CN117243868B - Camellia extract with soothing effect and preparation method and application thereof - Google Patents
Camellia extract with soothing effect and preparation method and application thereof Download PDFInfo
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Classifications
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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
- 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
- A61Q19/00—Preparations for care of the skin
- A61Q19/005—Preparations for sensitive skin
-
- 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
- A61K2800/78—Enzyme modulators, e.g. Enzyme agonists
- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
-
- 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
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- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Birds (AREA)
- Rheumatology (AREA)
- Epidemiology (AREA)
- Microbiology (AREA)
- Botany (AREA)
- Biotechnology (AREA)
- Engineering & Computer Science (AREA)
- Dermatology (AREA)
- Pain & Pain Management (AREA)
- Mycology (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Organic Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Cosmetics (AREA)
Abstract
The invention relates to a camellia extract with a soothing effect, and a preparation method and application thereof. The preparation method is characterized in that the camellia extract is prepared efficiently by an extraction process of low-pressure internal boiling combined enzymolysis, the whole operation process is simple and feasible, the period is short, the extraction process temperature is low, the loss is less, the extraction efficiency of active ingredients is high, the obtained extract has high flavone and polyphenol content and low saponin content, and under the specific composition of three active matters, the inhibition effect of the camellia extract on hyaluronidase, inflammatory factors TNF-alpha and IL-6 is obviously enhanced, so that the camellia extract can be used for the release effect of skin care products.
Description
Technical Field
The invention relates to the field of cosmetics, in particular to a camellia extract with a soothing effect, and a preparation method and application thereof.
Background
Camellia japonica (Camellia japonica L.) is a plant belonging to the genus Camellia of the family Theaceae, and is originally produced in China, and is also called camellia, microcystis, camellia, winter resistance, etc. Warm, moist and semi-yin environment is preferred, and the people are afraid of high temperature and are prohibited from burning sun. There is a distribution in the northwest of Yunnan to the west of Guizhou, in the middle of Sichuan, in the northwest of Hunan and in the northwest of Guangxi. The camellia is rich in various bioactive components such as protein, amino acid, saponin, reducing sugar, polysaccharide, polyphenol, flavone, anthocyanin, vitamin and the like, is an important efficacy additive in cosmetics and daily chemical products, and has the skin care effects of relieving, whitening, resisting oxidation, resisting aging, moisturizing and the like.
The active substances of the camellia extract obtained by the existing preparation method are low in active substance content and ambiguous in composition, and organic solvents such as methanol, ethyl acetate, n-hexane and n-butanol are used, so that the safety risk of solvent residues exists, and the active substances are not applicable to skin care products; some technologies use macroporous resin purification technology, and although the purity is high, the preparation period is long, the cost is high, and the technology is not suitable for large-scale production. In addition, the prior art does not clearly extract the camellia flavone and polyphenol at the same time, and remove the saponin components in the camellia flavone and polyphenol, so that the components have serious foaming in the concentration process, and the solvent recovery efficiency is low, so that the large-scale production is not facilitated.
Chinese patent application CN113797261a discloses a preparation method of camellia extract/leaf, which uses fresh camellia and/or mountain tea as raw material, ethanol as solvent, and the extract is obtained through the procedures of cleaning, crushing, ultrasonic-assisted extraction, concentration, refining, etc., the yield of flavone and polyphenol in the obtained extract is obviously improved, and the antioxidation capability is enhanced. However, the removal of saponins was not involved in this method, nor was the soothing efficacy of the resulting extract evaluated.
The patent application document CN113577165A discloses an extraction method for camellia polyphenol, which takes camellia powder as a raw material, and obtains the camellia polyphenol through leaching, extraction, concentration and drying, wherein the extraction liquid only relates to the extraction of the polyphenol, and contains acetone, and the extractant contains organic solvents such as ethyl acetate and the like.
Disclosure of Invention
Based on the above, in order to solve at least one technical problem in the prior art, the invention provides a method for efficiently preparing the camellia extract with the relieving effect, and the obtained extract has high flavone and polyphenol content, low saponin content and obvious relieving effect.
The first object of the present invention is to provide a preparation method of a camellia extract with soothing effect, comprising the steps of:
s1, desorption: adding 80-90wt% ethanol into flos Camelliae Japonicae powder, and desorbing at normal temperature;
s2, extracting: heating the camellia feed liquid desorbed at normal temperature in water bath at 40-50deg.C under vacuum degree of-0.1 Mpa to-0.08 Mpa, rapidly adding deionized water and mixed enzyme after slight boiling of the surface, and extracting at vacuum degree and temperature; the mixed enzyme comprises glucosidase, arabinosidase and galactosidase;
s3, concentrating: after the extracting solution in the step S2 is cooled to room temperature, adding ethanol while stirring until the ethanol concentration in the final solution reaches 75-80wt%, and then stirring, standing and filtering to obtain a concentrated solution;
s4, preparing: adding water, polyalcohol and sodium metabisulfite into the concentrated solution, adjusting pH to 5.0-6.0, stirring, and filtering to obtain flos Camelliae Japonicae extract.
In one embodiment, in step S1, the camellia powder has a particle size of 80 mesh, and the ratio of the camellia powder to ethanol having a concentration of 80-90wt% is 1: (0.5-1).
In one embodiment, in step S2, the deionized water is used in an amount of 10 times the weight of the camellia powder, and the mixed enzyme is used in an amount of 0.5% by weight of the camellia powder.
In one embodiment, the mixed enzyme is composed of glucosidase, arabinosidase and galactosidase, and the weight ratio of the mixed enzyme to the arabinosidase is 2-3:1-2:1-2.
In one embodiment, the deionized water is at a temperature of 40-50 ℃ and the pH is adjusted to 8-9 with arginine.
In one embodiment, in step S4, the mass ratio of the concentrated solution, water, polyol, sodium metabisulfite is 5-10: 15-25: 70-80: 0.03-0.05, wherein the total weight of the extract is 10 times of the weight of the camellia powder.
In one embodiment, the polyol is one or more of glycerol, butanediol, and propylene glycol.
The second object of the present invention is to provide a camellia extract prepared by the above preparation method.
In one embodiment, the camellia extract has a flavone content of > 5mg/mL, a polyphenol content of > 5mg/mL, and a saponin content of < 0.1mg/mL.
The third object of the invention is to provide the application of the camellia extract in preparing skin care products with relieving effect. Typically the cosmetic comprises the camellia extract described above and additives which may comprise any one or more of a combination of surfactants, thickeners, conditioning agents, humectants, preservatives, chelating agents, fragrances and water.
In one embodiment, the skin care product is: spray, essence, skin care cream/cream, or mask.
Compared with the prior art, the invention has the following beneficial effects:
the camellia extract is prepared efficiently by the extraction process of low-pressure internal boiling combined enzymolysis, has high flavone and polyphenol content and low saponin content, and the relief efficacy of the camellia extract is obviously enhanced due to the specific composition of the three active substances. The whole operation process is simple and feasible, the period is short, and the extraction efficiency of the active ingredients is high. Only the solvents with high safety such as ethanol, water, polyalcohol and the like are used; the temperature in the extraction process is low, the energy consumption is low, and the heat-sensitive substance loss is reduced; in addition, after removing the saponin, the camellia extract has good inhibition effect on hyaluronidase, inflammatory factors TNF-alpha and IL-6, and can be used for relieving effect in cosmetics.
Detailed Description
The first object of the present invention is to provide a preparation method of camellia extract with soothing effect, comprising the following steps:
s1, desorption: adding 80-90% ethanol into flos Camelliae Japonicae powder, and desorbing at normal temperature.
Camellia japonica (Camellia japonica L.) is a plant belonging to the genus Camellia of the family Theaceae, and is originally produced in China, and is also called camellia, microcystis, camellia, winter resistance, etc. Warm, moist and semi-yin environment is preferred, and the people are afraid of high temperature and are prohibited from burning sun. There is a distribution in the northwest of Yunnan to the west of Guizhou, in the middle of Sichuan, in the northwest of Hunan and in the northwest of Guangxi. The camellia is rich in various bioactive components such as protein, amino acid, saponin, reducing sugar, polysaccharide, polyphenol, flavone, anthocyanin, vitamin and the like, is an important efficacy additive in cosmetics and daily chemical products, and has the skin care effects of relieving, whitening, resisting oxidation, resisting aging, moisturizing and the like.
Camellia japonica are various, and the color is white or red and sometimes yellow.
The extract according to the invention is obtained from camellia, preferably from white camellia of china. Preferably, the camellia used in the present invention grows in Shandong China.
The camellia powder is preferably in the form of a dispersible powder. For example, fresh camellia flowers are first separated from the stems, then opened and laid flat on a shelf. They are then dehydrated under mild conditions, either in the absence of light at room temperature or in a through-air dryer at a temperature below 35 ℃. The flowers are preferably dried until a solids content of more than 80%, preferably more than 85% is obtained.
The flowers are then reduced to a dispersible powder by any milling method generally known to those skilled in the art, for example in a cutting mill at room temperature, or according to a preferred embodiment by cryogenic milling. For cryogenic milling, the flowers are preferably cooled to-80 ℃ in a closed thermostatically controlled enclosure and immediately milled in a propeller mixer at a temperature of-20 to-80 ℃ to obtain a fine and regular powder. The frozen preservation advantageously makes it possible to ensure an efficient grinding, to obtain a homogeneous powder, to limit the coloration of the powder and to ensure better preservation of the soothing properties of the molecules contained in the flowers.
The high-concentration ethanol is adopted for normal temperature desorption, the high-concentration ethanol has good permeation effect, is beneficial to convection of internal and external substances in the subsequent internal boiling extraction process, improves the extraction efficiency, and can also reserve the active ingredients of camellia pollen to the greatest extent.
For extraction efficiency and economy, the camellia powder is usually crushed to 80 meshes, and desorption time is controlled to be 20-30min.
S2, extracting: heating the camellia feed liquid desorbed at normal temperature in water bath at 40-50deg.C under vacuum degree of-0.1 Mpa to-0.08 Mpa, rapidly adding deionized water and mixed enzyme after slight boiling of the surface, and extracting at vacuum degree and temperature; the mixed enzymes include glucosidase, arabinosidase and galactosidase.
The working principle of the decompression internal boiling extraction technology is that vacuum decompression is adopted to reduce the internal pressure of an extraction container, thereby reducing the boiling point of a solution, enabling a material to be rapidly and effectively extracted under low-temperature boiling, avoiding the thermal decomposition, oxidization, polymerization and the like of active ingredients, and being particularly suitable for extracting the active ingredients with heat sensitivity, instability, easy oxidization and the like. In the step, the extraction is carried out by low-pressure internal boiling combined enzymolysis, so that active ingredients can be effectively reserved, and saponin ingredients can be removed.
The light boiling means a state in which bubbles appear in the liquid, and the bubbles are continuously generated and continuously rise, but are not severe.
The extraction process of the low-pressure internal boiling combined enzymolysis in the step is used for efficiently preparing the camellia extract, and the camellia extract has high flavone and polyphenol content and low saponin content.
S3, concentrating: and (2) after the extracting solution in the step (S2) is cooled to room temperature, adding ethanol while stirring until the ethanol concentration in the final solution reaches 75-80wt%, and then stirring, standing and filtering to obtain a concentrated solution.
The stirring speed is preferably 30-40r/min.
S4, preparing: adding water, polyalcohol and sodium metabisulfite into the concentrated solution, adjusting pH to 5.0-6.0 with citric acid, stirring, and filtering to obtain flos Camelliae Japonicae extract.
Preferably, the mass ratio of the concentrated solution to the water to the polyalcohol to the sodium metabisulfite in the camellia extract is 5-10: 15-25: 70-80: 0.03-0.05, wherein the total weight of the obtained extract is 10 times of the weight of the camellia powder.
The second object of the present invention is to provide a camellia extract prepared by the above preparation method.
Preferably, the flavone content in the camellia extract is more than 5mg/mL, the polyphenol content is more than 5mg/mL, and the saponin content is less than 0.1mg/mL.
The third object of the invention is to provide the application of the camellia extract in preparing skin care products with relieving effect. The skin care product can be spray, essence, skin care cream/cream, facial mask, etc.
Typically the skin care product will comprise the camellia extract described above and additives which may comprise any one or more of surfactants, thickeners, conditioning agents, humectants, preservatives, chelating agents, fragrances and water in combination.
In order that the invention may be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments that are illustrated in the appended drawings. Preferred embodiments of the present invention are given in the examples. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The camellia used in the following examples and comparative examples were produced in Shandong, and glucosidase, arabinosidase, galactosidase were purchased from Shanghai Michelia Biochemical technologies Co., ltd, and the other reagents used were all commercially available; the methods used in the following examples and comparative examples, unless otherwise specified, were all carried out by conventional methods.
The percentages stated in the examples and comparative examples below, for example without any specific meaning, are percentages by weight.
Example 1
(1) And (3) desorption: 10g of dried camellia is crushed to 80 meshes, then added into a round bottom distillation flask, and ethanol with the concentration of 80% is added according to the feed liquid ratio of 1:1 for desorption at normal temperature for 20min.
(2) Extracting: heating round bottom distillation flask in 50deg.C water bath, vacuumizing to-0.1 Mpa, rapidly adding deionized water (pH is adjusted to 8.1 with arginine) at 50deg.C and mixed enzyme (wherein glucosidase 0.3%, arabinosidase 0.1%, galactosidase 0.1% based on weight of camellia powder) at 50deg.C by 10 times of the weight of the materials, and extracting at vacuum and temperature for 25min.
(3) Concentrating: after cooling, stirring the mixed solution at 40r/min, slowly adding 95% ethanol until the ethanol concentration in the final solution reaches 75%, stirring for 20min, standing for 1h, filtering, and concentrating the filtrate to 5g.
(4) Preparing: adding glycerol and sodium metabisulfite into the concentrated solution, regulating pH to 5.4 with citric acid, and filtering to obtain 100g of camellia extract, which comprises 5% camellia concentrated solution, 20% water, 74.95% glycerol and 0.05% sodium metabisulfite.
Example 2
(1) And (3) desorption: 10g of dried camellia is crushed to 80 meshes, then added into a round bottom distillation flask, and ethanol with the concentration of 85% is added according to the feed-liquid ratio of 1:0.5 for desorption at normal temperature for 25min.
(2) Extracting: heating round bottom distillation flask in 50deg.C water bath, vacuumizing to-0.09 Mpa, rapidly adding deionized water (pH is adjusted to 8.4 with arginine) at 50deg.C and mixed enzyme (wherein glucosidase 0.2%, arabinosidase 0.2%, galactosidase 0.1% based on weight of camellia powder) at 50deg.C by 10 times of the weight of the materials, and extracting at vacuum and temperature for 30min.
(3) Concentrating: after cooling to room temperature, stirring the mixed solution at 40r/min, slowly adding 95% ethanol until the ethanol concentration in the final solution reaches 75%, stirring for 20min, standing for 1h, filtering, and concentrating the filtrate to 8g.
(4) Adding propylene glycol and sodium metabisulfite into the concentrated solution, regulating the pH to 5.6 by using citric acid, and filtering to obtain 100g of camellia extract, wherein the composition of the camellia extract comprises 8% of camellia concentrated solution, 21% of water, 70.97% of propylene glycol and 0.03% of sodium metabisulfite.
Example 3
(1) And (3) desorption: 10g of dried camellia is crushed to 80 meshes, then added into a round bottom distillation flask, and ethanol with the concentration of 90% is added according to the feed liquid ratio of 1:0.8 for desorption at normal temperature for 20min.
(2) Extracting: heating round bottom distillation flask in 50deg.C water bath, vacuumizing to-0.08 Mpa, rapidly adding deionized water (pH is adjusted to 8.2 with arginine) at 50deg.C and mixed enzyme (wherein glucosidase 0.2%, arabinosidase 0.1%, galactosidase 0.2% based on weight of camellia powder) at 50deg.C by 10 times of the weight of the materials, and extracting at vacuum and temperature for 28min.
(3) Concentrating: after cooling to room temperature, stirring the mixed solution at 35r/min, slowly adding 95% ethanol until the ethanol concentration in the final solution reaches 78%, stirring for 20min, standing for 1h, filtering, and concentrating the filtrate to 10g.
(4) Preparing: adding butanediol and sodium metabisulfite into the concentrated solution, regulating pH to 5.3 with citric acid, and filtering to obtain 100g of camellia extract, which comprises 10% camellia concentrated solution, 15% water, 74.95% butanediol and 0.05% sodium metabisulfite.
Example 4
(1) And (3) desorption: 10g of dried camellia is crushed to 80 meshes, then added into a round bottom distillation flask, and ethanol with the concentration of 85% is added according to the feed-liquid ratio of 1:0.5 for desorption for 30min at normal temperature.
(2) Extracting: heating the round bottom distillation flask in 45deg.C water bath, vacuumizing to-0.09 Mpa, boiling the surface, rapidly adding deionized water (pH is adjusted to 8.5 with arginine) at 45deg.C, and extracting for 20min.
(3) Concentrating: after cooling to room temperature, stirring the mixed solution at 30r/min, slowly adding 95% ethanol until the ethanol concentration in the final solution reaches 80%, stirring for 25min, standing for 1h, filtering, and concentrating the filtrate to 5g.
(4) Preparing: adding water, glycerol, propylene glycol and sodium metabisulfite into the concentrated solution, regulating the pH to 6.0 by using citric acid, and filtering to obtain 100g of camellia extract, wherein the composition of the camellia extract comprises 5% of camellia concentrated solution, 20% of water, 54.95% of glycerol, 20% of propylene glycol and 0.05% of sodium metabisulfite.
Example 5
(1) And (3) desorption: 10g of dried camellia is crushed to 80 meshes, then added into a round bottom distillation flask, and ethanol with the concentration of 80% is added according to the feed liquid ratio of 1:1 for desorption for 30min at normal temperature.
(2) Extracting: heating round bottom distillation flask in water bath at 48deg.C, vacuumizing to-0.1 Mpa, rapidly adding deionized water (pH is adjusted to 9 with arginine) at 48deg.C by 10 times of the weight of the materials to be extracted after slight boiling, mixing enzyme (0.3% glucosidase, 0.1% arabinosidase and 0.1% galactosidase) with 0.5% camellia powder weight, maintaining vacuum degree and temperature, and extracting for 30min.
(3) Concentrating: after cooling, stirring the mixed solution at 35r/min, slowly adding 95% ethanol until the ethanol concentration in the final solution reaches 80%, stirring for 25min, standing for 1h, filtering, and concentrating the filtrate to 8g.
(4) Preparing: adding water, butanediol, propylene glycol and sodium metabisulfite into the concentrated solution, regulating the pH to 5.0 by using citric acid, and filtering to obtain 100g of camellia extract, wherein the composition of the camellia extract comprises 8% of camellia concentrated solution, 20% of water, 50.95% of butanediol, 21% of propylene glycol and 0.05% of sodium metabisulfite.
Example 6
(1) And (3) desorption: 10g of dried camellia is crushed to 80 meshes, then added into a round bottom distillation flask, and ethanol with the concentration of 90% is added according to the feed liquid ratio of 1:0.8 for desorption at normal temperature for 25min.
(2) Extracting: heating the round bottom distillation flask in 40deg.C water bath, vacuumizing to-0.08 Mpa, boiling slightly, rapidly adding deionized water (pH is adjusted to 8 with arginine) at 40deg.C, and extracting for 20min under vacuum and temperature conditions with mixed enzyme (0.3% glucosidase, 0.1% arabinosidase and 0.1% galactosidase) accounting for 0.5% of the weight of camellia powder.
(3) Concentrating: after cooling to room temperature, stirring the mixed solution at 30r/min, slowly adding 95% ethanol until the ethanol concentration in the final solution reaches 78%, stirring for 30min, standing for 1h, filtering, and concentrating the filtrate to 10g.
(4) Preparing: adding water, propylene glycol and sodium metabisulfite into the concentrated solution, regulating the pH to 6.0 by using citric acid, and filtering to obtain 100g of camellia extract, wherein the composition of the camellia extract comprises 10% of camellia concentrated solution, 19% of water, 70.95% of propylene glycol and 0.05% of sodium metabisulfite.
Example 7
(1) And (3) desorption: 10g of dried camellia is crushed to 80 meshes, then added into a round bottom distillation flask, and ethanol with the concentration of 87% is added according to the feed liquid ratio of 1:0.7 for desorption at normal temperature for 20min.
(2) Extracting: heating the round bottom distillation flask in 45deg.C water bath, vacuumizing to-0.08 Mpa, rapidly adding deionized water (pH is adjusted to 8.2 with arginine) at 45deg.C by 10 times of the weight of the materials to be extracted after slight boiling of the surface, mixing enzyme (0.3% glucosidase, 0.1% arabinosidase and 0.1% galactosidase) with 0.5% camellia powder weight, maintaining vacuum degree and temperature, and extracting for 22min.
(3) Concentrating: after cooling to room temperature, stirring the mixed solution at 40r/min, slowly adding 95% ethanol until the ethanol concentration in the final solution reaches 75%, stirring for 30min, standing for 1h, filtering, and concentrating the filtrate to 7g.
(4) Preparing: adding water, butanediol and sodium metabisulfite into the concentrated solution, regulating pH to 5.7 with citric acid, and filtering to obtain 100g of camellia extract, wherein the composition of the camellia extract comprises 7% of camellia concentrated solution, 18% of water, 74.97% of butanediol and 0.03% of sodium metabisulfite.
Example 8
(1) And (3) desorption: 10g of dried camellia is crushed to 80 meshes, then added into a round bottom distillation flask, and ethanol with the concentration of 83% is added according to the feed liquid ratio of 1:0.6 for desorption for 30min at normal temperature.
(2) Extracting: heating round bottom distillation flask in water bath at 47 deg.C, vacuumizing to-0.09 Mpa, rapidly adding deionized water (pH is adjusted to 8.7 with arginine) at 47 deg.C by 10 times of the weight of the materials to be extracted after slight boiling of the surface, mixing enzyme (0.3% glucosidase, 0.1% arabinosidase and 0.1% galactosidase) with 0.5% camellia powder weight, maintaining vacuum degree and temperature, and extracting for 28min.
(3) Concentrating: after cooling, stirring the mixed solution at 30r/min, slowly adding 95% ethanol until the ethanol concentration in the final solution reaches 80%, stirring for 25min, standing for 1h, filtering, and concentrating the filtrate to 8g.
(4) Preparing: adding water, glycerol, butanediol and sodium metabisulfite into the concentrated solution, regulating pH to 5.5 with citric acid, and filtering to obtain 100g of camellia extract, wherein the composition of the camellia extract comprises 8% of camellia concentrated solution, 18% of water, 35% of glycerol, 38.97% of butanediol and 0.03% of sodium metabisulfite.
Comparative example 1
The difference from example 1 is that the internal boiling process is eliminated, and the extraction process uses a conventional solvent combined enzyme extraction process, specifically:
(1) Extracting: 10g of dried camellia is crushed to 80 meshes, added into a round bottom distillation flask, deionized water (pH is adjusted to 8.1 by arginine in advance) with the weight of the extracted material being 10 times and 50 ℃ is added, mixed enzyme (wherein, 0.3 percent of glucosidase, 0.1 percent of arabinosidase and 0.1 percent of galactosidase are calculated according to the weight of the camellia powder) with the weight of 0.5 percent of camellia powder is added, and the mixture is stirred and extracted for 25 minutes under the conditions of vacuum degree of-0.1 Mpa and 50 ℃.
(2) Concentrating: after cooling to room temperature, stirring the mixed solution at 40r/min, slowly adding 95% ethanol until the ethanol concentration in the final solution reaches 75%, stirring for 20min, standing for 1h, filtering, and concentrating the filtrate to 5g.
(3) Preparing: adding glycerol and sodium metabisulfite into the concentrated solution, regulating pH to 5.4 with citric acid, and filtering to obtain 100g of camellia extract, which comprises 5% camellia concentrated solution, 20% water, 74.95% glycerol and 0.05% sodium metabisulfite.
Comparative example 2
The difference is that the inactivated mixed enzyme is added in the step (2) as in the example 1, and other conditions are not changed.
Comparative example 3
(1) And (3) desorption: 10g of dried camellia is crushed to 80 meshes, then added into a round bottom distillation flask, and ethanol with the concentration of 50% is added according to the feed liquid ratio of 1:1 for desorption at normal temperature for 20min.
(2) Extracting: heating round bottom distillation flask in 50deg.C water bath, vacuumizing to-0.12 Mpa, rapidly adding deionized water (pH is adjusted to 8.1 with arginine) at 50deg.C and mixed enzyme (wherein glucosidase 0.3%, arabinosidase 0.1%, galactosidase 0.1% based on weight of camellia powder) at 50deg.C by 10 times of the weight of the materials, and extracting at vacuum and temperature for 25min.
(3) Concentrating: after cooling to room temperature, stirring the mixed solution at 40r/min, slowly adding 95% ethanol until the ethanol concentration in the final solution reaches 75%, stirring for 20min, standing for 1h, filtering, and concentrating the filtrate to 5g.
(4) Adding glycerol and sodium metabisulfite into the concentrated solution, regulating pH to 5.4 with citric acid, and filtering to obtain 100g of camellia extract, wherein the composition of the camellia extract comprises 5% camellia concentrated solution, 20% water, 74.95% glycerol and 0.05% sodium metabisulfite.
Comparative example 4
A camellia extract is prepared from commercially available camellia total flavonoids and camellia polyphenols to obtain a solution with total flavonoids content of 6.17mg/mL and polyphenol content of 6.02mg/mL, and the solvent is the same glycerol aqueous solution as the camellia extract described in example 1.
Comparative example 5
A camellia extract is prepared from commercially available camellia total flavone powder in a solution with total flavone content of 12.19mg/mL, and the solvent is the same glycerol aqueous solution as the camellia extract described in example 1.
Comparative example 6
A camellia extract was prepared from commercially available camellia polyphenol powder to obtain a solution with a polyphenol content of 12.19mg/mL, and the solvent was the same aqueous glycerol solution as that of the camellia extract described in example 1.
Comparative example 7
A flos Camelliae Japonicae extract is prepared from commercially available total flavonoids of flos Camelliae Japonicae, polyphenols of flos Camelliae Japonicae, and saponins of flos Camelliae Japonicae into solution with flavone content of 6.17mg/mL, polyphenols content of 6.02mg/mL, and saponins content of 2.50 mg/mL, and the solvent is glycerol aqueous solution identical to that of flos Camelliae Japonicae extract described in example 1.
Test example 1: active content detection
Testing the total flavone content of the samples of examples 1-8 and comparative examples 1-3 by referring to DB 34/T2743-2016 method prescribed by spectrophotometry for determining total flavone content in flos Sophorae Immaturus and its products; the samples of examples 1 to 8 and comparative examples 1 to 3 were tested for total saponins with reference to T/GDFDTAEC 03-2022 determination of total saponins in health food-spectrophotometry.
TABLE 1 detection of the content of active substances in camellia extract
Analysis of results: the total flavone and polyphenol contents of the camellia extract obtained by the embodiment of the invention are more than 5mg/mL, which is obviously higher than that of the comparative example; the total saponin content is less than 0.1mg/mL, which is significantly lower than that of the comparative example. The preparation process of the invention has great influence on the content of active substances. The invention adopts the extraction technology of low-pressure internal boiling combined enzymolysis, combines the selection of the extracting solution, the control of the proportion of the feed liquid and the synergistic effect, and can efficiently prepare the camellia extract with high flavone and polyphenol content and low saponin content.
Test example 2: test of soothing efficacy
1. Hyaluronidase activity inhibition rate
The camellia extracts obtained in examples 1 to 8 and comparative examples 1 to 4 were diluted with pure water, respectively, to give: 20 Three samples with different concentrations of mg/mL, 50 mg/mL and 100mg/mL were tested for inhibition of hyaluronidase activity by the method of reference "study of anti-allergic and antipruritic efficacy of Shumin formula extract", and the results are shown in Table 2.
TABLE 2 inhibition of hyaluronidase Activity by camellia extract (unit:%)
Analysis of results: the inhibition rate of the hyaluronidase activity of the examples 1-8 under different concentrations is obviously better than that of the comparative examples 1-3, which proves that the camellia extract prepared by the process has good relieving effect; meanwhile, as can be seen from example 1 and comparative examples 4-6, the camellia polyphenol and flavone can synergistically increase the soothing effect, and the soothing effect of the camellia extract of example 1 is stronger than that of comparative example 4, which shows that the soothing effect of the extract obtained by the preparation process of the invention is better than that of a sample of simply compounded camellia flavone and polyphenol; from comparative examples 4 and 7, it is known that saponins significantly reduce the soothing efficacy.
2. RAW264.7 mouse macrophage inflammatory factor TNF-a and IL-6 secretion inhibition
Referring to the method in screening of plant source soothing active substances and Activity study, the camellia extract of examples 1-8 and comparative examples 1-7 with concentration of 100mg/mL was tested for the effect on the macrophage viability of RAW264.7 mice, and cell viability was found to be higher than 90%, indicating that the concentration was safe. The subsequent test samples showed inhibitory effects on the secretion of inflammatory factors TNF-a and IL-6 from RAW264.7 mouse macrophages, and the results are shown in Table 3.
TABLE 3 RAW264.7 inhibition of macrophage inflammatory factor TNF-a and IL-6 secretion by mice
Analysis of results: 100mg/mL of examples 1-8 had higher anti-inflammatory effects than comparative examples 1-7, and comparative example 4 had better anti-inflammatory effects than other comparative examples, indicating that the flavones and polyphenols of the camellia extract synergistically increased the anti-inflammatory effects, and comparative example 4 had better anti-inflammatory effects than comparative example 7, indicating that the anti-inflammatory effects of the camellia extract with saponins were reduced.
3. Camellia soothing spray human body efficacy test
The camellia soothing spray was prepared according to the amounts of the raw materials shown in the following table.
Table 4 camellia soothing spray formulation
Test scheme:
selecting at least 20 healthy Chinese subjects, and screening sensitive skin subjects through lactic acid stinging experiments.
Lactic acid stinging experiment: the test was performed by selecting the nasolabial folds on one side of the subjects according to a random table at room temperature, dropping 50uL of a 10% lactic acid solution 1cm X2 cm of cosmetic cotton using a pipette, and applying the solution to the nasolabial folds to inquire about subjective symptoms of the subjects at 2.5min and 5.0min, and scoring the test according to a score of 4 (0 is no tingling sensation, 1 is light tingling, 2 is medium tingling, and 3 is heavy tingling). The scores were then added together and the total score >3 was positive for lactic acid stinging response.
The clinical symptoms (e.g., stinging, itching, burning, redness, dryness) of the subjects were scored by trained professionals or dermatologists at each visit point (0 for no response, 1 for mild, 2 for moderate, 3 for heavy) by the lactic acid stinging-screened sensitive muscle subjects for 28 days continuously using camellia spray samples.
Test results:
through evaluation analysis, 20 subjects were 10% lactic acid stinging positive (table 5), and the evaluation results were effective examples.
TABLE 5 10% lactic acid stinging positive assessment
After using the test product, the experimental results of the facial skin sensitivity are shown in the following table (table 6):
TABLE 6 differential analysis of skin sensitivity
Experimental results show that after the spray for relieving the camellia oleifera flowers is continuously used for 28 days, the skin sensitive stimulation state can be obviously improved, and clinical symptoms such as skin stinging, itching, burning, redness, dryness and the like are obviously improved, so that the camellia oleifera extract has the relieving effect.
In summary, the preparation method of the camellia extract adopts the extraction process of low-pressure internal boiling combined enzymolysis, has synergistic effect, combines the selection of the extracting solution, controls the proportion of the extracting solution and the like, has simple and easy operation process, short period, low temperature in the extraction process, less loss and less organic solvent, can comprehensively degrade camellia powder, extract various bioactive components in the camellia powder, efficiently prepare the camellia extract, has high flavone and polyphenol content and low saponin content, obviously improves the inhibition effect on hyaluronidase, inflammatory factors TNF-alpha and IL-6, and has obvious relieving effect when being applied to skin care products.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (5)
1. A method for preparing camellia extract with soothing effect, which is characterized by comprising the following steps:
s1, desorption: adding 80-90wt% ethanol into flos Camelliae Japonicae powder, and desorbing at normal temperature;
s2, extracting: heating the camellia feed liquid desorbed at normal temperature in water bath at 40-50deg.C under vacuum degree of-0.1 Mpa to-0.08 Mpa, rapidly adding deionized water and mixed enzyme after slight boiling of the surface, and extracting at vacuum degree and temperature; the mixed enzyme comprises glucosidase, arabinosidase and galactosidase;
s3, concentrating: after the extracting solution in the step S2 is cooled to room temperature, adding ethanol while stirring until the ethanol concentration in the final solution reaches 75-80wt%, stirring, standing, filtering, concentrating the filtrate, and recovering ethanol to obtain a concentrated solution;
s4, preparing: adding water, polyalcohol and sodium metabisulfite into the concentrated solution, adjusting pH to 5.0-6.0, stirring, and filtering to obtain flos Camelliae Japonicae extract;
in the step S1, the granularity of the camellia powder is 80 meshes, and the feed liquid ratio of the camellia powder to the ethanol with the concentration of 80-90wt% is 1:0.5-1;
in the step S2, the dosage of the deionized water is 10 times of the weight of the camellia powder, and the dosage of the mixed enzyme is 0.5% of the weight of the camellia powder;
the weight ratio of the glucosidase, arabinosidase and galactosidase in the mixed enzyme is 2-3: 1-2: 1-2;
the deionized water temperature is 40-50 ℃, and arginine is used for regulating the pH value to 8-9;
in the step S4, the mass ratio of the concentrated solution to the water to the polyol to the sodium metabisulfite is 5-10 respectively: 15-25: 70-80: 0.03-0.05, wherein the total weight of the extract is 10 times of the weight of the camellia powder.
2. A camellia extract obtained by the process of claim 1.
3. The camellia extract of claim 2, wherein the camellia extract has a flavone content of > 5mg/mL, a polyphenol content of > 5mg/mL, and a saponin content of < 0.1mg/mL.
4. Use of a camellia extract as claimed in claim 2 or 3 for the preparation of a skin care product with soothing effect.
5. The use according to claim 4, wherein the skin care product is: spray, essence, skin care cream/cream, or mask.
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