WO2022199510A1 - 一种舒缓修护组合物及其制备方法和应用 - Google Patents

一种舒缓修护组合物及其制备方法和应用 Download PDF

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WO2022199510A1
WO2022199510A1 PCT/CN2022/081927 CN2022081927W WO2022199510A1 WO 2022199510 A1 WO2022199510 A1 WO 2022199510A1 CN 2022081927 W CN2022081927 W CN 2022081927W WO 2022199510 A1 WO2022199510 A1 WO 2022199510A1
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soothing
preparation
skin
parts
repairing composition
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PCT/CN2022/081927
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English (en)
French (fr)
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孟宏
曲召辉
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太和康美(北京)中医研究院有限公司
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Priority to KR1020237034944A priority Critical patent/KR20230149856A/ko
Publication of WO2022199510A1 publication Critical patent/WO2022199510A1/zh

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9794—Liliopsida [monocotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005—Antimicrobial preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/005—Preparations for sensitive skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/08—Anti-ageing preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52—Stabilizers
    • A61K2800/522—Antioxidants; Radical scavengers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59—Mixtures
    • A61K2800/592—Mixtures of compounds complementing their respective functions
    • A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/74—Biological properties of particular ingredients
    • A61K2800/75—Anti-irritant
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

Definitions

  • the invention relates to the field of plant extraction research, in particular to a soothing and repairing composition and a preparation method and application thereof.
  • Patent (CN112137932A) discloses an anti-allergic repair composition, which is composed of Kochia kochia (KOCHIA SCOPARIA) extract, chamomile (CHAMOMILLA RECUTITA) flower extract, Salvia miltiorrhiza (SALVIA MILTIORRHIZA) root extract, purslane (PORTULACA OLERACEA) Extract, Kava (PIPER METHYSTICUM) leaf/root/stem extract composition.
  • the composition only relieves the symptoms of problem skin from the perspective of soothing redness, dry itching, burning, stinging and the like.
  • the main purpose of the present invention is to provide a soothing and repairing composition and a preparation method thereof.
  • the composition acts through the interaction of various components and acts in multiple ways, so as to solve the problems induced by various factors such as environment, region, staying up late, stress and changing seasons. skin problems.
  • the soothing and repairing composition of the invention has the functions of instantly soothing skin redness, itching and stinging, scavenging free radicals, anti-inflammatory, improving skin tolerance, repairing skin barrier and the like.
  • a first aspect of the present invention provides a soothing and repairing composition.
  • the soothing and repairing composition comprises the following components in parts by weight: 5-40 parts of purslane, 1-30 parts of Kochia, 5-20 parts of duckweed, 1-20 parts of honeysuckle, ebony 3-15 servings, Nepeta 1-10 servings.
  • the soothing and repairing composition is prepared by a preparation method comprising the following steps:
  • step (3) coarse filtrate is finely filtered to obtain filtrate
  • the weight ratio of the total weight of raw materials to water in step (2) of the preparation method is 1:15-1:70 (m/m) (based on the dry weight of raw materials).
  • the weight ratio of the total weight of the raw materials to the water can be 1:15 (m/m), 1:16 (m/m), 1:17 (m/m), 1:18(m/m), 1:19(m/m), 1:20(m/m), 1:25(m/m), 1:30(m/m), 1:35(m /m), 1:40(m/m), 1:45(m/m), 1:50(m/m), 1:55(m/m), 1:60(m/m), 1:65(m/m), 1:70(m/m).
  • the weight ratio of the total weight of the raw materials to the water is 1:20-1:50 (m/m) (based on the dry weight of the raw materials).
  • the extraction temperature in step (2) of the preparation method is 100-130°C.
  • the extraction temperature in step (2) of the preparation method is 110°C.
  • the extraction pressure in step (2) of the preparation method is 0.1-0.3 MPa.
  • the extraction pressure in step (2) of the preparation method is 0.15 MPa.
  • the extraction time in step (2) of the preparation method is 1-3h.
  • the extraction time in step (2) of the preparation method is 1.5h.
  • the filter cloth in step (3) of the preparation method is 60-100 mesh.
  • step (3) of the preparation method the medicinal residues are filtered out by coarse filtration.
  • the fine filtration method in step (4) of the preparation method is plate and frame filtration.
  • the pore size of the filter plate of the fine filter plate frame is 0.3-0.5 ⁇ m.
  • the filter plate of the fine filter plate frame is SCP-1120 type.
  • the sterilization method in step (5) of the preparation method is a conventional sterilization method.
  • the sterilization method in step (5) of the preparation method is high temperature sterilization.
  • the sterilization temperature in step (5) of the preparation method is 90-95°C.
  • the sterilization time in step (5) of the preparation method is 30-60 min.
  • step (5) of the preparation method further includes adding a preservative.
  • the preservatives added in step (5) of the preparation method are pentanediol and hexanediol.
  • step (5) of the preparation method based on the weight of the filtrate, the addition amount of pentanediol is 1-5 wt %, and the addition amount of hexanediol is 0.5-2 wt %.
  • the pretreatment of raw materials in step (1) of the preparation method includes picking out foreign objects and cleaning.
  • the second aspect of the present invention provides a preparation method of the soothing and repairing composition of the first aspect of the present invention.
  • the preparation method of the soothing and repairing composition comprises the following steps:
  • step (3) filtering the extract in step (2) with a 60-100 mesh filter cloth to obtain a coarse filtrate
  • step (3) finely filter the crude filtrate in step (3) with a plate-and-frame filtration method, and the filter plate aperture is 0.3-0.5 ⁇ m to obtain a filtrate;
  • the weight ratio of the total weight of the raw materials to the water can be 1:15 (m/m), 1:16 (m/m), 1:17 (m/m), 1:18(m/m), 1:19(m/m), 1:20(m/m), 1:25(m/m), 1:30(m/m), 1:35(m /m), 1:40(m/m), 1:45(m/m), 1:50(m/m), 1:55(m/m), 1:60(m/m), 1:65(m/m), 1:70(m/m).
  • the weight ratio of the total weight of the raw materials to the water is 1:20-1:50 (m/m) (based on the dry weight of the raw materials).
  • the extraction temperature in step (2) of the preparation method is 110°C.
  • the extraction pressure in step (2) of the preparation method is 0.15 MPa.
  • the extraction time in step (2) of the preparation method is 1.5h.
  • step (3) of the preparation method the medicinal residues are filtered out by coarse filtration.
  • the fine filtration method in step (4) of the preparation method is plate and frame filtration.
  • the filter plate of the fine filter plate frame is SCP-1120 type.
  • the sterilization method in step (5) of the preparation method is a conventional sterilization method.
  • the sterilization method in step (5) of the preparation method is high temperature sterilization.
  • the sterilization temperature in step (5) of the preparation method is 90-95°C.
  • the sterilization time in step (5) of the preparation method is 30-60 min.
  • step (5) of the preparation method further includes adding a preservative.
  • the preservatives added in step (5) of the preparation method are pentanediol and hexanediol.
  • step (5) of the preparation method based on the weight of the filtrate, the addition amount of pentanediol is 1-5 wt %, and the addition amount of hexanediol is 0.5-2 wt %.
  • the pretreatment of raw materials in step (1) of the preparation method includes picking out foreign objects and cleaning.
  • the third aspect of the present invention provides the soothing and repairing composition of the first aspect of the present invention and/or the soothing and repairing composition prepared by the preparation method of the soothing and repairing composition of the second aspect of the present invention in cosmetics and/or Application in the field of skin care products.
  • the skin care product is a facial mask, cream, lotion, skin care lotion, facial cleanser, shampoo, conditioner or shower gel, etc., and is not limited by the dosage form.
  • the soothing and repairing composition of the present invention contains six functional components of purslane, kochia, duckweed, honeysuckle, ebony, and nepeta, and has a multi-channel synergistic effect.
  • Anti-inflammatory, antibacterial, repairing skin barrier, improving skin tolerance” and other functions solve skin problems caused by various factors such as environment, region, staying up late, stress and changing seasons, such as sensitive skin.
  • the present invention adopts a high temperature and high pressure extraction process, which improves the total sugar content, total flavonoid content and polyphenol content of the functional components in the soothing and repairing composition, promotes the expression of the functional components, accelerates the reaction process, improves the utilization rate of raw materials, and saves production costs.
  • Fig. 1 is capsaicin stimulation experiment result figure
  • Fig. 2 is embodiment 1, embodiment 7, comparative example 3-comparative example 11 itching sensation score chart after lactic acid stimulation;
  • Fig. 3 is embodiment 1, embodiment 7, comparative example 3-comparative example 11 tingling sensation score chart after lactic acid stimulation;
  • Fig. 4 is embodiment 1, embodiment 7, comparative example 19-comparative example 20 tingling sensation score after stimulation with lactic acid;
  • Fig. 5 is embodiment 1, embodiment 7, comparative example 19-comparative example 20 itching sensation score chart after lactic acid stimulation;
  • Figure 6 is a graph of the free radical scavenging rate of ABTS.
  • the sources of the raw materials used in the present invention are shown in Table 1. Unless otherwise specified, the raw materials and instruments used in the present invention are conventional raw materials or instruments.
  • raw material name Supplier/Manufacturer Origin purslane Beijing Qiancao Chinese Herbal Pieces Co., Ltd. Hebei Kochia Beijing Qiancao Chinese Herbal Pieces Co., Ltd. Hebei duckweed Tongrentang Hebei honeysuckle Beijing Qiancao Chinese Herbal Pieces Co., Ltd. Hebei Ume Beijing Qiancao Chinese Herbal Pieces Co., Ltd. Sichuan Nepeta Tongrentang Hebei Hexylene glycol Dezhixin Germany Pentylene glycol Dezhixin Germany
  • Embodiment 1 Weigh 30g of purslane, 20g of Kochia kohlrabi, 15g of duckweed, 10g of honeysuckle, 10g of black plum, 5g of Nepeta; add 4500g of deionized water according to the ratio of material to liquid 1:50 (m/m); at 110 °C, extract under 0.15MPa for 1.5h; first filter the extract with 100 mesh filter cloth, then filter with 0.3-0.5 ⁇ m filter plate; Sterilize at 95°C for 30 minutes to obtain the composition.
  • Embodiment 2 Weigh 5g of purslane, 1g of Kochia kohlrabi, 5g of duckweed, 1g of honeysuckle, 3g of black plum, 1g of Nepeta; add 1120g of deionized water according to the material-to-liquid ratio 1:70 (m/m); °C, extract under 0.1MPa for 1.5h; first filter the extract with 100 mesh filter cloth, then filter with 0.3-0.5 ⁇ m filter plate; add 2% pentanediol, 1.5% hexanediol for anticorrosion, water bath 90- Sterilize at 95°C for 30 minutes to obtain the composition.
  • Embodiment 3 Weigh 40g of purslane, 30g of Kochia kohlrabi, 20g of duckweed, 20g of honeysuckle, 15g of black plum, 10g of Nepeta; add 2700g of deionized water according to the ratio of material to liquid 1:20 (m/m); at 130 °C, extract under 0.3MPa for 1.5h; first filter the extract with 100 mesh filter cloth, then filter with 0.3-0.5 ⁇ m filter plate; add 2% pentanediol, 1.5% hexanediol for anticorrosion, water bath 90- Sterilize at 95°C for 30 minutes to obtain the composition.
  • Embodiment 4 Weigh 30g of purslane, 20g of Kochia kohlrabi, 15g of duckweed, 10g of honeysuckle, 10g of black plum, 5g of Nepeta; add 1800g of deionized water according to the ratio of material to liquid 1:20 (m/m); at 110 °C, extract under 0.15MPa for 1.5h; first filter the extract with 100 mesh filter cloth, then filter with 0.3-0.5 ⁇ m filter plate; add 2% pentanediol, 1.5% hexanediol for anticorrosion, water bath 90- Sterilize at 95°C for 30 minutes to obtain the composition.
  • Example 5 Weigh 30g of purslane, 20g of Kochia kohlrabi, 15g of duckweed, 10g of honeysuckle, 10g of black plum, 5g of Nepeta; add 4500g of deionized water according to the ratio of material to liquid 1:50 (m/m); 100° C. , extract under 0.1MPa for 1.5h; first filter the extract with 100 mesh filter cloth, then filter with 0.3-0.5 ⁇ m filter plate; add 2% pentanediol, 1.5% hexanediol for corrosion protection, water bath 90- Sterilize at 95°C for 30 minutes to obtain the composition.
  • Embodiment 6 Weigh 30g of purslane, 20g of Kochia kohlrabi, 15g of duckweed, 10g of honeysuckle, 10g of black plum, 5g of Nepeta; add 1800g of deionized water according to the ratio of material to liquid 1:20 (m/m); at 130 °C, extract under 0.3MPa for 1.5h; first filter the extract with 100 mesh filter cloth, then filter with 0.3-0.5 ⁇ m filter plate; add 2% pentanediol, 1.5% hexanediol for anticorrosion, water bath 90- Sterilize at 95°C for 30 minutes to obtain the composition.
  • Embodiment 7 Weigh 20g of purslane, 20g of Kochia kohlrabi, 15g of duckweed, 10g of honeysuckle, 5g of black plum, 5g of Nepeta; add 3750g of deionized water according to the ratio of material to liquid 1:50 (m/m); at 110 °C, extract under 0.15MPa for 1.5h; first filter the extract with 100 mesh filter cloth, then filter with 0.3-0.5 ⁇ m filter plate; add 2% pentanediol, 1.5% hexanediol for anticorrosion, water bath 90- Sterilize at 95°C for 30 minutes to obtain the composition.
  • the extracts of Comparative Examples 3-11 were prepared according to the raw materials and processes in Table 2 respectively; then the extract was filtered once with a 100-mesh filter cloth, and then filtered with a 0.3-0.5 ⁇ m filter plate; 2% pentanediol, 1.5% hexanediol were added Alcohol preservation, water bath sterilization at 90-95 DEG C for 30 min, to obtain the composition.
  • Test Example 1 Basic Index Test of Plant Compositions with Different Preparation Processes
  • Solid content measured with a solid content meter.
  • each index was measured in the filtrate before concentration.
  • the high temperature and high pressure method is a method of extracting active ingredients under high-pressure airtight conditions. This extraction method can accelerate the reaction during the reaction. At the same time, the airtight conditions can also make the water vapor fully contact each medicinal material and improve the reaction efficiency. As can be seen from Table 4, compared with the common water extraction method, the high temperature and high pressure method increases the total sugar content, total flavonoid content and polyphenol content of the composition, avoids resource waste due to insufficient utilization of raw materials, and greatly saves costs.
  • Example 1 comparing Example 1, Examples 5-6 and Comparative Example 2, it can be found that when the temperature and pressure of the high temperature and high pressure treatment exceed a certain range, the higher temperature and pressure basically no longer improve the extraction efficiency of the plant, but Excessive pressure not only brings security risks, but also increases energy consumption and wastes energy.
  • the high temperature and high pressure extraction conditions of the present invention are that the extraction pressure is 0.1-0.3MPa, and the extraction temperature is 100°C-130°C.
  • Double decoction is to cook all the medicinal materials in a pot at the same time.
  • Single decoction is to cook each herb separately, and then mix the medicinal soup.
  • Table 5 the relevant index data of Example 1 and Comparative Examples 12-17 are tested, and the results are as shown in Table 5.
  • the color of the solution in Example 1 is similar to it and has a higher solid content, indicating that a certain weak interaction occurs between the medicinal material and the medicinal material during re-decocting, resulting in a supramolecular chemical phenomenon, which promotes the dissolution of the functional ingredients. in the extract. Because the ebony extract is prone to irritation to the skin due to its low pH value (2.62), the ebony extract was discarded in the later experiments.
  • Test samples Example 1, Comparative Examples 12-18
  • Test site left and right arm inner side
  • the inner sides of the left and right arms of the subjects were selected as the test parts, and a square area with a size of 2cm ⁇ 2cm was used for circular marking; Sit for 10 minutes under the condition of 43-52%, measure the blank value of skin red value with Mexamter MX18 (pigment test probe) from CK Company in Germany, and then enter the smearing experiment stage; use 0.02% capsaicin aqueous solution (about 0.01mL) Stimulate the test area; after continuous stimulation for 15min and 30min, carry out numerical collection; then apply the test sample (5wt% solution, about 0.05mL) in the test area for 15min, 30min, and 45min for data collection; apply 0.05mL to the blank control Pure water; positive control group smeared with 0.2wt% Deminshu water solution; count the values measured each time at the experimental site of the subjects, and analyze the change of red value.
  • Mexamter MX18 pigment test probe
  • Example 1 has a remarkable repairing effect on the skin after stimulation, and can quickly reduce the redness of the skin due to stimulation, and repair damaged skin.
  • Comparative example 18 (mixed solution) and comparative example 15 (honeysuckle) have a certain repairing effect, but the repairing effect is not as good as that of Example 1. This is because during the re-decocting process, certain weak interactions can occur between the medicinal materials and the medicinal materials, resulting in supramolecular chemical phenomena and promoting the efficacy of the active ingredients.
  • Test Example 2 Comparison of the efficacy of the formula extracts with different ratios
  • Test samples Example 1, Example 7, Comparative Examples 3-11 and Comparative Examples 19-20, the samples were diluted to 5% aqueous solution.
  • Test population 120 volunteers (aged 18-55, male or female) were selected and divided into 12 groups. 10 people per group.
  • the lactic acid stimulation method was to apply filter paper (about 0.8 cm in diameter) soaked with 50 ⁇ L of 10% lactic acid solution at the nasolabial folds on both sides of the volunteers for 10 min, and then remove the filter paper.
  • the tester applies the samples to the test areas on both sides at the same time.
  • the two samples in the same group are randomly distributed on both sides.
  • the amount of the sample applied in each area is 0.1mL. 10min and 15min, the volunteers subjectively evaluated the itching and tingling sensations at the nasolabial folds on both sides (the total score was 5 points, the more severe the itching and tingling sensations, the higher the score, and 0-1 points represented no feeling.
  • both the examples and the comparative examples have the effect of instantly relieving itching and stinging.
  • the effects of instant relieving itching and stinging pain of Examples 1 and 7 are significantly better than the instant pruritic and stinging pain relief effects of the soothing and repairing compositions prepared by any combination of five or three kinds of raw materials in Comparative Examples 3-11.
  • the six components of the composition of the invention have a synergistic effect. If one or several raw materials are removed, the effect of the soothing and repairing composition will be greatly reduced.
  • Example 1 has better effect of instantly relieving itching and tingling, indicating that the distribution ratio of each group of formulations will affect the effect to varying degrees.
  • the embodiments of the present invention are the optimal component allocation ratios obtained through multiple experimental screenings. Because there are too many intermediate experimental procedures, they cannot be listed one by one.
  • the above examples are typical examples and comparative examples.
  • compositions, proportion and preparation process of the composition will affect the expression of its efficacy.
  • the six functional components of purslane, Kochia, honeysuckle, duckweed, ebony, and nepeta in the formula of the present invention have a multi-channel synergistic effect. , produced unexpected technical effects.
  • Test samples Example 1, Comparative Example 8, Comparative Example 9, Comparative Example 20.
  • the experimental method for scavenging free radicals is as follows: prepare 7mmol ⁇ L -1 ABTS stock solution and 140mmol ⁇ L -1 potassium persulfate stock solution. A certain amount of 7 mmol ⁇ L -1 ABTS and 140 mmol ⁇ L -1 potassium persulfate were mixed, and after standing in the dark at room temperature for a period of time, ABTS free radical stock solution was formed. Take a certain amount of ABTS free radical stock solution and dilute it with 50% ethanol, so that the final test negative control absorbance value is 0.70 ⁇ 0.02.
  • Free radicals are a kind of very active active molecular groups (because most of them contain free oxygen atoms, so they are usually called oxygen free radicals. If not specified, free radicals refer to oxygen free radicals), which are usually metabolized by the human body. As a product, damage to the body from environmental factors such as pollution, UV rays and sunlight can also increase free radicals. The harm of free radicals to the human body: 1. The electrons of the cell membrane are easily lost, so the cell membrane is easily attacked by free radicals. Once the electrons are taken away by free radicals, the cell membrane will lose its elasticity and lose some or all functions, resulting in cardiovascular disease. Disease (it is generally believed that free radicals are the root cause of all diseases and aging).
  • a blood clot can block a blood vessel, which is coronary heart disease if it occurs in the coronary arteries that supply blood to the heart, or a stroke if it occurs in the brain.
  • the culprit that causes atherosclerosis is these bad cholesterol oxidized by free radicals; 3. Free radicals act on the enzyme system in the human body, resulting in the release of collagenase and hard elastase, which act on the skin Collagen and hard elastin are excessively cross-linked and degraded, resulting in loss of skin elasticity and wrinkles.
  • the soothing and repairing composition of the present invention has a good free radical scavenging effect. As shown in FIG. 6 , when the concentration of the extract in Example 1 is 0.5% and 2.0%, the free radical scavenging rate can reach 100%.
  • the free radical scavenging rate of the soothing and repairing composition in Example 1 of the present invention is higher than the free radical scavenging rate of the soothing and repairing compositions obtained in Comparative Example 8, Comparative Example 9 and Comparative Example 20, which indicates that the present invention uses purslane , Kochia, Honeysuckle, Duckweed, Ebony, Nepeta, the six functional components combined have produced obvious synergy and synergy, different groups promote each other and have better free radical scavenging effect.
  • Example 6 The composition of Example 1 improves skin effect
  • Volunteers can improve skin itching 15 minutes after applying Example 1, up to 96%, while the effect of the comparative example is obviously low, and the highest improvement rate is only 52%. After 1-3 days of use, most of the volunteers in Example 1 can improve skin redness and swelling up to 80%, while the improvement effect of the comparative example does not exceed 16%. The dry and peeling skin of 75% of the volunteers can be improved after using Example 1 for 1-3 days, while the improvement effect of the comparative example does not exceed 40%. Seven days after using Example 1, 100% of the volunteers could improve skin itching, redness, dryness and desquamation symptoms, while the improvement effect of the comparative example was obviously not as good as that of Example 1.
  • the invention combines the six functional components of purslane, kochia, honeysuckle, duckweed, ebony and nepeta to produce an obvious synergistic effect, which can better relieve the symptoms of itching, redness, dryness and desquamation of the skin, and at the same time Has the effect of repairing the skin barrier.
  • composition of the present invention In order to better verify other effects of the composition of the present invention, the anti-inflammatory and antibacterial effects of the soothing and repairing composition of the present invention were further tested.
  • IL-1 ⁇ plays an important role in the process of immune regulation and inflammatory response, and is considered to be one of the main endogenous mediators that cause febrile response in the process of inflammatory response.
  • Test samples Example 1, Comparative Example 8, Comparative Example 20;
  • Inoculation Inoculate the cells into a 24-well plate and incubate at 37°C in a 5% CO2 incubator for 18-24h.
  • IL-1 ⁇ content Take the cell supernatant from each well, and detect the content of IL-1 ⁇ , a cellular inflammatory factor, according to the operation instructions of the ELISA kit. The results are shown in Table 11.
  • LPS-induced (LPS+) induced a significant increase in the expression of inflammatory factor IL-1 ⁇ (P ⁇ 0.01), indicating that LPS-induced modeling was successful; compared with SC (0.1% DMSO, LPS+) , Dexamethasone in PC (dexamethasone) group at 0.001% administration concentration can significantly down-regulate the expression of IL-1 ⁇ (P ⁇ 0.01), indicating that the test results are effective.
  • Table 11 shows the results of the detection of the expression of the inflammatory factor IL-1 ⁇ in the soothing and repairing composition of the present invention.
  • the soothing and repairing composition of the present invention is in the concentration range of 0.08%, 0.16% and 0.31%. , has a significant inhibitory effect on the expression of inflammatory factor IL-1 ⁇ ; at a concentration of 0.08%, compared with Comparative Example 8 and Comparative Example 20, the soothing and repairing composition of the present invention has a significant inhibitory effect on the expression of inflammatory factor IL-1 ⁇ .
  • the bacteriostatic effect of the soothing and repairing composition of the present invention was detected.
  • the soothing and repairing composition of the present invention has a good bacteriostatic effect on Staphylococcus epidermidis and Staphylococcus aureus.
  • the chicken embryo chorioallantoic membrane test and the in vitro short-term exposure test of rabbit corneal epithelial cells were carried out, and the experimental results showed no irritation.
  • the results of the red blood cell hemolysis and coagulation test showed that there was no coagulation phenomenon.
  • the soothing and repairing composition of the present invention contains six functional components of purslane, kochia, duckweed, honeysuckle, ebony, and nepeta.
  • Anti-inflammatory, antibacterial, repairing skin barrier, improving skin tolerance” and other functions solve skin problems caused by various factors such as environment, region, staying up late, stress and changing seasons, such as sensitive skin. In terms of safety, it has very reliable safety and can be used in the field of cosmetics with confidence.

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Abstract

本发明公开了一种舒缓修护组合物及其制备方法，属于植物提取研究领域。该组合物包括马齿苋、地肤子、浮萍、金银花、乌梅、荆芥，通过各组分相互作用，多通路起效，解决环境、地域、熬夜、压力和换季等各类因素诱导的肌肤问题。本发明舒缓修护组合物具有即时舒缓皮肤发红、瘙痒、刺痛，清除自由基、抗炎、提高皮肤耐受性、修复皮肤屏障等功效。将其应用于化妆品中，预计具有抗刺激、舒缓肌肤、抗氧化、抗炎、修复皮肤屏障等功效。

Description

一种舒缓修护组合物及其制备方法和应用 技术领域
本发明涉及植物提取研究领域，具体涉及一种舒缓修护组合物及其制备方法和应用。
背景技术
随着社会城市化和工业化的迅速发展，环境污染、化妆品刺激导致出现越来越多的问题肌肤如“敏感肌”、“口罩脸”、“激素脸”。由于疫情的原因，大家需要每天都带着口罩，使得各类皮肤问题加重，在身体上和心理上都给消费者带来了很大困扰。这些皮肤问题有许多相似的症状，伴有皮肤屏障功能受损、皮肤不耐受、皮肤炎症等情况，其修复机制较为复杂，需多通路协同作用。简单来说就是需要修复屏障、抑菌、消炎、消肿止痒、提高皮肤耐受性等功效同时作用于肌肤，单一通路机制修复无法从根本上解决问题，只能一时缓解症状，易反复发做。
专利(CN112137932A)公开一种抗敏修复组合物，由地肤子(KOCHIA SCOPARIA)提取物、母菊(CHAMOMILLA RECUTITA)花提取物、丹参(SALVIA MILTIORRHIZA)根提取物、马齿苋(PORTULACA OLERACEA)提取物、卡瓦胡椒(PIPER METHYSTICUM)叶/根/茎提取物组成。但该组合物仅从舒缓肌肤泛红、干痒、灼热、刺痛等角度缓解问题肌肤的症状。
基于此，针对上述作用通路单一、无法从根本上解决肌肤问题的现状，开发一种通过多种通路协同作用缓解问题肌肤的植物提取物是非常有必要的。
发明内容
本发明的主要目的是提供一种舒缓修护组合物及其制备方法，该组合物通过各组分相互作用，多通路起效，解决环境、地域、熬夜、压力和换季等各类因素诱导的肌肤问题。
本发明舒缓修护组合物具有即时舒缓皮肤发红、瘙痒、刺痛，清除自由基、抗炎、提高皮肤耐受性、修复皮肤屏障等功效。
为此，本申请提供的技术方案如下：
本发明第一方面提供了一种舒缓修护组合物。
根据本发明，所述舒缓修护组合物包括以下重量份数的组分：马齿苋5-40份、地肤子1-30份、浮萍5-20份、金银花1-20份、乌梅3-15份、荆芥1-10份。
根据本发明，所述舒缓修护组合物通过包括以下步骤的制备方法制备：
(1)原料预处理；
(2)将总原料和去离子水按照一定料液比提取，得提取液；
(3)将步骤(2)提取液过滤，得粗滤液；
(4)将步骤(3)粗滤液精滤，得滤液；
(5)灭菌。
根据本发明，所述制备方法步骤(2)中原料总重量与水的重量比为1:15-1:70(m/m)(以原料干重计)。
根据本发明，所述制备方法步骤(2)中原料总重量与水的重量比可以是1:15(m/m)、1:16(m/m)、1:17(m/m)、1:18(m/m)、1:19(m/m)、1:20(m/m)、1:25(m/m)、1:30(m/m)、1:35(m/m)、1:40(m/m)、、1:45(m/m)、1:50(m/m)、1:55(m/m)、1:60(m/m)、1:65(m/m)、1:70(m/m)。
根据本发明的一些具体实施方式，所述制备方法步骤(2)中原料总重量与水的重量比为1:20-1:50(m/m)(以原料干重计)。
根据本发明，所述制备方法步骤(2)中提取温度为100-130℃。
根据本发明的一些具体实施方式，所述制备方法步骤(2)中提取温度为110℃。
根据本发明，所述制备方法步骤(2)中提取压力为0.1-0.3MPa。
根据本发明的一些具体实施方式，所述制备方法步骤(2)中提取压力为0.15MPa。
根据本发明，所述制备方法步骤(2)中提取时间为1-3h。
根据本发明的一些具体实施方式，所述制备方法步骤(2)中提取时间为1.5h。
根据本发明，所述制备方法步骤(3)中过滤滤布60-100目。
根据本发明，所述制备方法步骤(3)中粗滤滤掉药渣。
根据本发明，所述制备方法步骤(4)中精滤方式为板框过滤。
根据本发明，所述制备方法步骤(4)中精滤板框过滤滤板孔径为0.3-0.5μm。
根据本发明，所述制备方法步骤(4)中精滤板框过滤滤板为SCP-1120型。
根据本发明，所述制备方法步骤(5)中灭菌方式为常规灭菌方式。
根据本发明，所述制备方法步骤(5)中灭菌方式为高温灭菌。
根据本发明的一些具体实施方式，所述制备方法步骤(5)中灭菌温度为90-95℃。
根据本发明的一些具体实施方式，所述制备方法步骤(5)中灭菌时间为30-60min。
根据本发明的一些具体实施方式，所述制备方法步骤(5)还包括添加防腐剂。
根据本发明的一些具体实施方式，所述制备方法步骤(5)中添加防腐剂为戊二醇，己二醇。
根据本发明的一些具体实施方式，所述制备方法步骤(5)中以滤液重量计，戊二醇添加量为1-5wt％，己二醇添加量为0.5-2wt％。
根据本发明，所述制备方法步骤(1)中原料预处理包括挑拣异物、清洗。
本发明第二方面提供了本发明第一方面所述舒缓修护组合物的制备方法。
根据本发明，所述舒缓修护组合物的制备方法包括以下步骤：
(1)原料预处理，称量马齿苋5-40份，地肤子1-30份、浮萍5-20份、金银花1-20份、乌梅3-15份、荆芥1-10份；
(2)将总原料和去离子水按照1:15-1:70(m/m)料液比，在提取温度为100-130℃，提取压力为0.1-0.3MPa条件下提取1-3h，得提取液；
(3)将步骤(2)提取液用60-100目滤布过滤，得粗滤液；
(4)将步骤(3)粗滤液用板框过滤方式精滤，滤板孔径为0.3-0.5μm，得滤液；
(5)灭菌。
根据本发明，所述制备方法步骤(2)中原料总重量与水的重量比可以是1:15(m/m)、1:16(m/m)、1:17(m/m)、1:18(m/m)、1:19(m/m)、1:20(m/m)、1:25(m/m)、1:30(m/m)、1:35(m/m)、1:40(m/m)、、1:45(m/m)、1:50(m/m)、1:55(m/m)、1:60(m/m)、1:65(m/m)、1:70(m/m)。
根据本发明的一些具体实施方式，所述制备方法步骤(2)中原料总重量与水的重量比为1:20-1:50(m/m)(以原料干重计)。
根据本发明的一些具体实施方式，所述制备方法步骤(2)中提取温度为 110℃。
根据本发明的一些具体实施方式，所述制备方法步骤(2)中提取压力为0.15MPa。
根据本发明的一些具体实施方式，所述制备方法步骤(2)中提取时间为1.5h。
根据本发明，所述制备方法步骤(3)中粗滤滤掉药渣。
根据本发明，所述制备方法步骤(4)中精滤方式为板框过滤。
根据本发明，所述制备方法步骤(4)中精滤板框过滤滤板为SCP-1120型。
根据本发明，所述制备方法步骤(5)中灭菌方式为常规灭菌方式。
根据本发明，所述制备方法步骤(5)中灭菌方式为高温灭菌。
根据本发明的一些具体实施方式，所述制备方法步骤(5)中灭菌温度为90-95℃。
根据本发明的一些具体实施方式，所述制备方法步骤(5)中灭菌时间为30-60min。
根据本发明的一些具体实施方式，所述制备方法步骤(5)还包括添加防腐剂。
根据本发明的一些具体实施方式，所述制备方法步骤(5)中添加防腐剂为戊二醇，己二醇。
根据本发明的一些具体实施方式，所述制备方法步骤(5)中以滤液重量计，戊二醇添加量为1-5wt％，己二醇添加量为0.5-2wt％。
根据本发明，所述制备方法步骤(1)中原料预处理包括挑拣异物、清洗。
本发明第三方面提供了本发明第一方面所述舒缓修护组合物和/或本发明第二方面所述舒缓修护组合物的制备方法制备得到的舒缓修护组合物在化妆品和/或护肤品领域中的应用。
根据本发明，所述护肤品为面膜、膏霜、乳液、护肤水、洗面奶、洗发水、护发素或沐浴露等，不受剂型的限制。
本发明的有益效果
(1)本发明舒缓修护组合物包含马齿苋、地肤子、浮萍、金银花、乌梅、荆芥六种功效成分，多通路协同作用，通过“拮抗刺激、舒缓肌肤、清除自由基、抗炎、抑菌、修护皮肤屏障、提高皮肤耐受性”等作用解决环境、地域、熬夜、 压力和换季等各类因素诱导的肌肤问题，如敏感肌。
(2)本发明采用高温高压提取工艺，提高了舒缓修护组合物中功效成分总糖含量、总黄酮含量和多酚含量，促进功效成分表达，加速反应进程，提高原料利用率，节约生产成本。
附图说明
图1是辣椒碱刺激实验结果图；
图2是实施例1、实施例7、对比例3-对比例11乳酸刺激后瘙痒感评分图；
图3是实施例1、实施例7、对比例3-对比例11乳酸刺激后刺痛感评分图；
图4是实施例1、实施例7、对比例19-对比例20乳酸刺激后刺痛感评分图；
图5是实施例1、实施例7、对比例19-对比例20乳酸刺激后瘙痒感评分图；
图6是ABTS自由基清除率图。
具体实施方式
以下结合附图和实施例对本发明进行详细说明，但本发明并不受下述实施例限定。
本发明使用原料的来源见表1，如无特殊说明本发明所使用原料及仪器均为常规原料或仪器。
表1 使用原料来源
原料名称 供应商/生产商 产地
马齿苋 北京仟草中药饮片有限公司 河北
地肤子 北京仟草中药饮片有限公司 河北
浮萍 同仁堂 河北
金银花 北京仟草中药饮片有限公司 河北
乌梅 北京仟草中药饮片有限公司 四川
荆芥 同仁堂 河北
己二醇 德之馨 德国
戊二醇 德之馨 德国
实施例1：称取马齿苋30g、地肤子20g、浮萍15g、金银花10g、乌梅10g、荆芥5g；按照料液比1:50(m/m)加入4500g去离子水；在110℃，0.15MPa条件下提取1.5h；先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤； 加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到组合物。
实施例2：称取马齿苋5g、地肤子1g、浮萍5g、金银花1g、乌梅3g、荆芥1g；按照料液比1:70(m/m)加入1120g去离子水；在100℃，0.1MPa条件下提取1.5h；先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到组合物。
实施例3：称取马齿苋40g、地肤子30g、浮萍20g、金银花20g、乌梅15g、荆芥10g；按照料液比1:20(m/m)加入2700g去离子水；在130℃，0.3MPa条件下提取1.5h；先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到组合物。
实施例4：称取马齿苋30g、地肤子20g、浮萍15g、金银花10g、乌梅10g、荆芥5g；按照料液比1:20(m/m)加入1800g去离子水；在110℃，0.15MPa条件下提取1.5h；先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到组合物。
实施例5：称取马齿苋30g、地肤子20g、浮萍15g、金银花10g、乌梅10g、荆芥5g；按照料液比1:50(m/m)加入4500g去离子水；100℃，在0.1MPa条件下提取1.5h；先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到组合物。
实施例6：称取马齿苋30g、地肤子20g、浮萍15g、金银花10g、乌梅10g、荆芥5g；按照料液比1:20(m/m)加入1800g去离子水；在130℃，0.3MPa条件下提取1.5h；先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到组合物。
实施例7：称取马齿苋20g、地肤子20g、浮萍15g、金银花10g、乌梅5g、荆芥5g；按照料液比1:50(m/m)加入3750g去离子水；在110℃，0.15MPa条件下提取1.5h；先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到组合物。
对比例1
称取马齿苋30g、地肤子20g、浮萍15g、金银花10g、乌梅10g、荆芥5g，按照料液比1:50(m/m)加入4500g去离子水；80℃条件下水浴提取1.5h；先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％ 己二醇防腐，水浴锅90-95℃灭菌30min，得到组合物。
对比例2
称取马齿苋30g、地肤子20g、浮萍15g、金银花10g、乌梅10g、荆芥5g，按照料液比1:50(m/m)加入4500g去离子水；在150℃，0.5MPa条件下提取1.5h；先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到组合物。
对比例3-11
分别按照表2原料和工艺制备对比例3-11提取液；然后先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到组合物。
表2 对比例3-11原料组分配比和制备工艺
Figure PCTCN2022081927-appb-000001
对比例12-17
分别按照表3原料和工艺制备对比例12-17提取液；然后先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到组合物。
表3 对比例12-17原料组分配比和制备工艺
原料/工艺 对比例12 对比例13 对比例14 对比例15 对比例16 对比例17
马齿苋/g 30g - - - - -
地肤子/g - 20g - - - -
浮萍/g - - 15g - - -
金银花/g - - - 10g - -
乌梅/g - - - - 10g -
荆芥/g - - - - - 5g
料液比/(m/m) 1:50 1:50 1:50 1:50 1:50 1:50
提取温度 110℃ 110℃ 110℃ 110℃ 110℃ 110℃
提取压力 0.15 0.15 0.15 0.15 0.15 0.15
提取时间 1.5h 1.5h 1.5h 1.5h 1.5h 1.5h
对比例18
按照对比例12：对比例13：对比例14：对比例15：对比例16：对比例17提取物＝6：4：4：2：2：1取上述提取物4500g，混合搅拌均匀后得到混合液。
对比例19
称取马齿苋1g、地肤子1g、浮萍1g、金银花20g、乌梅20g、荆芥20g，按照料液比1:50(m/m)加入3150g去离子水；在110℃，0.15MPa条件下提取1.5h；先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到提取物。
对比例20
称取马齿苋5g、地肤子5g、浮萍5g、金银花5g、乌梅20g、荆芥20g，按照料液比1:50(m/m)加入3000g去离子水；110℃，0.15MPa提取1.5h；先用100目滤布将提取液过滤一遍，再用0.3-0.5μm滤板过滤；加入2％戊二醇，1.5％己二醇防腐，水浴锅90-95℃灭菌30min，得到提取物。
试验例1：不同制备工艺植物组合物基本指标测试
1.1多糖、总糖含量测定
采用苯酚-硫酸法进行(具体参照银耳中多糖的含量测定[J].黑龙江医药科学,1999(06):32-32.)。
1.2pH值：利用pH计测得。
1.3固含量：利用固含仪测得。
为了防止浓缩倍数误差对提取物有效成分含量的影响，各指标测定均为浓缩前滤液。
表4 不同制备工艺植物组合物的基本指标
Figure PCTCN2022081927-appb-000002
Figure PCTCN2022081927-appb-000003
利用水提法制备组方组合物时，发现一些重量很轻的药材会飘在液体表面上，即使搅拌也无法解决这个问题，容易造成药材反应不充分，大大降低了提取效率。高温高压法是在压强较高的密闭条件下提取活性成分的方法，该提取法可以在反应时加速反应，同时密闭的条件也可以使水蒸气充分接触各药材，提升反应效率。由表4可知，与普通水提法相比，高温高压法处理提高了组合物的总糖含量、总黄酮含量和多酚含量，避免因原料利用不充分产生的资源浪费，大大节约了成本。同时，对比实施例1、实施例5-6和对比例2可以发现，当高温高压处理的温度和压力超过某一范围后，较高的温度和压力基本不再提高提高植物的提取效率，但过高的压力不仅带来了安全隐患，也会增加能耗，产生能源浪费。综上所述，本发明高温高压提取条件为提取压力0.1-0.3MPa，提取温度为100℃-130℃。
表5 单一原料和组合原料提取物的基本指标
  pH值 固含量/％ 溶液颜色
实施例1(高温高压法) 4.98 2.8 黑褐色
对比例12(马齿苋) 5.85 1.2 土黄色
对比例13(地肤子) 5.81 1.0 棕色
对比例14(浮萍) 6.10 1.0 黑褐色
对比例15(金银花) 5.29 1.6 黄色
对比例16(乌梅) 2.62 1.6 棕色
对比例17(荆芥) 5.63 0.4 淡黄色
对比例18(混合液) 5.21 1.3 黑褐色
中药在煎制时分为单煎和复煎两种，复煎是将所有药材同时放在锅内煮，单煎是将每味药材分别煮好后，然后将药汤混合。为了验证单煎和复煎对组方功效 的影响，对实施例1和对比例12-17的相关指标数据进行测试，结果如表5所示。与对比例18相比，实施例1溶液颜色与其相似，具有较高的固含量，说明复煎时药材和药材之间发生了一定的弱相互作用，产生超分子化学现象，促进功效成分溶于提取液中。因乌梅提取物由于pH值(2.62)过低，对皮肤容易产生刺激，后期实验中舍弃乌梅提取物。
1.4辣椒碱试验
测试样品：实施例1、对比例12-18
测试部位：左、右手臂内侧；
选择受试者左、右手臂内侧作为受试部位，以规格为2cm×2cm的方形区域进行循环标记；用清水清洗受试区(同一区域)，受试者在温度20.6～21.2℃，相对湿度43～52％条件下静坐10min，用德国CK公司的Mexamter MX18(色素测试探头)测量皮肤红值的空白值，随后进入涂抹实验阶段；用质量分数为0.02％的辣椒素水溶液(约0.01mL)对受试区域进行刺激；持续刺激15min及30min后，进行数值采集；然后在受试区域涂抹测试样品(5wt％溶液，约0.05mL)15min、30min、45min后进行数据采集；空白对照涂抹0.05mL纯水；阳性对照组涂抹0.2wt％
Figure PCTCN2022081927-appb-000004
德敏舒水溶液；统计受试者实验部位每次测得的数值，分析红值的变化。
皮肤红值变化反映在测试周期内，实验区域皮肤泛红随时间变化规律。其值越大，皮肤泛红的程度越大。皮肤红值变化率(％)＝(T-T空白值)/T空白值×100％。
从图1中可以看出，实施例1对皮肤刺激后的修复效果显著，能快速降低皮肤因刺激产生的泛红现象，修复受损肌肤。对比例18(混合液)和对比例15(金银花)有一定的修复效果，但是修复效果不如实施例1。这是因为复煎过程中，药材和药材之间可以发生一定的弱相互作用，产生超分子化学现象，促进活性成分的功效发挥。
试验例2：不同配比下组方提取物功效比较
测试样品：实施例1、实施例7、对比例3-11和对比例19-20，将样品稀释为5％水溶液。
测试人群：选择120名(18-55岁，男女不限)志愿者，将其分为12组。每组10人。
乳酸刺激方法为在志愿者两侧鼻唇沟处同时敷贴浸透50μL 10％乳酸溶液的滤纸(直径约0.8cm)10min，去除滤纸。由测试人员在两侧测试区域同时涂抹样品，同一分组内两个样品随机分布于两侧，每个区域涂样量为0.1mL，在样品使用前、使用后0min、0.5min、2min、5min、10min、15min，由志愿者主观评价两侧鼻唇沟处的瘙痒感、刺痛感感觉(总分值5分，瘙痒感、刺痛感越重分值越高，0-1分代表没有感觉或略微有一点感觉，1-3分代表轻度刺激，能感觉到瘙痒感和刺痛感，3-5分代表重度刺激，瘙痒感和刺痛感严重)。利用志愿者感官评价评测测试样品即时舒缓刺痛和瘙痒功效，实验结果如图2-5所示。
由图2-3可知，使用样品后，实施例和对比例均具有即时舒缓瘙痒和刺痛的功效。实施例1和实施例7即时舒缓瘙痒和刺痛的效果显著优于对比例3-11任意其中五种或三种原料组合制备的舒缓修护组合物即时舒缓瘙痒和刺痛的效果，说明本发明组方六种组分之间具有协同增效作用，若去掉某一种原料或几种原料，将会导致舒缓修护组合物效果大大降低。
由图4-5可是，与对比例19-20相比，实施例1具有更好的即时舒缓瘙痒和刺痛的功效，说明组方种各组分配比会对效果造成不同程度的影响。本发明实施例是经过多次实验筛选得到的最优组分配比，因为中间实验过程太多，不能一一都放上，上述列举均为典型实施例和对比例。
综上，组合物组方和配比、制备工艺都会影响其功效表达，本发明组方中马齿苋、地肤子、金银花、浮萍、乌梅、荆芥六种功效成分，多通路协同作用，产生了意想不到的技术效果。
试验例3：功效验证
3.1清除自由基
测试样品：实施例1、对比例8、对比例9、对比例20。
实验方法：清除自由基实验方法如下：制备为7mmol·L -1 ABTS储备液和140mmol·L -1过硫酸钾储备液。将一定量7mmol·L -1 ABTS和140mmol·L -1过硫酸钾混合，在室温下避光静置一段时间后，形成ABTS自由基储备液。取一定量的ABTS自由基储备液，用50％乙醇稀释，使最终测试阴性对照吸光值为0.70±0.02。
自由基是一类非常活跃的活性分子基团(因为绝大部分含有自由的氧原子，所以通常又叫氧自由基。如果不特别说明，自由基就是指氧自由基)，通常是人 体代谢的产物，环境因素对身体的伤害也可增加自由基，如污染、紫外线和阳光。自由基对人体的害处：1.细胞膜的电子很容易丢失，所以细胞膜极易遭受自由基的攻击，一旦被自由基夺走电子，细胞膜就会失去弹性并丧失部分或一切功能，从而导致心血管疾病(一般认为自由基是一切疾病和衰老的根源)。更为严重的是自由基对基因的攻击，可以使基因的分子结构杯破坏，导致基因突变，从而引起整个生命发生系统性的混乱；2.人体内的坏胆固醇容易被自由基氧化，氧化后会形成泡沫细胞，它们会附着在血管壁上。积累到一定程度后，就会对血管形成阻塞，或者破裂成碎片进入血液中，当血液接触到这些碎片后就会凝聚形成血栓。血栓会使血管阻塞，如果发生在供应心脏血液的冠状动脉，就是得冠心病，如果发生在脑部，就会造成中风。也就是说，导致动脉粥样硬化的罪魁祸首，就是这些被自由基氧化的坏胆固醇；3.自由基作用于人体内酶系统，导致胶原蛋白酶和硬弹性蛋白酶的释放，这些酶作用于皮肤中的胶原蛋白和硬弹性蛋白并使这两种蛋白产生过度交联并降解，结果使皮肤失去弹性，出现皱纹。
本发明舒缓修护组合物具有很好的清除自由基效果，如图6所示，实施例1提取液在浓度为0.5％和2.0％时，对自由基的清除率可达到100％。本发明实施例1舒缓修护组合物对自由基清除率高于对比例8、对比例9和对比例20得到的舒缓修护组合物对自由基的清除率，这表明本发明将马齿苋、地肤子、金银花、浮萍、乌梅、荆芥六种功效成分组合产生了明显的增效协同作用，不同组生互相促进，具有更好的清除自由基功效。
3.2修复屏障、消肿效果
实验方法：招募100名有皮肤瘙痒、红肿、干燥脱屑志愿者，分为4组，每组25人，每天正常清洁护肤后，分别涂抹测试样品实施例1、对比例8、对比例9、对比例20(均为5％水溶液)，使用7天。
表6 实施例1组合物改善皮肤效果
  改善皮肤瘙痒 改善皮肤红肿 改善皮肤干燥脱皮
使用15分钟 24/25人，96％ 2/25人，8％ 1/25人，4％
使用1-3天 25/25人，100％ 20/25人，80％ 18/25人，72％
使用7天 25/25人，100％ 25/25人，100％ 25/25人，100％
表7 对比例8组合物改善皮肤效果
  改善皮肤瘙痒 改善皮肤红肿 改善皮肤干燥脱皮
使用15分钟 5/25人，20％ 0/25人，0％ 2/25人，20％
使用1-3天 12/25人，48％ 3/25人，12％ 10/25人，40％
使用7天 21/25人，84％ 7/25人，28％ 20/25人，80％
表8 对比例9组合物改善皮肤效果
  改善皮肤瘙痒 改善皮肤红肿 改善皮肤干燥脱皮
使用15分钟 3/25人，12％ 0/25人，0％ 2/25人，8％
使用1-3天 5/25人，20％ 2/25人，8％ 5/25人，20％
使用7天 12/25人，48％ 8/25人，32％ 13/25人，52％
表9 对比例20组合物改善皮肤效果
  改善皮肤瘙痒 改善皮肤红肿 改善皮肤干燥脱皮
使用15分钟 13/25人，52％ 0/25人，0％ 3/25人，20％
使用1-3天 18/25人，72％ 4/25人，16％ 9/25人，36％
使用7天 20/25人，80％ 11/25人，44％ 14/25人，56％
志愿者涂抹使用实施例1后15min就可以改善皮肤瘙痒感，高达96％，而对比例效果明显偏低，最高的改善率仅为52％。使用1-3天后，实施例1大部分志愿者可以改善皮肤红肿，高达80％，而对比例改善效果不超过16％。75％的志愿者皮肤干燥脱皮现象使用实施例1后1-3天后可得到改善，而对比例改善效果不超过40％。使用实施例1后7天100％志愿者皮肤瘙痒感、红肿、干燥脱屑症状都可以得到改善，而对比例改善效果明显不如实施例1。并且使用实施例1志愿者反馈，之后在使用其他产品时，皮肤过敏现象减少了，感觉也没那么刺激了，这也说明了本组方具有良好的修复屏障的效果。而其他组使用对比例的志愿者，没有反馈自己的皮肤屏障功能得到改善。本发明将马齿苋、地肤子、金银花、浮萍、乌梅、荆芥六种功效成分组合产生了明显的增效协同作用，能更好的缓解皮肤瘙痒、红肿、干燥脱屑症状，同时具有修复皮肤屏障的功效。
为了更好的验证本发明组方其他的效果，进一步对本发明舒缓修护组合物进行抗炎和抑菌效果检测。
3.3抗炎实验
采用脂多糖(LPS)诱导，作用对象为RAW264.7，模拟普遍的机体炎症，测试的炎症因子为IL-1β。IL-1β在免疫调节和炎症反应过程中起重要作用，被认 为是炎症反应过程中引起发热反应的主要内源性介质之一，一旦炎症因子在皮肤细胞中含量增加，皮肤温度高于正常温度，将加剧皮肤炎症反应，引发机体炎症级联反应。
测试样品：实施例1、对比例8、对比例20；
实验方法：采用LPS诱导RAW264.7细胞炎症模型进行抗炎检测：
(1)接种：将细胞接种至24孔板中，37℃，5％CO 2培养箱孵育18-24h。
(2)配液：根据表10配制受试物和阳性对照。
(3)给样：根据表10试验分组和浓度设置，待24孔板中细胞铺板生长18-24h后，进行分组给样，每个处理组设3个复孔。组1中，空白对照与阴性对照组均加入含0.1％DMSO的细胞培养基，阳性对照加入含有0.001％地塞米松的细胞培养基；组2中，空白对照与阴性对照组均加入细胞培养基，样品组加入含有相应浓度样品的细胞培养基，于37℃，5％CO 2培养箱继续培养18-24h。
表10 实验分组和浓度设置
Figure PCTCN2022081927-appb-000005
(4)LPS诱导：培养24h后，将板内培养基吸出，均加入PBS轻洗一次，空白对照组加入细胞培养基，阴性对照组、样品组和阳性对照组加入含有LPS的细胞培养基，37℃，5％CO 2培养箱继续培养24h后收集上清液。
(5)IL-1β含量检测：取各孔细胞上清液，根据ELISA试剂盒操作说明，进行细胞炎症因子IL-1β含量检测，结果见表11。
表11 炎症因子IL-1β表达检测结果
Figure PCTCN2022081927-appb-000006
与BC(LPS-)组相比，LPS诱导(LPS+)引起炎症因子IL-1β表达量显著升高(P<0.01)，表明LPS诱导造模成功；与SC(0.1％DMSO，LPS+)相比，PC(地塞米松)组中地塞米松在0.001％给药浓度下，可显著下调IL-1β的表达量(P<0.01)，表明本次检测结果有效。
本发明舒缓修护组合物炎症因子IL-1β表达检测结果作用如表11所示，与NC(LPS+)组相比，本发明舒缓修护组合物在0.08％、0.16％、0.31％浓度范围内，对炎症因子IL-1β表达具有显著性抑制作用；在0.08％浓度时，与对比例8、对比例20相比，本发明舒缓修护组合物对炎症因子IL-1β表达具有显著性抑制作用。
3.4抑菌效果
按照QB/T 2738-2012日化产品抗菌抑菌效果的评价方法检测本发明舒缓修护组合物的抑菌效果。
表12 本发明舒缓修护组合物抑菌效果
Figure PCTCN2022081927-appb-000007
Figure PCTCN2022081927-appb-000008
如表12所示，本发明舒缓修护组合物对表皮葡萄球菌和金黄色葡萄球菌具有良好的抑菌效果。
3.5安全性
为了保证本组方的安全性，进行鸡胚绒毛尿囊膜试验和兔角膜上皮细胞体外短时暴露试验，实验结果显示没有刺激性。红细胞溶血凝血试验结果显示，无凝血现象。
综上，本发明舒缓修护组合物包含马齿苋、地肤子、浮萍、金银花、乌梅、荆芥六种功效成分，多通路协同作用，通过“拮抗刺激、舒缓肌肤、清除自由基、抗炎、抑菌、修护皮肤屏障、提高皮肤耐受性”等作用解决环境、地域、熬夜、压力和换季等各类因素诱导的肌肤问题，如敏感肌。在安全方面，具有非常可靠的安全性，可以放心将其应用于化妆品领域。
本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定，对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动，这里无法对所有的实施方式予以穷举，凡是属于本发明的技术方案所引伸出的显而易见的变化或变动仍处于本发明的保护范围之列。

Claims (9)

  1. 一种舒缓修护组合物，其特征在于，所述舒缓修护组合物包括以下重量份数的组分：马齿苋5-40份、地肤子1-30份、浮萍5-20份、金银花1-20份、乌梅3-15份、荆芥1-10份。
  2. 根据权利要求1所述的舒缓修护组合物，其特征在于，所述舒缓修护组合物通过包括以下步骤的制备方法制备：
    (1)原料预处理；
    (2)将总原料和去离子水按照一定料液比提取，得提取液；
    (3)将步骤(2)提取液过滤，得粗滤液；
    (4)将步骤(3)粗滤液精滤，得滤液；
    (5)灭菌。
  3. 根据权利要求2所述的舒缓修护组合物，其特征在于，所述制备方法步骤(2)中原料总重量与水的重量比为1:15-1:70(m/m)(以原料干重计)。
  4. 根据权利要求2所述的舒缓修护组合物，其特征在于，所述制备方法步骤(2)中提取温度为100-130℃，提取压力为0.1-0.3MPa，提取时间为1-3h。
  5. 根据权利要求2所述的舒缓修护组合物，其特征在于，所述制备方法步骤(3)中过滤滤布60-100目。
  6. 根据权利要求2所述的舒缓修护组合物，其特征在于，所述制备方法步骤(4)中精滤方式为板框过滤，和/或所述滤板孔径为0.3-0.5μm。
  7. 一种舒缓修护组合物的制备方法，其特征在于，所述制备方法包括以下步骤：
    (1)原料预处理，称量马齿苋5-40份、地肤子1-30份、浮萍5-20份、金银花1-20份、乌梅3-15份、荆芥1-10份；
    (2)将总原料和去离子水按照1:15-1:70(m/m)料液比，在提取温度为100-130℃，提取压力为0.1-0.3MPa条件下提取1-3h，得提取液；
    (3)将步骤(2)提取液用60-100目滤布过滤，得粗滤液；
    (4)将步骤(3)粗滤液用板框过滤方式精滤，滤板孔径为0.2-10μm，得滤液；
    (5)灭菌。
  8. 权利要求1-6中任一项所述的舒缓修护组合物或权利要求7所述的舒缓修护 组合物的制备方法制备得到的舒缓修护组合物在化妆品和/或护肤品领域中的应用。
  9. 根据权利要求8所述的应用，其特征在于，所述舒缓修护组合物在制备具有舒缓肌肤、清除自由基、抗炎、提高皮肤耐受性、修复皮肤屏障功效的化妆品和/或护肤品中的应用。
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