Composite plant extract coated micro-capsule, preparation method thereof and application of micro-capsule in preparation of anti-hair-loss and hair-growing essential oil
By preparing composite microcapsules of 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin, plant extracts and ginger essential oil, the shortcomings of microencapsulated hair loss preparations in stability and release control were solved, and significant anti-hair loss effect and hair growth promotion were achieved.
Patent Information
- Application Number
- CN202510720785.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-30
- Publication Date
- 2025-08-19
- Estimated Expiration
- 2045-05-30
AI Technical Summary
In the prior art, plant extract microencapsulated hair loss preparations have shortcomings in stability, release control and anti-hair loss effects, and it is difficult to effectively promote hair growth and prevent hair loss.
Complex plant extract-encapsulated microcapsules were prepared by 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin, plant extract and ginger essential oil. Through specific fermentation and high-concentration ethanol extraction methods, the coating effect and sustained release of the microcapsules were enhanced and the activity of type I 5α reductase enzyme was inhibited.
It significantly improves the efficacy and sustained release of microcapsules, effectively promotes hair growth and prevents hair loss, and enhances the anti-hair loss effect.
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Abstract
Description
Technical Field
[0001] The invention relates to a composite plant extract-wrapped microcapsule, a preparation method thereof and application thereof in the preparation of anti-hair loss and hair growth essential oil, belonging to the technical field of hair preparations. Background Art
[0002] Plant extract microcapsules are a technology that uses microencapsulation technology to encapsulate the active ingredients of plant extracts in tiny carriers. Microcapsules are typically composed of a wall material (encapsulation material) and a core material (plant extract). The wall material is often a natural or synthetic polymer (such as gelatin, chitosan, liposomes, polylactic acid, etc.), forming tiny particles that protect the core material from external environmental influences.
[0003] Microencapsulation can protect active ingredients by preventing degradation caused by oxidation, light, high temperature, or acidic or alkaline environments; control release by achieving targeted or sustained release through wall material design, extending the duration of action; improve stability by addressing the volatility and storage difficulties of liquid extracts; improve applicability by masking bitter or pungent odors, facilitating processing into solid dosage forms (such as tablets and powders); and enhance bioavailability by promoting the absorption of ingredients into the body through nanoscale microcapsules. Microencapsulation has applications in specific areas such as cosmetics, food, medicine, and agriculture.
[0004] Anti-hair loss preparations are a type of functional product that reduces hair loss and promotes hair regeneration by regulating the scalp environment, activating hair follicle activity, or inhibiting hair loss-related mechanisms (such as hormones and inflammation). Plant extracts, due to their natural nature and low side effects, have become a key ingredient in anti-hair loss preparations. Their effects include: inhibiting hair loss-related pathways, inhibiting DHT production, improving androgenic alopecia, providing antioxidant benefits, inhibiting 5α-reductase activity, and reducing hair follicle atrophy; promoting hair growth, activating dermal papilla cells, promoting hair follicle proliferation and angiogenesis, and prolonging the anagen phase; improving the scalp environment, providing antibacterial and anti-inflammatory effects, alleviating seborrheic alopecia, promoting local blood circulation, and enhancing nutrient supply to hair follicles.
[0005] Compared with synthetic drugs (such as minoxidil, which may cause scalp irritation), plant ingredients are milder and suitable for long-term use; plant extracts often contain a variety of active ingredients (such as flavonoids, saponins, polysaccharides), which can simultaneously be anti-inflammatory, pro-circulatory, and anti-oxidant; the natural ingredients of plants are in line with the "clean beauty" trend and enhance the market acceptance of products.
[0006] Microencapsulating plant extracts into hair loss preparations is a hot research topic. This approach improves stability, inhibits degradation of active ingredients, and prolongs their activity through microencapsulation, such as liposomes. It also enhances permeability, promoting the passage of active ingredients across the scalp barrier. It also provides controlled release, targeting the hair follicle region, minimizing ingredient waste, and achieving high efficacy. However, developing microencapsulated composite plant extracts for use in hair loss prevention products to enhance their effectiveness remains a technical challenge. Summary of the Invention
[0007] In response to the above technical problems, the present invention provides a composite plant extract-encapsulated microcapsule, a preparation method thereof, and an application of the microcapsule in the preparation of an anti-hair loss and hair growth essential oil.
[0008] The present invention provides composite plant extract-encapsulated microcapsules, the raw materials of which include 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin, a plant extract, and ginger essential oil. The combination of 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin can significantly enhance the encapsulation effect of the microcapsules, increase their efficacy and sustained release, and enhance their effectiveness in preventing hair loss and promoting hair growth. The plant extract and ginger essential oil serve as active ingredients, enabling the microcapsules to effectively promote hair growth and prevent hair loss.
[0009] In a preferred embodiment, the composite plant extract encapsulates the microcapsules, and the raw materials include 5-10 parts of 2,6-dimethyl-β-cyclodextrin, 4-8 parts of γ-cyclodextrin, 0.8-2.5 parts of plant extract and 0.2-0.5 parts of ginger essential oil, in parts by weight.
[0010] In a preferred embodiment, the composite plant extract is encapsulated in microcapsules, and the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.6-0.8, which can obtain microcapsules with better preservation and sustained release effects, and give the microcapsules better drug efficacy.
[0011] In a preferred embodiment, the preparation method of the plant extract comprises: (1) crushing Platycladus orientalis leaves and Polygonum multiflorum, heating and mixing with water, and then cooling; (2) adding glucose and Listeria innocua ATCC33090 to obtain a fermentation material, fermenting to obtain a fermentation product, sterilizing, and concentrating; (3) adding ethanol to obtain a mixture, heating and extracting, filtering, concentrating the filtrate, and drying to obtain the plant extract.
[0012] In a preferred embodiment, the weight ratio of Platycladus orientalis leaves to Polygonum multiflorum is 1:0.8-1.5.
[0013] In a preferred embodiment, the weight ratio of the total weight of Platycladus orientalis leaves and Polygonum multiflorum to water is 1:10-30.
[0014] In a preferred embodiment, heating and mixing followed by cooling includes heating and boiling followed by cooling.
[0015] In a preferred embodiment, the temperature is cooled to 15-30°C.
[0016] In a preferred embodiment, the amount of glucose in the fermentation material is 1-4.4 wt%.
[0017] In a preferred embodiment, the amount of Listeria innocua ATCC33090 in the fermentation material is 10 10 to 10 13 pcs / g.
[0018] In a preferred embodiment, the fermentation temperature and time are 25-40° C. and 3-7 days.
[0019] In a preferred embodiment, the concentration comprises concentration under reduced pressure.
[0020] In a preferred embodiment, the weight of the concentrate in (2) is 1.5-5 times the total weight of Platycladus orientalis leaves and Polygonum multiflorum.
[0021] In a preferred embodiment, the concentration of ethanol in the mixture is 65-80 wt%.
[0022] In a preferred embodiment, the temperature and time of heating extraction are 40-60° C. and 3-10 hours.
[0023] In a preferred embodiment, the concentration in (3) is to a weight that is 0.1-0.25 times the weight of the filtrate.
[0024] The present invention also provides a method for preparing the composite plant extract-encapsulated microcapsules, comprising the following steps: heating and stirring 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water; adding plant extract and ginger essential oil, stirring, and then high-pressure homogenization, concentrating, and drying to obtain composite plant extract-encapsulated microcapsules.
[0025] In a preferred embodiment, the weight ratio of water to the total weight of 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:40-150.
[0026] In a preferred embodiment, the temperature and time of heating and stirring are 30-45° C. and 0.5-2 hours.
[0027] The present invention also provides the use of the composite plant extract-encapsulated microcapsules in the preparation of cosmetics or hair loss prevention and hair growth drugs.
[0028] The present invention also provides the use of the composite plant extract-encapsulated microcapsules in the preparation of anti-hair loss and hair growth essential oil.
[0029] Compared with the prior art, the present invention is progressive in that:
[0030] The present invention uses 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin, plant extracts and ginger essential oil to prepare encapsulated microcapsules; the combination of 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin can give the microcapsules a significantly improved coating effect, increase the efficacy and sustained release of the microcapsules, and enhance the anti-hair loss and hair promotion efficacy of the microcapsules; the plant extracts and ginger essential oil are used as active ingredients, so that the microcapsules can effectively promote hair growth and prevent hair loss.
[0031] The microcapsules prepared by the present invention can effectively inhibit the activity of type II 5α reductase and have the effect of preventing hair loss and promoting hair growth.
[0032] The plant extract produced by fermenting Listeria innocua ATCC33090 in this invention effectively enhances the microcapsule's ability to inhibit type II 5α-reductase enzyme activity. The use of this fermentation bacterium enriches the variety and concentration of active ingredients that inhibit type II 5α-reductase activity, imparting superior microcapsule efficacy. Compared to other bacteria, the Listeria innocua ATCC33090 employed in this invention exhibits superior effects in promoting hair growth and preventing hair loss. The specific selection of fermentation bacteria in this invention effectively enhances the efficacy of microcapsules.
[0033] The present invention adopts a high-concentration ethanol extraction method to effectively improve the microcapsule effect, and the effect is better when the ethanol extraction concentration is controlled at 65-80wt%.
[0034] The present invention utilizes 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin to synergistically enhance microcapsule stability and maintain the efficacy of the microcapsules in inhibiting type II 5-α-reductase activity. When the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.6-0.8, the microcapsule's efficacy is even better. DETAILED DESCRIPTION
[0035] The present invention demonstrates the technology of the present invention through specific implementation methods. Through the content of the specific implementation methods, the technical content of the present invention can be more clearly and completely understood.
[0036] The present invention provides composite plant extract-encapsulated microcapsules, the raw materials of which include 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin, plant extracts, and ginger essential oil. The combination of 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin can significantly enhance the encapsulation effect of the microcapsules, increase their efficacy and uniform release, and enhance their effectiveness in preventing hair loss and promoting hair growth. The plant extracts and ginger essential oil serve as active ingredients, enabling the microcapsules to effectively promote hair growth and prevent hair loss.
[0037] In a preferred embodiment, the composite plant extract encapsulates the microcapsules, and the raw materials include 5-10 parts of 2,6-dimethyl-β-cyclodextrin, 4-8 parts of γ-cyclodextrin, 0.8-2.5 parts of plant extract and 0.2-0.5 parts of ginger essential oil, in parts by weight.
[0038] In a preferred embodiment, the composite plant extract is encapsulated in microcapsules, and the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.6-0.8, which can obtain microcapsules with better preservation and uniform release effects, and give the microcapsules better drug efficacy.
[0039] In a preferred embodiment, the preparation method of the plant extract comprises: (1) crushing Platycladus orientalis leaves and Polygonum multiflorum, heating and mixing with water, and then cooling; (2) adding glucose and Listeria innocua ATCC33090 to obtain a fermentation material, fermenting to obtain a fermentation product, sterilizing, and concentrating; (3) adding ethanol to obtain a mixture, heating and extracting, filtering, concentrating the filtrate, and drying to obtain the plant extract.
[0040] In a preferred embodiment, the weight ratio of Platycladus orientalis leaves to Polygonum multiflorum is 1:0.8-1.5.
[0041] In a preferred embodiment, the weight ratio of the total weight of Platycladus orientalis leaves and Polygonum multiflorum to water is 1:10-30.
[0042] In a preferred embodiment, heating and mixing followed by cooling includes heating and boiling followed by cooling.
[0043] In a preferred embodiment, the temperature is cooled to 15-30°C.
[0044] In a preferred embodiment, the amount of glucose in the fermentation material is 1-4.4 wt%.
[0045] In a preferred embodiment, the amount of Listeria innocua ATCC33090 in the fermentation material is 10 10 to 10 13 pcs / g.
[0046] In a preferred embodiment, the fermentation temperature and time are 25-40° C. and 3-7 days.
[0047] In a preferred embodiment, the concentration comprises concentration under reduced pressure.
[0048] In a preferred embodiment, the weight of the concentrate in (2) is 1.5-5 times the total weight of Platycladus orientalis leaves and Polygonum multiflorum.
[0049] In a preferred embodiment, the concentration of ethanol in the mixture is 65-80 wt%.
[0050] In a preferred embodiment, the temperature and time of heating extraction are 40-60° C. and 3-10 hours.
[0051] In a preferred embodiment, the concentration in (3) is to a weight that is 0.1-0.25 times the weight of the filtrate.
[0052] The present invention also provides a method for preparing the composite plant extract-encapsulated microcapsules, comprising the following steps: heating and stirring 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water; adding plant extract and ginger essential oil, stirring, and then high-pressure homogenization, concentrating, and drying to obtain composite plant extract-encapsulated microcapsules.
[0053] In a preferred embodiment, the weight ratio of water to the total weight of 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:40-150.
[0054] In a preferred embodiment, the temperature and time of heating and stirring are 30-45° C. and 0.5-2 hours.
[0055] The present invention also provides the use of the composite plant extract-encapsulated microcapsules in the preparation of cosmetics or hair loss prevention and hair growth drugs.
[0056] The present invention also provides the use of the composite plant extract-encapsulated microcapsules in the preparation of anti-hair loss and hair growth essential oil.
[0057] Specific examples of the present invention are as follows.
[0058] 2,6-Dimethyl-β-cyclodextrin: Zibo Qianhui Biotechnology Co., Ltd. γ-cyclodextrin: Leshengyuan Biotechnology (Nanjing) Co., Ltd. Listeria innocua ATCC33090: Xinyang Laiyao Biotechnology Co., Ltd. Ginger essential oil: Wuhan Jiangxin Biotechnology Co., Ltd.
[0059] Preparation Example 1:
[0060] The preparation method is as follows: weigh the following raw materials in parts by weight: 8.0 parts of 2,6-dimethyl-β-cyclodextrin, 6.4 parts of γ-cyclodextrin, 2.0 parts of plant extract and 0.4 parts of ginger essential oil; the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.8;
[0061] The preparation method of the plant extract is as follows:
[0062] (1) Crush the Platycladus orientalis leaves and Polygonum multiflorum in a weight ratio of 1:1.2, then heat and boil with water in a weight ratio of the total weight of the Platycladus orientalis leaves and Polygonum multiflorum to water of 1:20, and then cool to 25°C;
[0063] (2) Glucose and Listeria innocua ATCC33090 were added to obtain a fermentation material (the amounts of glucose and Listeria innocua ATCC33090 in the fermentation material were 3.28 wt% and 5.5 × 10 12 / g), and aerobic fermentation was carried out at 30°C for 5 days (air flow rate 0.3L / (min·1L fermentation space)) to obtain a fermentation product, which was sterilized and concentrated under reduced pressure at 55°C to a weight twice the total weight of Platycladus orientalis leaves and Polygonum multiflorum;
[0064] (3) Add ethanol to obtain a mixture (the concentration of ethanol in the mixture is 70 wt%), heat at 50°C, stir at 60 rpm and extract for 5 hours, filter through a 0.22 μm filter membrane, concentrate the filtrate under reduced pressure at 50°C to a weight of 0.15 times the weight of the filtrate, and freeze-dry at -40°C to a water content of 1.27 wt% to obtain a plant extract.
[0065] 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water (the total weight ratio of water to 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:55) are heated at 35°C and stirred at 60 rpm for 0.6 hour; plant extract and ginger essential oil are added and stirred at 500 rpm for 0.6 hour, followed by high-pressure homogenization (pressure 100 MPa, 3 cycles, flow rate 30 L / min, homogenization temperature 35°C), concentrated under reduced pressure at 50°C to 16.7% by weight of the homogenate, and freeze-dried at -40°C to a water content of 2.13 wt% to obtain composite plant extract-encapsulated microcapsules.
[0066] Preparation Example 2:
[0067] The preparation method is as follows: weigh the following raw materials according to weight: 7.9 parts of 2,6-dimethyl-β-cyclodextrin, 4.8 parts of γ-cyclodextrin, 1.75 parts of plant extract and 0.45 parts of ginger essential oil; the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.61;
[0068] The preparation method of the plant extract is as follows:
[0069] (1) Crush Platycladus orientalis leaves and Polygonum multiflorum in a weight ratio of 1:0.8, then heat and boil with water in a weight ratio of the total weight of Platycladus orientalis leaves and Polygonum multiflorum to water of 1:22, and then cool to 25°C;
[0070] (2) Glucose and Listeria innocua ATCC33090 were added to obtain a fermentation material (the amounts of glucose and Listeria innocua ATCC33090 in the fermentation material were 3.05 wt% and 6×10 12 / g), and aerobic fermentation was carried out at 32°C for 4.5 days (air flow rate 0.3L / (min·1L fermentation space)) to obtain a fermentation product, which was sterilized and concentrated under reduced pressure at 55°C to a weight of 2.1 times the total weight of Platycladus orientalis leaves and Polygonum multiflorum;
[0071] (3) Add ethanol to obtain a mixture (the concentration of ethanol in the mixture is 80 wt%), heat at 50°C, stir at 60 rpm and extract for 5.5 hours, filter through a 0.22 μm filter membrane, concentrate the filtrate under reduced pressure at 50°C to a weight of 0.14 times the weight of the filtrate, and freeze-dry at -40°C to a water content of 1.21 wt%, to obtain a plant extract.
[0072] 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water (the total weight ratio of water to 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:50) are heated at 35°C and stirred at 60 rpm for 0.7 hour; plant extract and ginger essential oil are added and stirred at 400 rpm for 0.7 hour, followed by high-pressure homogenization (pressure 100 MPa, 3 cycles, flow rate 30 L / min, homogenization temperature 35°C), concentrated under reduced pressure at 50°C to 16.2% by weight of the homogenate, and freeze-dried at -40°C to a water content of 2.18 wt% to obtain composite plant extract-encapsulated microcapsules.
[0073] Preparation Example 3:
[0074] The preparation method is as follows: weigh the following raw materials in parts by weight: 14.4 parts of 2,6-dimethyl-β-cyclodextrin, 2.0 parts of plant extract and 0.4 parts of ginger essential oil; the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.8;
[0075] The preparation method of the plant extract is as follows:
[0076] (1) Crush the Platycladus orientalis leaves and Polygonum multiflorum in a weight ratio of 1:1.2, then heat and boil with water in a weight ratio of the total weight of the Platycladus orientalis leaves and Polygonum multiflorum to water of 1:20, and then cool to 25°C;
[0077] (2) Glucose and Listeria innocua ATCC33090 were added to obtain a fermentation material (the amounts of glucose and Listeria innocua ATCC33090 in the fermentation material were 3.28 wt% and 5.5 × 10 12 / g), and aerobic fermentation was carried out at 30°C for 5 days (air flow rate 0.3L / (min·1L fermentation space)) to obtain a fermentation product, which was sterilized and concentrated under reduced pressure at 55°C to a weight twice the total weight of Platycladus orientalis leaves and Polygonum multiflorum;
[0078] (3) Add ethanol to obtain a mixture (the concentration of ethanol in the mixture is 70 wt%), heat at 50°C, stir at 60 rpm and extract for 5 hours, filter through a 0.22 μm filter membrane, concentrate the filtrate under reduced pressure at 50°C to a weight of 0.15 times the weight of the filtrate, and freeze-dry at -40°C to a water content of 1.27 wt% to obtain a plant extract.
[0079] 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water (the total weight ratio of water to 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:55) are heated at 35°C and stirred at 60 rpm for 0.6 hour; plant extract and ginger essential oil are added and stirred at 500 rpm for 0.6 hour, followed by high-pressure homogenization (pressure 100 MPa, 3 cycles, flow rate 30 L / min, homogenization temperature 35°C), concentrated under reduced pressure at 50°C to 16.7% by weight of the homogenate, and freeze-dried at -40°C to a water content of 2.13 wt% to obtain composite plant extract-encapsulated microcapsules.
[0080] Preparation Example 4:
[0081] The preparation method is as follows: weigh the following raw materials according to weight: 14.4 parts of γ-cyclodextrin, 2.0 parts of plant extract and 0.4 parts of ginger essential oil; the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.8;
[0082] The preparation method of the plant extract is as follows:
[0083] (1) Crush the Platycladus orientalis leaves and Polygonum multiflorum in a weight ratio of 1:1.2, then heat and boil with water in a weight ratio of the total weight of the Platycladus orientalis leaves and Polygonum multiflorum to water of 1:20, and then cool to 25°C;
[0084] (2) Glucose and Listeria innocua ATCC33090 were added to obtain a fermentation material (the amounts of glucose and Listeria innocua ATCC33090 in the fermentation material were 3.28 wt% and 5.5 × 10 12 / g), and aerobic fermentation was carried out at 30°C for 5 days (air flow rate 0.3L / (min·1L fermentation space)) to obtain a fermentation product, which was sterilized and concentrated under reduced pressure at 55°C to a weight twice the total weight of Platycladus orientalis leaves and Polygonum multiflorum;
[0085] (3) Add ethanol to obtain a mixture (the concentration of ethanol in the mixture is 70 wt%), heat at 50°C, stir at 60 rpm and extract for 5 hours, filter through a 0.22 μm filter membrane, concentrate the filtrate under reduced pressure at 50°C to a weight of 0.15 times the weight of the filtrate, and freeze-dry at -40°C to a water content of 1.27 wt% to obtain a plant extract.
[0086] 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water (the total weight ratio of water to 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:55) are heated at 35°C and stirred at 60 rpm for 0.6 hour; plant extract and ginger essential oil are added and stirred at 500 rpm for 0.6 hour, followed by high-pressure homogenization (pressure 100 MPa, 3 cycles, flow rate 30 L / min, homogenization temperature 35°C), concentrated under reduced pressure at 50°C to 16.7% by weight of the homogenate, and freeze-dried at -40°C to a water content of 2.13 wt% to obtain composite plant extract-encapsulated microcapsules.
[0087] Preparation Example 5:
[0088] The preparation method is as follows: weigh the following raw materials according to weight: 12 parts of 2,6-dimethyl-β-cyclodextrin, 2.4 parts of γ-cyclodextrin, 2.0 parts of plant extract and 0.4 parts of ginger essential oil; the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.2;
[0089] The preparation method of the plant extract is as follows:
[0090] (1) Crush the Platycladus orientalis leaves and Polygonum multiflorum in a weight ratio of 1:1.2, then heat and boil with water in a weight ratio of the total weight of the Platycladus orientalis leaves and Polygonum multiflorum to water of 1:20, and then cool to 25°C;
[0091] (2) Glucose and Listeria innocua ATCC33090 were added to obtain a fermentation material (the amounts of glucose and Listeria innocua ATCC33090 in the fermentation material were 3.28 wt% and 5.5 × 10 12 / g), and aerobic fermentation was carried out at 30°C for 5 days (air flow rate 0.3L / (min·1L fermentation space)) to obtain a fermentation product, which was sterilized and concentrated under reduced pressure at 55°C to a weight twice the total weight of Platycladus orientalis leaves and Polygonum multiflorum;
[0092] (3) Add ethanol to obtain a mixture (the concentration of ethanol in the mixture is 70 wt%), heat at 50°C, stir at 60 rpm and extract for 5 hours, filter through a 0.22 μm filter membrane, concentrate the filtrate under reduced pressure at 50°C to a weight of 0.15 times the weight of the filtrate, and freeze-dry at -40°C to a water content of 1.27 wt% to obtain a plant extract.
[0093] 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water (the total weight ratio of water to 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:55) are heated at 35°C and stirred at 60 rpm for 0.6 hour; plant extract and ginger essential oil are added and stirred at 500 rpm for 0.6 hour, followed by high-pressure homogenization (pressure 100 MPa, 3 cycles, flow rate 30 L / min, homogenization temperature 35°C), concentrated under reduced pressure at 50°C to 16.7% by weight of the homogenate, and freeze-dried at -40°C to a water content of 2.13 wt% to obtain composite plant extract-encapsulated microcapsules.
[0094] Preparation Example 6:
[0095] The preparation method is as follows: weigh the following raw materials according to weight: 3.6 parts of 2,6-dimethyl-β-cyclodextrin, 10.8 parts of γ-cyclodextrin, 2.0 parts of plant extract and 0.4 parts of ginger essential oil; the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:3;
[0096] The preparation method of the plant extract is as follows:
[0097] (1) Crush the Platycladus orientalis leaves and Polygonum multiflorum in a weight ratio of 1:1.2, then heat and boil with water in a weight ratio of the total weight of the Platycladus orientalis leaves and Polygonum multiflorum to water of 1:20, and then cool to 25°C;
[0098] (2) Glucose and Listeria innocua ATCC33090 were added to obtain a fermentation material (the amounts of glucose and Listeria innocua ATCC33090 in the fermentation material were 3.28 wt% and 5.5 × 10 12 / g), and aerobic fermentation was carried out at 30°C for 5 days (air flow rate 0.3L / (min·1L fermentation space)) to obtain a fermentation product, which was sterilized and concentrated under reduced pressure at 55°C to a weight twice the total weight of Platycladus orientalis leaves and Polygonum multiflorum;
[0099] (3) Add ethanol to obtain a mixture (the concentration of ethanol in the mixture is 70 wt%), heat at 50°C, stir at 60 rpm and extract for 5 hours, filter through a 0.22 μm filter membrane, concentrate the filtrate under reduced pressure at 50°C to a weight of 0.15 times the weight of the filtrate, and freeze-dry at -40°C to a water content of 1.27 wt% to obtain a plant extract.
[0100] 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water (the total weight ratio of water to 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:55) are heated at 35°C and stirred at 60 rpm for 0.6 hour; plant extract and ginger essential oil are added and stirred at 500 rpm for 0.6 hour, followed by high-pressure homogenization (pressure 100 MPa, 3 cycles, flow rate 30 L / min, homogenization temperature 35°C), concentrated under reduced pressure at 50°C to 16.7% by weight of the homogenate, and freeze-dried at -40°C to a water content of 2.13 wt% to obtain composite plant extract-encapsulated microcapsules.
[0101] Preparation Example 7:
[0102] The preparation method is as follows: weigh the following raw materials in parts by weight: 8.0 parts of 2,6-dimethyl-β-cyclodextrin, 6.4 parts of γ-cyclodextrin, 2.0 parts of plant extract and 0.4 parts of ginger essential oil; the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.8;
[0103] The preparation method of the plant extract is as follows:
[0104] (1) Crush the Platycladus orientalis leaves and Polygonum multiflorum in a weight ratio of 1:1.2, then heat and boil with water in a weight ratio of the total weight of the Platycladus orientalis leaves and Polygonum multiflorum to water of 1:20, and then cool to 25°C;
[0105] (2) The cooled material was concentrated under reduced pressure at 55°C to a weight twice the total weight of Platycladus orientalis leaves and Polygonum multiflorum;
[0106] (3) Add ethanol to obtain a mixture (the concentration of ethanol in the mixture is 70 wt%), heat at 50°C, stir at 60 rpm and extract for 5 hours, filter through a 0.22 μm filter membrane, concentrate the filtrate under reduced pressure at 50°C to a weight of 0.15 times the weight of the filtrate, and freeze-dry at -40°C to a water content of 1.27 wt% to obtain a plant extract.
[0107] 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water (the total weight ratio of water to 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:55) are heated at 35°C and stirred at 60 rpm for 0.6 hour; plant extract and ginger essential oil are added and stirred at 500 rpm for 0.6 hour, followed by high-pressure homogenization (pressure 100 MPa, 3 cycles, flow rate 30 L / min, homogenization temperature 35°C), concentrated under reduced pressure at 50°C to 16.7% by weight of the homogenate, and freeze-dried at -40°C to a water content of 2.13 wt% to obtain composite plant extract-encapsulated microcapsules.
[0108] Preparation Example 8:
[0109] The preparation method is as follows: weigh the following raw materials in parts by weight: 8.0 parts of 2,6-dimethyl-β-cyclodextrin, 6.4 parts of γ-cyclodextrin, 2.0 parts of plant extract and 0.4 parts of ginger essential oil; the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.8;
[0110] The preparation method of the plant extract is as follows:
[0111] (1) Crush the Platycladus orientalis leaves and Polygonum multiflorum in a weight ratio of 1:1.2, then heat and boil with water in a weight ratio of the total weight of the Platycladus orientalis leaves and Polygonum multiflorum to water of 1:20, and then cool to 25°C;
[0112] (2) Glucose and Bacillus subtilis CICC 10262 were added to obtain a fermentation material (the amount of glucose and Bacillus subtilis in the fermentation material was 3.28 wt% and 5.5 × 10 12 / g), and aerobic fermentation was carried out at 30°C for 5 days (air flow rate 0.3L / (min·1L fermentation space)) to obtain a fermentation product, which was sterilized and concentrated under reduced pressure at 55°C to a weight twice the total weight of Platycladus orientalis leaves and Polygonum multiflorum;
[0113] (3) Add ethanol to obtain a mixture (the concentration of ethanol in the mixture is 70 wt%), heat at 50°C, stir at 60 rpm and extract for 5 hours, filter through a 0.22 μm filter membrane, concentrate the filtrate under reduced pressure at 50°C to a weight of 0.15 times the weight of the filtrate, and freeze-dry at -40°C to a water content of 1.27 wt% to obtain a plant extract.
[0114] 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water (the total weight ratio of water to 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:55) are heated at 35°C and stirred at 60 rpm for 0.6 hour; plant extract and ginger essential oil are added and stirred at 500 rpm for 0.6 hour, followed by high-pressure homogenization (pressure 100 MPa, 3 cycles, flow rate 30 L / min, homogenization temperature 35°C), concentrated under reduced pressure at 50°C to 16.7% by weight of the homogenate, and freeze-dried at -40°C to a water content of 2.13 wt% to obtain composite plant extract-encapsulated microcapsules.
[0115] Preparation Example 9:
[0116] The preparation method is as follows: weigh the following raw materials in parts by weight: 8.0 parts of 2,6-dimethyl-β-cyclodextrin, 6.4 parts of γ-cyclodextrin, 2.0 parts of plant extract and 0.4 parts of ginger essential oil; the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.8;
[0117] The preparation method of the plant extract is as follows:
[0118] (1) Crush the Platycladus orientalis leaves and Polygonum multiflorum in a weight ratio of 1:1.2, then heat and boil with water in a weight ratio of the total weight of the Platycladus orientalis leaves and Polygonum multiflorum to water of 1:20, and then cool to 25°C;
[0119] (2) Glucose and acetic acid bacteria SHBCC D11405 were added to obtain fermentation material (the amount of glucose and acetic acid bacteria in the fermentation material was 3.28 wt% and 5.5 × 10 12 / g), and aerobic fermentation was carried out at 30°C for 5 days (air flow rate 0.3L / (min·1L fermentation space)) to obtain a fermentation product, which was sterilized and concentrated under reduced pressure at 55°C to a weight twice the total weight of Platycladus orientalis leaves and Polygonum multiflorum;
[0120] (3) Add ethanol to obtain a mixture (the concentration of ethanol in the mixture is 70 wt%), heat at 50°C, stir at 60 rpm and extract for 5 hours, filter through a 0.22 μm filter membrane, concentrate the filtrate under reduced pressure at 50°C to a weight of 0.15 times the weight of the filtrate, and freeze-dry at -40°C to a water content of 1.27 wt% to obtain a plant extract.
[0121] 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water (the total weight ratio of water to 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:55) are heated at 35°C and stirred at 60 rpm for 0.6 hour; plant extract and ginger essential oil are added and stirred at 500 rpm for 0.6 hour, followed by high-pressure homogenization (pressure 100 MPa, 3 cycles, flow rate 30 L / min, homogenization temperature 35°C), concentrated under reduced pressure at 50°C to 16.7% by weight of the homogenate, and freeze-dried at -40°C to a water content of 2.13 wt% to obtain composite plant extract-encapsulated microcapsules.
[0122] Preparation Example 10:
[0123] The preparation method is as follows: weigh the following raw materials in parts by weight: 8.0 parts of 2,6-dimethyl-β-cyclodextrin, 6.4 parts of γ-cyclodextrin, 2.0 parts of plant extract and 0.4 parts of ginger essential oil; the weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.8;
[0124] The preparation method of the plant extract is as follows:
[0125] (1) Crush the Platycladus orientalis leaves and Polygonum multiflorum in a weight ratio of 1:1.2, then heat and boil with water in a weight ratio of the total weight of the Platycladus orientalis leaves and Polygonum multiflorum to water of 1:20, and then cool to 25°C;
[0126] (2) Glucose and Listeria innocua ATCC33090 were added to obtain a fermentation material (the amounts of glucose and Listeria innocua ATCC33090 in the fermentation material were 3.28 wt% and 5.5 × 1012 / g), and aerobic fermentation was carried out at 30°C for 5 days (air flow rate 0.3L / (min·1L fermentation space)) to obtain a fermentation product, which was sterilized and concentrated under reduced pressure at 55°C to a weight twice the total weight of Platycladus orientalis leaves and Polygonum multiflorum;
[0127] (3) Add ethanol to obtain a mixture (the concentration of ethanol in the mixture is 35 wt%), heat at 50°C, stir at 60 rpm and extract for 5 hours, filter through a 0.22 μm filter membrane, concentrate the filtrate under reduced pressure at 50°C to a weight of 0.15 times the weight of the filtrate, and freeze-dry at -40°C to a water content of 1.27 wt% to obtain a plant extract.
[0128] 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water (the total weight ratio of water to 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:55) are heated at 35°C and stirred at 60 rpm for 0.6 hour; plant extract and ginger essential oil are added and stirred at 500 rpm for 0.6 hour, followed by high-pressure homogenization (pressure 100 MPa, 3 cycles, flow rate 30 L / min, homogenization temperature 35°C), concentrated under reduced pressure at 50°C to 16.7% by weight of the homogenate, and freeze-dried at -40°C to a water content of 2.13 wt% to obtain composite plant extract-encapsulated microcapsules.
[0129] Test: Anti-hair loss test
[0130] Type II 5α-reductase is directly involved in the pathological process of androgenic alopecia and hair follicle atrophy by regulating the production of DHT. Inhibiting the activity of type II 5α-reductase can inhibit hair loss and promote hair growth.
[0131] The product of the above preparation example was mixed with 25 wt % ethanol aqueous solution at a weight ratio of 2:48 at 30° C. and 100 rpm, stirred for 0.3 hour, and sterilized to obtain a sample.
[0132] 5 mL of deionized water, 2 μL of a 1 mmol / L testosterone solution, 600 μL of a 10 mg / mL rat steroid 5α-reductase SRD5A2 (type II 5α-reductase) solution, and 200 μL of a 1 mmol / L NADPH solution were mixed to obtain an enzyme solution. The enzyme solution was incubated at 37°C in a 5% CO2 environment for 40 minutes. 0.5 mL of the sample was added to the total amount of the enzyme solution and mixed to obtain a test solution, which was incubated at 37°C in a 5% CO2 environment for 40 minutes. The absorbance of the enzyme solution before and after incubation and the absorbance of the test solution before and after incubation at 340 nm were then measured using a UV-visible spectrophotometer. The decrease in absorbance of the test solution before and after incubation for different samples was calculated, recorded as ΔAn (where n is 1-10, corresponding to the sample numbers of Preparation Examples 1-10), and the decrease in absorbance of the enzyme solution before and after incubation was calculated, recorded as ΔA0. The type II 5α-reductase activity inhibition rate for each group was calculated according to the following formula: / % = 100% × (ΔA0 - ΔAn) ÷ ΔA0. The α value of the type II 5α-reductase activity inhibition rate for each group compared to the product of Preparation Example 1 was also calculated. The results are shown in Table 1.
[0133] Table 1: Inhibition rate of type II 5α-reductase enzyme activity
[0134]
[0135] Combined with the test results in Table 1, it can be seen that the microcapsules prepared by the present invention can effectively inhibit the activity of type II 5α reductase and have the effect of preventing hair loss and promoting hair growth.
[0136] Combining the test results of Preparation Example 1 and Preparation Example 7, it can be concluded that the plant extract prepared by fermentation of Listeria innocua ATCC33090 in the present invention can effectively enhance the microcapsule's activity in inhibiting type II 5α-reductase. The use of this fermentation bacteria can enrich the types and concentrations of active ingredients that inhibit type II 5α-reductase activity, giving the microcapsule an excellent effect.
[0137] Combined with the test results of Preparation Examples 1 and 8-9, it can be concluded that the Listeria innocua ATCC33090 used in the present invention has a better effect in promoting hair growth and preventing hair loss than other bacteria. The selection of specific fermentation bacteria in the present invention can effectively improve the efficiency of microcapsules.
[0138] Combined with the test results of Preparation Examples 1 and 10, it can be seen that the high-concentration ethanol extraction method of the present invention can effectively improve the microcapsule effect, and the effect is better when the concentration is controlled at 65-80wt%.
[0139] To investigate the effects of 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin on the preservation of microcapsules, the products obtained in Preparation Examples 1 and 3-6 were stored at 35°C for 3 months and then tested for inhibition of type II 5α-reductase activity using the same method described above. The results are shown in Table 1. The retention rate (β) of the inhibition rate of type II 5α-reductase activity after 3 months of storage compared to the unstored state was then calculated. The results are shown in Table 2.
[0140] Table 2: 3-month inhibition rate and β value of type II 5α-reductase enzyme activity
[0141]
[0142]
[0143] From the test results in Table 2, it can be seen that the microcapsules prepared by the present invention have high stability, and the active ingredient efficiency retention rate reaches 96.47% after being placed at 35°C for 3 months.
[0144] Combined with the comparison of Preparation Examples 1 and 3-4, it can be seen that when only one of 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is used to coat and prepare microcapsules, the active ingredient maintenance efficiency of the obtained microcapsules is low and the maximum efficacy cannot be exerted. 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin can synergistically enhance the stability of the microcapsules and synergistically enhance the effect of the microcapsules on the efficacy of the type II 5α reductase activity inhibition rate. According to the comparison of Preparation Examples 1 and 5-6, when the weight ratio of 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:0.6-0.8, the efficacy retention effect of the microcapsules is better.
Claims
1. A composite plant extract-encapsulated microcapsule, characterized in that: The raw materials include 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin, plant extracts and ginger essential oil.
2. The composite plant extract-encapsulated microcapsule according to claim 1, characterized in that: In parts by weight, the raw materials include 5-10 parts of 2,6-dimethyl-β-cyclodextrin, 4-8 parts of γ-cyclodextrin, 0.8-2.5 parts of plant extract and 0.2-0.5 parts of ginger essential oil.
3. The composite plant extract-encapsulated microcapsule according to claim 1, characterized in that: The weight ratio of 2,6-dimethyl-β-cyclodextrin to γ-cyclodextrin is 1:0.6-0.
8.
4. The composite plant extract-encapsulated microcapsule according to claim 1, characterized in that: The preparation method of the plant extract comprises the following steps: (1) crushing Platycladus orientalis leaves and Polygonum multiflorum, heating and mixing with water, and then cooling; (2) adding glucose and Listeria innocua ATCC33090 to obtain a fermentation material, fermenting to obtain a fermentation product, sterilizing, and concentrating; (3) adding ethanol to obtain a mixture, heating and extracting, filtering, concentrating the filtrate, and drying to obtain the plant extract.
5. The composite plant extract-encapsulated microcapsule according to claim 4, characterized in that: The weight ratio of Platycladus orientalis leaves to Polygonum multiflorum is 1:0.8-1.5; Or, the dosage of Listeria innocua ATCC33090 in the fermentation material is 10 10 to 10 13 pcs / g.
6. The composite plant extract-encapsulated microcapsule according to claim 4, characterized in that: The fermentation temperature and time are 25-40℃, 3-7 days; Alternatively, the concentration of ethanol in the mixture is 65-80 wt %; Alternatively, the temperature and time of heating extraction are 40-60° C. and 3-10 hours.
7. A method for preparing microcapsules encapsulated with a composite plant extract according to any one of claims 1 to 6, characterized in that: The method comprises the following steps: heating and stirring 2,6-dimethyl-β-cyclodextrin, γ-cyclodextrin and water; adding plant extract and ginger essential oil, stirring, and then high-pressure homogenizing, concentrating, and drying to obtain composite plant extract-wrapped microcapsules.
8. The preparation method according to claim 7, characterized in that The weight ratio of water to the total weight of 2,6-dimethyl-β-cyclodextrin and γ-cyclodextrin is 1:40-150.
9. Use of the composite plant extract-encapsulated microcapsules according to any one of claims 1 to 6 in the preparation of cosmetics or anti-hair loss and hair growth drugs.
10. Use of the composite plant extract-encapsulated microcapsules according to any one of claims 1 to 6 in the preparation of an anti-hair loss and hair growth essential oil.
Citation Information
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