analyses were two-tailed tests; P > 0.05 indicated no significant difference between the two groups, and P < 0.05 indicated a significant difference between the two groups. Unless otherwise specified, all other statistical data processing in this paper was performed in the same manner.

[0117] Analysis of Table 2 shows that the antioxidant capacity of the herbal compositions in Examples 1 and 4 is comparable to that of the strong antioxidant vitamin C. Experimental results indicate that the herbal compositions possess good in vitro antioxidant activity. Furthermore, the herbal composition prepared in Example 2, due to the use of rapid freezing for the first drying step, exhibited a lower antioxidant effect than that in Example 1. This suggests that slowing down the cooling rate is beneficial for improving the extraction rate of active ingredients, as a lower cooling rate facilitates the formation of larger needle-like ice crystals that disrupt the plant's cell structure, releasing the effective substances. Examples 5-8, using a single urea solution, sodium phosphate solution, and sodium dodecyl sulfate solution respectively during ultrasonic extraction, all showed inferior antioxidant effects compared to Example 1. This indicates that the synergistic effect of sodium phosphate, urea, and trisodium ascorbate palmitate phosphate can improve the extraction rate of active ingredients. Example 9 prepared the herbal composition using conventional supercritical CO2 extraction. However, because water-soluble active substances are difficult to dissolve in the lipophilic supercritical CO2 fluid, and polyphenols and flavonoids with antioxidant properties are too polar to be extracted into the supercritical CO2 fluid, the antioxidant effect of Example 9 was poor. Example 12 reversed the order of steps, first using low-temperature crushing and drying to break the cell walls, then supercritical extraction, and finally ultrasonic extraction. The resulting herbal composition had a lower antioxidant effect than Example 1. This is because some active ingredients with antioxidant properties were extracted during supercritical extraction, and due to their low solubility, they usually remained in the first separation vessel, leading to a lower concentration of active ingredients in the final product, thus resulting in a poorer antioxidant effect.

[0118] Test Example 2: In vitro moisturizing effect of herbal composition

[0119] The inhibitory effect of the herbal compositions in each example on hyaluronidase was determined using the modified Elson-Morgan method to evaluate the moisturizing effect of the compositions. Take 0.5 mL of a 100 mg / L herbal composition solution into a 10 mL test tube as the sample solution. Add 0.5 mL of 500 U / mL hyaluronidase and mix well. Incubate at 37 ℃ for 20 min. Remove the test tube and add 0.1 mL of 2.5 mol / L calcium chloride solution. Incubate at 37 ℃ for 20 min. Remove the test tube and add 0.5 mL of 0.5 mg / mL potassium hyaluronic acid solution. Incubate at 37 ℃ for 40 min. Remove the test tube and let it stand for 5 min. Add 2 drops of 5 mol / L NaOH solution and 0.5 mL of acetylacetone solution. Incubate in a boiling water bath for 15 min, then cool in an ice water bath for 5 min. Remove the test tube and let it stand for 10 min. Add 0.5 mL of distilled water, 0.5 mL of Ehrlich's reagent, and 2 mL of concentrated HCl. Add anhydrous ethanol to a final volume of 10 mL. Shake well and let stand for 30 min. Develop the color at 530 °C. The absorbance was measured at nm, with dipotassium glycyrrhizate of the same mass concentration used as a positive control. The hyaluronidase inhibition rate of each sample was calculated using the following formula: Hyaluronidase inhibition rate (%) = (1 - (CD) / (AB)) × 100%, where A is the absorbance of the solution without the sample; B is the absorbance of the solution without the sample and enzyme; C is the absorbance of the solution containing the sample and enzyme; and D is the absorbance of the solution containing the sample and without the enzyme. The hyaluronidase inhibition rate detection results for each Example 1 are shown in Table 3.

[0120] Table 3

[0121]

[0122] In the table, compared with the model control group, *: P<0.05, indicating a significant difference, **: p<0.01, indicating a highly significant difference.

[0123] The results showed that the herbal composition provided by the present invention has a good hyaluronidase inhibition rate, indicating that the herbal composition has a good in vitro moisturizing effect; the herbal composition of Example 1 is significantly better than other extracts, and its antihyaluronidase ability is comparable to that of dipotassium glycyrrhizate.

[0124] Test Example 3: In vitro anti-inflammatory effect of herbal composition

[0125] HaCaT cells were cultured in DMEM at 37°C under CO2 conditions, with the medium changed every 48 hours until cell confluence reached 80% or higher. They were then divided into the following groups: a control group (normal cell culture), an LPS model group (model injury group), a treatment group (herbal composition + model group), and a positive control group (dexamethasone + model group). Except for the control group, all other groups were treated with 1 μg / mL LPS for 24 hours, followed by culture in either normal medium (LPS model group), medium containing 100 mg / L of the herbal composition (treatment group), or medium containing 100 mg / L of dexamethasone (positive control group) for another 24 hours. The supernatant was then collected, and the concentration of pro-inflammatory factors in the supernatant was detected using an ELISA kit (Abcam).

[0126] The concentrations of pro-inflammatory factors TNF-α and IL-1β were detected according to the kit method. The main steps included: diluting the supernatant to the detection range of the ELISA kit, then adding it to a 96-well plate coated with antibody and incubating it, then adding the antibody of the target analyte and the colorimetric reagent TMB, adding the reaction stop solution, and then using a microplate reader to detect the readings. A standard curve was plotted based on the standard provided in the kit, and the concentration of pro-inflammatory factors in the supernatant was calculated. The results are shown in Table 4.

[0127] Table 4

[0128]

[0129] In the table, compared with the model control group, *: P<0.05, indicating a significant difference, **: p<0.01, indicating a highly significant difference.

[0130] As shown in Table 4, after treatment of model cells with the herbal composition provided by the present invention, the levels of pro-inflammatory factors TNF-α and IL-1β secreted by the cells were significantly downregulated compared with those in the model group, indicating that the herbal composition has a good in vitro anti-inflammatory effect. In particular, the herbal composition of Example 1 showed a significantly better effect than other extracts. In addition, it was noted that in Example 2, due to the use of rapid freezing in the first drying step, the anti-inflammatory effect of the prepared herbal composition was not as good as that in Example 1. This indicates that slowing down the cooling rate is beneficial to improving the extraction rate of active ingredients, because a lower cooling rate is conducive to the formation of larger needle-like ice crystals that damage the cell structure of the plant and release the effective substances. In Examples 5-8, a single ethanol solution, urea solution, sodium phosphate solution, and sodium dodecyl sulfate solution were used for ultrasonic extraction, respectively. The anti-inflammatory effects of the resulting herbal compositions were all worse than those in Example 1. This indicates that the synergistic effect of sodium phosphate, urea, and trisodium ascorbate palmitate phosphate can improve the extraction rate of active ingredients. In Example 12, the order of steps was changed and the product from the first separation vessel was collected in order to retain the polar active ingredients. The concentration of active ingredients in the resulting herbal composition was lower, and therefore the anti-inflammatory effect was not as good as that in Example 1.

[0131] Test Example 4: In vivo anti-dermatitis effect of herbal composition

[0132] Balb / C mice aged 6-8 weeks were randomly divided into the following groups, with 5 mice in each group: blank control group, model group (i.e., model injury group), drug treatment group (herbal composition + model group), and positive control group (mometasone furoate cream + model group). One day before the formal experiment, the backs of the mice were shaved using a shaver over an area of ​​approximately 3 × 3 cm. 2 On days 1, 3, 5, and 7, 200 μL of a 1 wt% 2,4-dinitrochlorobenzene (DNCB) solution was applied to the backs of mice. Starting from day 4, 200 μL of a 1.5 g / mL herbal composition or a 0.1 wt% mometasone furoate cream was applied to the backs of mice daily for treatment. On day 7, the degree of skin inflammation in the mice was assessed by photograph. Simultaneously, the degree of epidermal water loss was evaluated using a skin imaging analyzer (model PRO-B, brand: meicet®). The total water loss (TWEL) and erythema values ​​of the mice are shown in Table 5. Photographs of the back skin and histopathological sections of the mice in Example 1, the positive control group, the blank control group, and the model group are shown in Table 5. Figure 1 .

[0133] Table 5

[0134]

[0135] In the table, compared with the model control group, *: P<0.05, indicating a significant difference, **: p<0.01, indicating a highly significant difference.

[0136] The above results show that the herbal composition provided by the present invention significantly reduced skin crusting and ulceration in mice after treatment, and the epidermal water loss rate and erythema value were significantly lower than those in the model group and the positive control group. Figure 1 HE staining results in skin tissue sections showed that, compared with the model group, the treatment group mice exhibited reduced epidermal thickening on the back, decreased inflammatory cell infiltration in the dermis, and improved pathological changes such as hyperkeratosis of the stratum corneum, thickening of the granular layer, and downward displacement of the basal layer. These results indicate that the herbal composition can effectively alleviate the inflammatory symptoms of DNCB-induced dermatitis.

[0137] Application Example 1

[0138] This embodiment provides a soothing moisturizing cream, which, by weight percentage, comprises the following components:

[0139] The herbal composition obtained in Example 1 contains 3.5% skin conditioning agent, 0.3% skin moisturizer, 10% moisturizer, 10.5% humectant, 2% emulsifier, 0.32% thickener, 0.04% pH adjuster, and the balance is water; the pH value of the resulting soothing moisturizing cream is 6.44.

[0140] The skin conditioning agent is composed of a mixture of sphingolipid, niacinamide, and camellia seed oil in a mass ratio of 1:0.5:1; the emollient is composed of a mixture of dioctyl ether, cetearyl alcohol, and behenyl alcohol in a mass ratio of 0.7:0.5:0.3; the moisturizer is composed of a mixture of butylene glycol, sodium hyaluronate, 1,2-pentanediol, 1,2-hexanediol, and ethylhexylglycerin in a mass ratio of 2.2:1.5:3:1.8:1.5; the emulsifier is composed of a mixture of cetearyl alcohol and olive oil esters in a mass ratio of 1.5:0.7; the thickener is composed of a mixture of Sphingomonas fermentation product extract (purchased from Shanghai Yuyu Company) and acrylate / C10-30 alkanol acrylate crosspolymer (purchased from Wuhan Lanabai Company) in a mass ratio of 0.9:0.5; and the pH adjuster is a 1M hydrochloric acid solution.

[0141] The preparation method of the moisturizing cream in this embodiment includes the following steps:

[0142] (1) Preparation of oil phase: Mix emulsifier, emollient and skin conditioner and heat to 80°C to melt them completely. Stir evenly and use as oil phase. Keep warm for later use.

[0143] (2) Preparation of aqueous phase: Mix the humectant, thickener and distilled water, homogenize with a homogenizer until there are no particles, heat to 80°C and homogenize again to obtain the aqueous phase, and keep it warm for later use.

[0144] (3) Preparation of herbal moisturizing cream: Pour the oil phase into the water phase, homogenize at 7000 rpm for 3 minutes, stir and cool to 40°C, add the herbal composition, stir evenly, add pH adjuster to adjust the pH of the material to 6.44, continue to homogenize at 7000 rpm for 2 minutes, and ultrasonic defoaming to obtain the herbal moisturizing cream.

[0145] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for extracting a herbal composition, characterized in that, Includes the following steps: (1) Wash the fresh plants and then mix them with the pretreatment solution to make pulp; (2) The slurry is subjected to ultrasonic treatment and filtered to obtain pretreated plant residue and filtrate; (3) The pretreated plant residue is subjected to a first freeze-drying to obtain dried plant powder; the filtrate is subjected to a second freeze-drying to obtain a first composition; (4) The dried plant powder was subjected to supercritical CO2 extraction, and the pressure was reduced and the mixture was collected to obtain the second composition; (5) The first composition and the second composition are mixed to obtain the herbal composition; The fresh plants, calculated by weight, consist of the following components: 4-8 parts wild chrysanthemum, 1-4 parts andrographis paniculata, 4-8 parts patchouli, and 8-12 parts perilla. The pretreatment solution comprises the following components by mass percentage: 5%~8% sodium phosphate, 2%~4% urea, 1%~3% trisodium ascorbate palmitate phosphate, and the balance being water; The conditions for the first freeze-drying are as follows: pre-cooling to -60~-80℃ at -2~-5℃ / min, and then drying at -20~-10℃, with a vacuum degree of 20~50Pa and a time of 12~24h; The supercritical CO2 extraction is performed at an extraction pressure of 15-25 MPa, an extraction temperature of 35-45°C, an extraction time of 170-200 min, and a supercritical CO2 flow rate of 55-65 kg / h. The mixing ratio of the dried plant powder and supercritical CO2 is 1 g: 1-2 mL. The pressure reduction is carried out in two stages in two series-connected separation vessels. In the first stage, the pressure is reduced to 5-10 MPa, and in the second stage, the pressure is reduced to 4-6 MPa, with the temperature of the second separation vessel being 5-15°C. The collection involves collecting the extract obtained from the second separation vessel as the second composition.

2. The extraction method of the herbal composition according to claim 1, characterized in that, The ultrasonic treatment has a power of 200~600W, a frequency of 20~40kHz, and a duration of 30~60min; And / or, the conditions for the second freeze-drying are as follows: pre-cooling to -60~-80℃, and then drying at -20~-10℃, wherein the vacuum degree of the drying is 20~50Pa, and the time is 12~24h.

3. A soothing moisturizing cream, characterized in that, The composition comprises the following components by weight percentage: 2%-5% of the herbal composition prepared by any of the preparation methods of claims 1-2, 0.25%-0.35% of the skin conditioning agent, 8%-12% of the emollient, 9.5%-11.5% of the moisturizer, 1.85%-2.25% of the emulsifier, 0.28%-0.36% of the thickener, a pH adjuster for adjusting the pH value to 6.0-7.0, and the balance being water.

4. The soothing moisturizing cream according to claim 3, characterized in that, The skin conditioning agent is selected from one or more of the following: loratadine, niacinamide, and camellia seed oil; And / or, the emollient is selected from one or more of dioctyl ether, cetearyl alcohol, behenyl alcohol, rice bran wax, polydimethylsiloxane, cetyl ethylhexanoate and diethoxyethyl succinate; And / or, the moisturizer is selected from one or more of butylene glycol, sodium hyaluronate, 1,2-pentanediol, 1,2-hexanediol and ethylhexylglycerin; And / or, the emulsifier is selected from one or more of cetearyl alcohol, olive oil ester and cetearyl glucoside; And / or, the thickener is selected from one or more of the following: Sphingomonas fermentation product extract and acrylate / C10-30 alkanol acrylate crosspolymers; And / or, the pH adjuster is a hydrochloric acid solution and / or a sodium hydroxide solution.

5. A soothing moisturizing cream according to claim 4, characterized in that, The skin conditioning agent is composed of nitroglycerin, niacinamide, and camellia seed oil in a mass ratio of (0.1~0.13):(0.05~0.1):(0.1~0.12); And / or, the emollient is composed of dioctyl ether, cetearyl alcohol, and behenol in a mass ratio of (3~4):(2~3):(1~2); And / or, the moisturizer is a mixture of the following materials in the following mass ratios: 2-3 kg of butylene glycol, 1-2 kg of sodium hyaluronate, 2-4 kg of 1,2-pentanediol, 1-3 kg of 1,2-hexanediol and 1-2 kg of ethylhexylglycerin; And / or, the emulsifier is a mixture of materials in the following mass ratio: 1-2 kg of cetearyl alcohol and 0.5-1.5 kg of olive oil ester; And / or, the thickener is a mixture of the following materials in the following mass ratio: 3-5 kg ​​of Sphingomonas fermentation product extract and 2-3 kg of acrylate / C10-30 alkanol acrylate crosspolymer; And / or, the concentration of the hydrochloric acid solution or sodium hydroxide solution is 1 mol / L; And / or, the pH value is adjusted to 6.3~6.

7.

6. The method for preparing a soothing moisturizing cream according to claim 4, characterized in that, Includes the following steps: (1) Preparation of oil phase: Mix emulsifier, emollient and skin conditioner and heat to 80-85℃ to melt, stir evenly, and use as oil phase, keep warm for later use; (2) Preparation of aqueous phase: Mix the humectant, thickener and distilled water, homogenize with a homogenizer until there are no particles, heat to 80-85℃ and homogenize again to obtain the aqueous phase, and keep it warm for later use. (3) Preparation of moisturizing cream: Pour the oil phase into the aqueous phase, homogenize at 7000-8000 rpm for 3 minutes, stir and cool to 40-45℃, add the herbal composition and stir evenly, then add pH adjuster to adjust pH to 6.0-7.0, continue to homogenize at 40-45℃ for 1-3 minutes to obtain moisturizing cream.

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