CN109512756B - Method for extracting plant material for cosmetic additive and extract - Google Patents
Method for extracting plant material for cosmetic additive and extract Download PDFInfo
- Publication number
- CN109512756B CN109512756B CN201711194829.XA CN201711194829A CN109512756B CN 109512756 B CN109512756 B CN 109512756B CN 201711194829 A CN201711194829 A CN 201711194829A CN 109512756 B CN109512756 B CN 109512756B
- Authority
- CN
- China
- Prior art keywords
- extracting
- solvent
- cosmetic
- extraction
- plant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
-
- 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
- A61K2800/80—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
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Dermatology (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a preparation method of a plant extract for cosmetic addition, which comprises the following specific steps: (1) extracting for the first time: selecting plant raw materials, mixing the raw materials and a first solvent according to a material-liquid ratio of 1: 10-100 m/m, and extracting for 0.5-2 h at 40-90 ℃; (2) and (3) second extraction: adding a second solvent according to the feed-liquid ratio of 1: 10-100 m/m, and extracting for 0.5-2 h at 40-90 ℃; (3) removing the first solvent; (4) fine filtering to obtain clear extract; the first solvent is one or a mixture of ethanol, chloroform and acetone; the second solvent is one or more of white oil, hydrogenated polyisobutene, hydrogenated polydecene, caprylic/capric triglyceride, isostearyl isostearate and vegetable oil. The method has higher extraction efficiency and lower extraction cost, and is more suitable for large-scale industrial production.
Description
Technical Field
The invention relates to a preparation method of a plant extract, in particular to a preparation method of a plant extract suitable for industrial production and used for cosmetic addition and the extract prepared by the method.
Background
Plant extracts have many advantages as cosmetic additives, such as natural components, low irritation, excellent efficacy, etc., and thus, the use of plant extracts as efficacy additives in cosmetics is increasing. The effective components of the plant material include oil-soluble components such as fatty acid, sterol, lignan, esters, polyene, pyrrole derivatives, ketones, quinones, etc., and some non-oil-soluble substances such as saccharides, amino acids, proteins, etc. The current main reasons for the application of plant extracts in the cosmetic field are (1) too low extraction efficiency, and the increase of extraction cost is caused by too low extraction effect due to the characteristics of plant raw materials, so that many enterprises preferentially select low-cost synthetic chemical raw materials to replace natural plant raw materials so as to increase economic benefit. (2) The stability of the plant material extract is poor. Plant raw materials are often not good in stability in various dosage forms of the added and evolved cosmetics, and are easy to deteriorate, separate out or precipitate in the storage and transportation processes, so that the product spoilage is increased, the cost is increased, the effect is directly influenced, and the use experience of consumers is reduced. In particular, for oil type cosmetics, the oil type cosmetics have extremely high requirements on clarity, and once slight precipitation and precipitation occur, the quality and the performance of the product can be influenced. Therefore, a plant extract preparation process which is suitable for industrial production and has high extraction rate and good extract stability is urgently needed by cosmetic enterprises at present.
The extraction method of the functional components of the existing plant raw materials is introduced as follows, and the existing preparation process comprises the following steps:
1. soaking and extracting
The flower and plant soaking oil has a long history of application, and ancient Egyptics and ancient Hispanics have learned to absorb the odor of petals and herbs with oil and fat for use as medicines or cosmetics. The soaking oil is usually vegetable oil as a solvent, the ratio of the raw materials to the oil is about 1:3(v/v), the soaking is carried out at normal temperature, the materials need to be repeatedly fed for 2-3 times, and the soaking time needs to be 1-3 months. The method has low extraction efficiency, high cost, and long extraction time, and is not suitable for industrial production.
2. Direct high-temperature extraction of oil
Ancient books such as Puji prescription and Taiping Shenghui prescription record a lot of ointments, which are prepared by frying Chinese herbs with oil and fat to remove dregs, and are used for treating skin diseases or beautifying. Until now, folk still keep many prescriptions and proved prescriptions, and sesame oil is heated and decocted in the traditional Chinese medicine to obtain medicinal oil for relieving various uncomfortable symptoms of skin. Therefore, direct high-temperature decoction by using oil is one of the traditional extraction methods, but the method is more original, has low extraction efficiency, can not effectively extract active ingredients in plants, has long time consumption, serious material waste, low extraction efficiency and the like, and seriously restricts industrial production.
3. Steam distillation process
Steam distillation is a common method for extracting plant essential oil, but the method is only suitable for extracting volatile components of aromatic substances in plants, and the nonvolatile components cannot be extracted and utilized.
4. Solvent extraction
Solvent extraction is a common method for producing plant extracts, generally takes ethanol, acetone, chloroform and the like as solvents, and has the characteristics of simple equipment, high extraction rate and the like. However, the extract prepared by the method has higher requirements on the formulation of cosmetics, is not suitable for being added into all formulations, and particularly has poor solubility in oil-type cosmetics, so that the plant extract can be precipitated after being added into the pure oil-type cosmetics, the product quality is seriously influenced, and the application of the plant extract in the pure oil-type cosmetics is restricted.
5. Supercritical extraction
Supercritical extraction is a new technique which has been developed in recent years, and supercritical fluid, generally supercritical CO, is used for extracting solvent2Has the advantages of no toxicity, no harm, high extraction rate, high extract purity and the like. But the equipment is complex, the input cost is high, the extraction cost is high, and the industrialized mass production is limited. And the compatibility of the extract obtained by supercritical extraction with oil is poor, so that the application of the extract in oil type cosmetics is influenced.
The existing method has a plurality of defects, and simultaneously, the problems of high preparation cost, environmental pollution caused by organic solvent discharge and the like are gradually highlighted due to the limitation of extraction efficiency. Therefore, there is a great need in the art to solve the above-mentioned problems in the preparation of plant extracts for the addition of cosmetic and care products.
Disclosure of Invention
The invention aims to improve the defects of the prior art, and provides a plant raw material extraction method which is suitable for industrial production, low in cost, high in extraction efficiency, more importantly suitable for various cosmetic formulations, stable in product performance after being added and good in compatibility.
The second purpose of the invention is to provide an extract prepared by the method.
The third purpose of the invention is to provide a new application of the extract.
The fourth object of the present invention is to provide a cosmetic containing the above extract.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a plant extract for cosmetic addition, wherein the preparation method comprises the following steps:
(1) extracting for the first time: weighing plant raw materials, mixing the raw materials and a first solvent according to the feed liquid mass ratio of 1: 10-100 m/m, and extracting for 0.5-2 h at the temperature of 40-90 ℃;
the first solvent used in the invention is one or a mixture of ethanol, chloroform and acetone.
The feed-liquid ratio and the extraction temperature have a crucial influence on the extraction efficiency and the extraction cost, and the feed-liquid ratio and the extraction parameters which are more matched with the physicochemical properties of the first extraction solvent can be selected according to the physicochemical properties of the first extraction solvent, so that the extraction efficiency can be improved, and the cooperativity with the next extraction solvent can be enhanced. The plant raw material and the solvent are contacted more fully in the feed liquid ratio range, the active ingredients in the plant raw material are easier to extract, the extraction efficiency is higher, meanwhile, the waste of the solvent and the plant raw material is not caused, and the extraction cost is more economic. The preferable range of the ratio of the first extraction material to the liquid is 1: 10-50 m/m, the extraction effect is better in the range, and the cooperativity with the solvent II is stronger.
The extraction temperature and the extraction time are preferably 40-90 ℃ for 0.5-2 h. The extraction temperature and time directly influence the property of the extract, and improper extraction temperature and time can cause oxidative denaturation of plant raw materials, loss of volatile components, change of the property of thermosensitive components and the like in the extraction process, so that the solubility and the material exchange rate of the effective components of the extract in a solvent are optimal, and the effect of the extract is excellent and stable.
The condition parameters of the step (1) are more suitable for matching with the step (2) and can generate synergistic effect with the step (2).
(2) And (3) second extraction: adding a second solvent according to the feed-liquid ratio of 1: 10-100 m/m, and extracting for 0.5-2 h at 40-90 ℃;
the second solvent used in the invention is one or a mixture of more of the following raw materials: white oil with kinematic viscosity (40 ℃) less than or equal to 30cSt, and white oils 3#, 5#, 7#, 10#, 15#, and 26# are recommended; hydrogenated polyisobutene having a kinematic viscosity (40 ℃) of less than or equal to 30cSt, preferably hydrogenated polyisobutene Parleam 6, Parleam EX; hydrogenated polydecene with a kinematic viscosity (40 ℃) of less than or equal to 30cSt, preferably PAO2, PAO4 and PAO 6; caprylic/capric triglyceride, isostearyl isostearate and vegetable oil. The vegetable oil is preferably soybean oil, sunflower seed oil, sesame oil, macadamia nut oil, sweet almond oil, olive oil, grape seed oil, oat oil, or tea oil.
The combination of the second solvent and the first solvent is particularly important for the technical effect of the invention, and the inventor verifies through experiments that the two solvents cannot be completely dissolved with each other, and the complete dissolution can ensure better extraction efficiency, but the added product has poor stability and is easy to have adverse conditions such as precipitation and the like. The two solvents cannot be completely immiscible, and the immiscible solvents cannot play a role in synergy, so that the extraction efficiency is very low and the stability of the extract is poor. Therefore, the mutual dissolution technical effect of the first solvent and the second solvent is optimal, in order to ensure that the extraction cost is more economic due to the higher extraction efficiency of the two solvents, the temperature and the time of the second extraction are controlled within the condition parameter range, the extraction effect of the mutual dissolution and the common extraction of the first solvent and the second solvent can be simultaneously improved, and the problems that the extraction efficiency tends to slowly increase the extraction cost and the like can be effectively avoided. According to the characteristics of the second solvent, the extraction temperature is not suitable to be too high, is optimally controlled below 90 ℃, is not too low, and is lower than 40 ℃, so that the solubility of the functional components in the second solvent and the compatibility of the first solvent and the second solvent are influenced, and the extraction efficiency is further influenced.
According to the description of the method, the selection of the solvent I and the solvent II is particularly important, the combination of the solvent I and the solvent II needs to be synergistic to improve the extraction efficiency of the plant raw materials, in order to adapt to industrial production, the extraction process needs to be short, the quality of the extract needs to be high, namely the addition stability is good, and the extraction cost also needs to be low. Therefore, the inventor of the present invention has experimentally verified that if the polarity of the solvent of the present invention is greater than that of the solvent one, the extraction efficiency and the stability of the extract are poor. The inventor surprisingly found that if the solvent is more polar than the solvent II, the first solvent and the second solvent can be partially dissolved with each other under certain conditions, which can enhance the solubility of the active ingredient in the second solvent, so that some substances which are originally insoluble in the oil or have poor solubility in the oil can be well dissolved in the second solvent. The two extracts are combined for extraction, so that all conditions required by the extraction of the plant raw materials of the cosmetics can be met, the extraction efficiency of the plant active ingredients is greatly improved, the obtained extract has stable property and excellent compatibility with other raw materials of the cosmetics.
In the invention, one of the solvents can be selected for single solvent extraction, or multiple solvents can be compounded and extracted according to the characteristics of the plant raw materials which are actually extracted, and the compounding ratio among the solvents can be compounded according to the experience of a person skilled in the art or the actual needs in any ratio without specific limitation. Because the second solvent is characterized by the great influence of water on the stability of the second solvent, the first solvent is preferably an anhydrous system, such as ethanol, and is preferably anhydrous ethanol.
The solvent II is an extraction solvent with weaker polarity than the solvent I, is mild and non-irritant, and has good compatibility with functional components in plant raw materials. The second solvent can be one of the solvents mentioned above for single solvent extraction, or can be a multi-solvent compound extraction according to the characteristics of the plant raw material actually extracted, and the compounding ratio between the solvents can be any ratio according to the experience of the person skilled in the art or the actual needs, and is not particularly limited.
The preferable range of the ratio of the second extraction in the step (2) is 1: 10-50 m/m.
(3) Removing the first solvent; the methods for removing the solvent known to those skilled in the art can be applied herein, and the preferred methods proposed in the present invention are: concentrating under reduced pressure at 40-80 deg.C until the solvent is completely removed, wherein the reduced pressure range is generally controlled to 0.01MPa to minus 0.15 MPa. The first solvent may have certain irritation to skin, and the removal of the first solvent can make the product performance milder, safe and has no toxic or side effect. The first solvent can also be removed by membrane concentration, ultrafiltration, reverse osmosis, pervaporation and the like.
(4) Fine filtering to clarify; the purpose of the step is to enable the final extract to be more stable and clear, and a filter plate with the aperture of 0.2-10 mu m is used in the fine filtration process for filtration.
In order to facilitate the steps of reduced pressure concentration and fine filtration and protect reduced pressure concentration and fine filtration equipment better, a coarse filtration step can be added between the step (2) and the step (3), wherein the coarse filtration condition is 60-100 meshes coarse filtration, and raw material residues are filtered. In order to keep the stability of the filtered feed liquid, a cooling step can be added before coarse filtration, and the feed liquid is cooled to 40 ℃ or below 40 ℃ and then coarse filtration is optimally carried out.
The plant material may also be pretreated prior to the first extraction in order to facilitate the penetration of the cell walls by the extraction solvent and to further increase the extraction efficiency. The step of pretreatment is not necessary, the extraction rate of the invention is high and mainly depends on the matching of the first solvent and the second solvent and the process steps and parameters used for the second solvent, the pretreatment can further shorten the extraction time on the basis of the extraction rate achieved by the invention, but the pretreatment step can also not be used for the plant raw materials which are inconvenient to pretreat. The steps of pretreatment recommended by the inventors are as follows, and other steps known to those skilled in the art to achieve the purpose of pretreatment may be applied thereto.
(1) Coarse crushing: crushing the raw materials to 20-60 meshes; the pulverizing step can be performed by pulverizing equipment known in the art, such as a cutting machine, a wall breaking machine, a pulverizer, etc., and can be performed at one time or step by step from coarse to fine.
(2) The high temperature and high pressure treatment is carried out, wherein the high temperature is generally at least equal to or higher than 100 ℃, and the temperature is preferably controlled to be 100-130 ℃. The high pressure is more than 0.1Mpa, and the effect is best when the pressure is controlled within the range of 0.1-0.2 Mpa. The treatment time is not longer, preferably within 30 min. The main components of the plant cell wall are cellulose and pectin, the invention adopts high-temperature and high-pressure pretreatment of raw materials, and water vapor is utilized to destroy hydrogen bonds among polysaccharide molecules, so that the cell wall structure is loose, the solvent can enter through the cell wall in the subsequent extraction process, and the extraction efficiency is better.
(3) Drying, the purpose of drying is to remove redundant water vapor after high temperature and high pressure, the later extraction process is more favorably carried out, the extract is more stable, and the drying is preferably carried out for 1-2 h at the temperature of 50-80 ℃. Other drying means known to those skilled in the art may also be applied here.
The application of the method in preparing oil type cosmetic additive is provided.
An oil-type cosmetic plant extract, which is prepared by the above method.
The plant raw material is not limited by specific varieties, can be a single plant raw material, and can also be a composition compounded by mixing multiple plant raw materials. The known plant materials which can be used for cosmetic additives can be extracted by the method of the invention. Compared with the extraction method in the prior art, the extraction method has the advantages of higher extraction efficiency, more stable extract property and better compatibility with various cosmetic formulations, and the extracted plant raw materials have the components which do not influence the realization of the beneficial effect of the invention, so the variety of the plant raw materials does not limit the realization of the beneficial effect of the invention. The "plant material" as used herein refers to all parts of a plant, including flowers, fruits, seeds, roots, bark, stems, leaves, fungal fruit bodies, etc. of the plant.
The invention has the beneficial effects that:
the invention provides a novel method for effectively extracting plant raw materials for cosmetics by using double solvents with different polarities, which optimizes extraction steps and extraction condition parameters according to the optimized matching of an extraction solvent and the selection of a specific solvent, so that the extraction efficiency of the plant raw materials is greatly increased, the evaluation of the plant extraction efficiency is mainly evaluated by the antioxidant and anti-inflammatory effects of the plant raw materials, the main effects of plant extracts added into the cosmetics are also two, and the extracts extracted by the method are far superior to the extracts extracted by the prior art in the two effects through effect experiments. The extraction method effectively shortens the extraction time, has high extraction efficiency, uses conventional and cheap equipment, effectively reduces the preparation cost, and is very suitable for large-scale industrial production. The plant extract obtained by the invention has more stable components and better compatibility with auxiliary materials of various formulations of cosmetics, and particularly when the plant extract is added into oil-containing cosmetics, the defects of precipitation, precipitation and the like of the extract in the prior art, which influence the quality and the efficacy of products, are effectively overcome, so that the cosmetics are easier to store and transport, the product quality is better, and the effect is better when the plant extract is used. The invention effectively reduces the dosage of organic solvent in the prior art, reduces the pollution to the environment, and is more economic and environment-friendly.
Drawings
FIG. 1 is a graph of the evaluation of the DPPH clearance rate of the extraction effect of samples 1-24;
FIG. 2 is a graph of the evaluation of DPPH clearance rate of 25-30 extraction effect samples;
FIG. 3 is a graph showing the DPPH clearance evaluation of the extraction effect of samples 31 to 36.
Detailed Description
In order to make the extraction method of the present invention more detailed for those skilled in the art, the inventors provide the following specific examples, and all the reagents involved are well known in the art and commercially available, and the instruments involved are also well known and available to those skilled in the art. The raw materials used in the following examples are only for illustrating the technical method and effects of the present invention in more detail, and are not intended to limit the raw materials, and other plant materials used for cosmetic additives may be used as the raw materials for the present invention. In order to ensure the stability of the second solvent and the extract, in the specific embodiment, each solvent used in the first solvent is an anhydrous solvent. The following examples are not to be construed as limiting the claims in any way.
The raw materials used in the specific embodiment of the present invention are shown in Table 1, and the equipment purchasers are shown in Table 2
TABLE 1 sources of raw materials
TABLE 2 Equipment sources
Example 1
(1) Extracting for the first time: weighing 10g of jasmine, adding 500g of ethanol according to the material-liquid ratio of 1:50m/m, mixing, and extracting for 2h at 40 ℃;
(2) and (3) second extraction: adding 600g of sunflower seed oil according to the feed-liquid ratio of 1:60m/m, and stirring and extracting for 1h at 50 ℃;
(3) concentrating under reduced pressure at 40 deg.C until ethanol is completely removed;
(4) filtering with filter plate with aperture of 10 μm, and filtering to obtain clear filtrate.
Example 2
(1) Extracting for the first time: weighing 10g of turmeric, adding ethanol according to the material-liquid ratio of 1:10m/m, mixing, and extracting for 1h at 60 ℃;
(2) and (3) second extraction: adding hydrogenated polyisobutene (20cSt) according to the feed-liquid ratio of 1:70m/m, and stirring and extracting for 0.5h at the temperature of 60 ℃;
(3) concentrating under reduced pressure at 50 deg.C until ethanol is completely removed;
(4) filtering with filter plate with aperture of 1 μm, and filtering to obtain clear filtrate.
Example 3
(1) Extracting for the first time: weighing 10g of angelica, adding absolute ethyl alcohol according to the material-liquid ratio of 1:100m/m, mixing, and extracting for 0.5h at 90 ℃;
(2) and (3) second extraction: adding caprylic acid/capric acid triglyceride according to the feed-liquid ratio of 1:100m/m, and stirring and extracting at 90 ℃ for 2 h;
(3) concentrating under reduced pressure at 80 deg.C until ethanol is completely removed;
(4) filtering with filter plate with pore diameter of 0.2 μm, and filtering to obtain clear filtrate.
Example 4
(1) Coarse crushing: pulverizing flos Matricariae Chamomillae to 20 mesh;
(2) high-temperature high-pressure treatment: treating at 100 deg.C under 0.1MPa for 5 min;
(3) and (3) drying: drying at 50 deg.C for 1 h;
(4) extracting for the first time: weighing 10g of coarsely ground chamomile, adding chloroform according to the material-liquid ratio of 1:60m/m, mixing, and extracting at 40 ℃ for 0.5 h;
(5) and (3) second extraction: adding white oil (7cSt) according to the feed-liquid ratio of 1:40m/m, and stirring and extracting at 40 ℃ for 1.5 h;
(6) concentrating under reduced pressure at 40 deg.C until chloroform is completely removed;
(7) filtering with filter plate with pore diameter of 0.2 μm, and filtering to obtain clear filtrate.
Example 5
(1) Coarse crushing: pulverizing Curcuma rhizome to 40 mesh;
(2) high-temperature high-pressure treatment: treating at 110 deg.C under 0.2MPa for 20 min;
(3) and (3) drying: drying at 60 ℃ for 2 h;
(4) extracting for the first time: weighing 10g of coarsely ground turmeric, adding chloroform according to the material-liquid ratio of 1:10m/m, mixing, and extracting at 80 ℃ for 1 h;
(5) and (3) second extraction: adding caprylic acid/capric acid triglyceride according to the feed-liquid ratio of 1:30m/m, and stirring and extracting at 80 ℃ for 2 h;
(6) concentrating under reduced pressure at 60 deg.C until chloroform is completely removed;
(7) filtering with filter plate with aperture of 10 μm, and filtering to obtain clear filtrate.
Example 6
(1) Coarse crushing: pulverizing fructus Sapindi Mukouossi to 60 mesh;
(2) high-temperature high-pressure treatment: treating at 130 deg.C under 0.2MPa for 30 min;
(3) and (3) drying: drying at 80 deg.C for 1.5 h;
(4) extracting for the first time: weighing 10g of coarsely ground soapberry, adding chloroform according to the material-liquid ratio of 1:70m/m, mixing, and extracting at 90 ℃ for 2 h;
(5) and (3) second extraction: adding hydrogenated polydecene (30cSt) according to the feed-liquid ratio of 1:50m/m, and stirring and extracting at 90 ℃ for 0.5 h;
(6) concentrating under reduced pressure at 80 deg.C until chloroform is completely removed;
(7) filtering with filter plate with aperture of 6 μm, and filtering to obtain clear filtrate.
Example 7
(1) Coarse crushing: crushing the fructus viticis to 30 meshes;
(2) high-temperature high-pressure treatment: treating at 100 deg.C under 0.1MPa for 5 min;
(3) and (3) drying: drying at 70 deg.C for 1 h;
(4) extracting for the first time: weighing 10g of coarsely crushed fructus viticis, adding acetone according to the material-liquid ratio of 1:20m/m, mixing, and extracting at 45 ℃ for 0.5 h;
(5) and (3) second extraction: adding isostearyl isostearate according to the feed-liquid ratio of 1:10m/m, and stirring and extracting for 1h at the temperature of 45 ℃;
(6) concentrating under reduced pressure at 45 deg.C until acetone is completely removed;
(7) filtering with filter plate with aperture of 2 μm, and filtering to obtain clear filtrate.
Example 8
(1) Coarse crushing: pulverizing folium kaki to 50 mesh;
(2) high-temperature high-pressure treatment: treating at 110 deg.C under 0.1MPa for 20 min;
(3) and (3) drying: drying at 55 deg.C for 1.5 h;
(4) extracting for the first time: weighing 10g of the persimmon leaves after coarse crushing, adding acetone according to the material-liquid ratio of 1:30m/m, mixing, and extracting for 1h at 55 ℃;
(5) and (3) second extraction: adding soybean oil according to the feed-liquid ratio of 1:20m/m, and stirring and extracting for 1h at the temperature of 55 ℃;
(6) concentrating under reduced pressure at 55 deg.C until acetone is completely removed;
(7) filtering with filter plate with pore diameter of 4 μm, and filtering to obtain clear filtrate.
Example 9
(1) Coarse crushing: crushing the prunella vulgaris to 60 meshes;
(2) high-temperature high-pressure treatment: treating at 130 deg.C under 0.2MPa for 30 min;
(3) and (3) drying: drying at 65 ℃ for 2 h;
(4) extracting for the first time: weighing 10g of coarsely ground selfheal, adding chloroform-ethanol mixed liquor (chloroform-ethanol is compounded according to the mass ratio of 1: 1) according to the material-liquid ratio of 1:40m/m, mixing, and extracting for 2 hours at 65 ℃;
(5) and (3) second extraction: adding sesame oil according to the material-liquid ratio of 1:100m/m, and stirring and extracting for 2h at 65 ℃;
(6) concentrating under reduced pressure at 65 deg.C until the solvent is completely removed;
(7) filtering with filter plate with aperture of 8 μm, and filtering to obtain clear filtrate.
Example 10
(1) Coarse crushing: pulverizing stigma croci to 40 mesh;
(2) high-temperature high-pressure treatment: treating at 100 deg.C under 0.1MPa for 30 min;
(3) and (3) drying: drying at 60 ℃ for 2 h;
(4) extracting for the first time: weighing 10g of coarsely crushed saffron crocus, adding ethanol according to the material-liquid ratio of 1:10m/m, mixing, and extracting at 80 ℃ for 1 h;
(5) and (3) second extraction: adding caprylic acid/capric acid triglyceride according to the feed-liquid ratio of 1:30m/m, and stirring and extracting at 80 ℃ for 2 h;
(6) cooling to below 40 deg.C, and coarse filtering with 60 mesh;
(7) concentrating under reduced pressure at 60 deg.C until the solvent is completely removed;
(8) cooling to below 40 deg.C, filtering with filter plate having aperture of 10 μm, and fine filtering to obtain clear filtrate.
Example 11
(1) Coarse crushing: pulverizing semen Ginkgo to 50 mesh;
(2) high-temperature high-pressure treatment: treating at 110 deg.C under 0.2MPa for 15 min;
(3) and (3) drying: drying at 75 ℃ for 1 h;
(4) extracting for the first time: weighing 10g of coarsely ground ginkgo, adding a chloroform-acetone mixed solvent (which is compounded according to the mass ratio of 1: 1) according to the material-liquid ratio of 1:30m/m, mixing, and extracting for 0.5h at 85 ℃;
(5) and (3) second extraction: adding a caprylic/capric triglyceride and hydrogenated polydecene (17cSt) compound according to the feed-liquid ratio of 1:30m/m (the two are compounded according to the mass ratio of 1: 1), and stirring and extracting for 0.5h at the temperature of 75 ℃;
(6) cooling to below 40 deg.C, and coarse-filtering with 80 mesh;
(7) concentrating under reduced pressure at 75 deg.C until the solvent is completely removed;
(8) cooling to below 40 deg.C, filtering with filter plate with aperture of 1 μm, and fine filtering to obtain clear filtrate.
Example 12
(1) Coarse crushing: pulverizing flos Matricariae Chamomillae to 60 mesh;
(2) high-temperature high-pressure treatment: treating at 130 deg.C under 0.1MPa for 10 min;
(3) and (3) drying: drying at 80 deg.C for 1.5 h;
(4) extracting for the first time: weighing 10g of coarsely crushed chamomile, adding a mixed solvent of ethanol and acetone (the mixture is compounded according to the ratio of 1: 1) according to the feed-liquid ratio of 1:50m/m, mixing, and extracting for 2 hours at 90 ℃;
(5) and (3) second extraction: adding a compound of olive oil and macadamia nut oil (the two are compounded according to the mass ratio of 1: 1) according to the material-liquid ratio of 1:50m/m, and stirring and extracting for 1h at the temperature of 60 ℃;
(6) cooling to below 40 deg.C, and coarse-filtering with 100 mesh sieve;
(7) concentrating under reduced pressure at 80 deg.C until the solvent is completely removed;
(8) cooling to below 40 deg.C, filtering with filter plate having aperture of 6 μm, and fine filtering to obtain clear filtrate.
Example 13
(1) Coarse crushing: pulverizing flos Matricariae Chamomillae to 20 mesh;
(2) high-temperature high-pressure treatment: treating at 125 deg.C under 0.1MPa for 15 min;
(3) and (3) drying: drying at 70 deg.C for 1 h;
(4) extracting for the first time: weighing 10g of coarsely ground chamomile, adding a chloroform-ethanol mixed solvent (which is compounded according to a mass ratio of 1: 1) according to a material-liquid ratio of 1:30m/m, mixing, and extracting for 2 hours at 90 ℃;
(5) and (3) second extraction: adding a white oil (16cSt) and hydrogenated polyisobutene (11cSt) mixed solvent according to the feed-liquid ratio of 1:30m/m (the two are compounded according to the mass ratio of 1: 1), and stirring and extracting for 1h at the temperature of 50 ℃;
(6) cooling to below 40 deg.C, and coarse filtering with 90 mesh sieve;
(7) concentrating under reduced pressure at 80 deg.C until the solvent is completely removed;
(8) cooling to below 40 deg.C, filtering with filter plate having aperture of 5 μm, and fine filtering to obtain clear filtrate.
Example 14
(1) Coarse crushing: pulverizing stigma croci to 30 mesh;
(2) high-temperature high-pressure treatment: treating at 130 deg.C under 0.1MPa for 15 min;
(3) and (3) drying: drying at 70 deg.C for 1 h;
(4) extracting for the first time: weighing 10g of coarsely crushed saffron crocus, adding ethanol according to the material-liquid ratio of 1:40m/m, mixing, and extracting at 90 ℃ for 1 h;
(5) and (3) second extraction: adding a grape seed oil and oat oil mixed solvent (the two are compounded according to the mass ratio of 1: 1) according to the feed-liquid ratio of 1:30m/m, and stirring and extracting for 1h at the temperature of 55 ℃;
(6) cooling to below 40 deg.C, and coarse filtering with 90 mesh sieve;
(7) concentrating under reduced pressure at 80 deg.C until the solvent is completely removed;
(8) cooling to below 40 deg.C, filtering with filter plate having aperture of 5 μm, and fine filtering to obtain clear filtrate.
Example 15
(1) Coarse crushing: pulverizing stigma croci to 50 mesh;
(2) high-temperature high-pressure treatment: treating at 130 deg.C under 0.2MPa for 10 min;
(3) and (3) drying: drying at 70 deg.C for 1 h;
(4) extracting for the first time: weighing 10g of coarsely crushed saffron crocus, adding chloroform according to the material-liquid ratio of 1:40m/m, mixing, and extracting at 60 ℃ for 1 h;
(5) and (3) second extraction: adding sweet almond oil according to the material-liquid ratio of 1:30m/m, and stirring and extracting for 1h at the temperature of 45 ℃;
(6) cooling to below 40 deg.C, and coarse filtering with 90 mesh sieve;
(7) concentrating under reduced pressure at 80 deg.C until the solvent is completely removed;
(8) cooling to below 40 deg.C, filtering with filter plate having aperture of 0.5 μm, and fine filtering to obtain clear filtrate.
Example 16
(1) Extracting for the first time: weighing 10g of saffron crocus, adding ethanol according to the material-liquid ratio of 1:30m/m, mixing, and extracting at 70 ℃ for 1 h;
(2) and (3) second extraction: adding caprylic acid/capric acid triglyceride according to the feed-liquid ratio of 1:30m/m, and stirring and extracting for 1h at 70 ℃;
(3) cooling to below 40 deg.C, and coarse-filtering with 100 mesh sieve;
(4) concentrating under reduced pressure at 65 deg.C until ethanol is completely removed;
(5) filtering with filter plate with aperture of 1 μm, and filtering to obtain clear filtrate.
Example 17
(1) Extracting for the first time: weighing 10g of saffron crocus, adding chloroform according to the material-liquid ratio of 1:100m/m, mixing, and extracting at 90 ℃ for 0.5 h;
(2) and (3) second extraction: adding macadamia nut oil according to the material-liquid ratio of 1:10m/m, and stirring and extracting for 2 hours at the temperature of 40 ℃;
(3) coarse filtering with 100 meshes;
(4) concentrating under reduced pressure at 40 deg.C until chloroform is completely removed;
(5) filtering with filter plate with aperture of 10 μm, and filtering to obtain clear filtrate.
Example 18
(1) Extracting for the first time: weighing 10g of saffron crocus, adding acetone according to the material-liquid ratio of 1:10m/m, mixing, and extracting at 40 ℃ for 2 h;
(2) and (3) second extraction: adding hydrogenated polyisobutene (20cSt) according to the feed-liquid ratio of 1:100m/m, and stirring and extracting for 0.5h at the temperature of 90 ℃;
(3) cooling to below 40 deg.C, and coarse-filtering with 100 mesh sieve;
(4) concentrating under reduced pressure at 80 deg.C until acetone is completely removed;
(5) filtering with filter plate with pore diameter of 0.2 μm, and filtering to obtain clear filtrate.
Example 19
(1) Coarse crushing: pulverizing stigma croci to 40 mesh;
(2) high-temperature high-pressure treatment: treating at 130 deg.C under 0.11MPa for 5 min;
(3) and (3) drying: drying at 50 deg.C for 2 h;
(4) extracting for the first time: weighing 10g of coarsely crushed saffron crocus, adding a mixed solvent of acetone and chloroform (the mixture is compounded according to a ratio of 1: 2) according to a material-liquid ratio of 1:50m/m, mixing, and extracting for 1h at 80 ℃;
(5) and (3) second extraction: adding a mixed solvent of white oil (10cSt) and isostearic acid isostearyl alcohol ester (the mixture is compounded according to the ratio of 1: 1) according to the feed-liquid ratio of 1:30m/m, and stirring and extracting for 2 hours at the temperature of 65 ℃;
(6) cooling to below 40 deg.C, and coarse-filtering with 100 mesh sieve;
(7) concentrating under reduced pressure at 70 deg.C until the solvent is completely removed;
(8) filtering with filter plate with aperture of 6 μm, and filtering to obtain clear filtrate.
Efficacy test of the invention
The cooperation of the solvent I and the solvent II, the optimized extraction process and the extraction parameters of the invention are combined, the synergistic effect can be achieved, the extraction rate is higher, the property of the extract is more excellent and more stable, the extraction cost is lower, and the method is suitable for industrial application.
Selection of solvent one and solvent two of the present invention
1. The solvent I is a representative solvent which is commonly used for plant extraction and has good compatibility with various active ingredients, and particularly has good effect of breaking cell walls; considering that the extraction effect of the solvent one is better than that of the solvent two, the extraction effect is finally determined to be ethanol, acetone and chloroform. The inventors believe that the above solvents have met the requirements of the present invention and therefore do not require further screening of solvent one, which also reduces the effort required for solvent two selection. 2. The selection process of the second solvent is briefly described as follows:
the second solvent is selected from solvent with polarity less than that of the first solvent, and oil is preferably selected as the second solvent.
(1) Vegetable oil: the properties of the vegetable oils are similar, so only one is selected as a representative, and the vegetable oils are respectively compounded and extracted with three solvents of the solvent I, and have better effects;
(2) white oil: selecting two kinds of white oil (generally, the numerical values near the critical value, such as 26 and 32) within and outside a limited viscosity range, and respectively compounding and extracting the white oil with three solvents of the first solvent, wherein the white oil within the viscosity range has a good effect, and the white oil outside the viscosity range has a poor effect;
(3) hydrogenated polyisobutene, hydrogenated polydecene: both of these are olefin polymers, only one of them is selected as a representative, and the white oil screening work is repeated, namely, the experiments are respectively carried out in the limited viscosity range and outside the viscosity range (generally, the values near the critical value, such as 26 and 32), so that different extraction effects are obtained;
(4) caprylic/capric triglyceride: the extract is compounded and extracted with three solvents of the first solvent, and has better effect;
(5) isostearyl isostearate: the extract is compounded and extracted with three solvents of the first solvent, and has better effect;
(6) polydimethylsiloxane (silicone oil): the silicon oil is a silicon chain, has poor dissolving effect on active ingredients of the carbon chain, and has poor extraction effect when being compounded with the solvent I respectively.
The above is an experimental idea of the solvent screening part, namely samples 1-24 of the solvent selection part. The raw materials and preparation methods of samples 1-24 were the same, except for the extraction solvents.
The preparation method comprises the following steps:
(1) coarse crushing: 10g of saffron crocus, and crushing to 40 meshes;
(2) high-temperature high-pressure treatment: treating at 100 deg.C under 0.10MPa for 30 min;
(3) and (3) drying: drying at 60 ℃ for 2 h;
(4) extracting for the first time: adding a first solvent according to the feed-liquid ratio of 1:10m/m, mixing, and extracting at 80 ℃ for 1 h;
(5) and (3) second extraction: adding a second solvent according to the feed-liquid ratio of 1:30m/m, and stirring and extracting for 2 hours at the temperature of 80 ℃;
(6) cooling to below 40 deg.C, and coarse-filtering with 60 mesh sieve to obtain filtrate;
(7) concentrating under reduced pressure at 60 deg.C until the solvent is completely removed;
(8) cooling to below 40 deg.C, and fine filtering to obtain clear filtrate.
The solvents used in samples 1-24 are shown in Table 3
TABLE 3 sample solvent table
3. And (3) testing results:
the content of the part is to screen a second solvent, wherein the first solvent is fixed into ethanol, chloroform and acetone.
(1) DPPH free radical scavenging experiments: the components of the plant extract are complex, and the analysis and quantification of the effective components of the extract are difficult, so that the extraction efficiency of the effective components is evaluated by the detection of antioxidant activity by a person skilled in the art, and the extract prepared by the process with good extraction efficiency has more excellent antioxidant activity. Antioxidant activity is generally evaluated using DPPH free radical scavenging experiments. DPPH (2, 2-biphenyl-1-picrylhydrazino) is a stable organic nitrogen free radical and is widely applied to in vitro antioxidant capacity research. Based on the characteristic absorption peak of DPPH at about 515nm, the antioxidant provides hydrogen atoms to reduce single electrons on DPPH to weaken the color, and the degree of free radical scavenging is evaluated according to the reduction of the light absorption value.
The results of the antioxidant activity test of samples 1-24 are shown in FIG. 1.
(2) Stability experiments, see table 4.
TABLE 4 comparison of stability of different solvent extracts
The experimental results are as follows:
1. samples 1-3 are prepared by extracting vegetable oil (the vegetable oil is similar in nature, and only sunflower seed oil is taken as an example) with a solvent I in a compounding manner, and the vegetable oil is compounded with ethanol, acetone and chloroform, so that the good extraction effect is achieved.
2. Samples 4-6 are prepared by extracting caprylic acid/capric acid triglyceride with ethanol, acetone and chloroform respectively in a compounding manner, and have good extraction effect.
3. Samples 7-9 are prepared by extracting isostearyl isostearate with ethanol, acetone and chloroform respectively in a compounding manner, and have good extraction effect.
4. Samples 10-12 are white oil (26cSt, which meets the requirement of the invention that the kinematic viscosity is less than or equal to 30cSt), and are respectively compounded and extracted with ethanol, acetone and chloroform, and the extraction effect is better.
5. Samples 13-15 are white oil (32cSt, which does not meet the requirement of the invention that the kinematic viscosity is less than or equal to 30cSt), and are respectively compounded and extracted with ethanol, acetone and chloroform, and the extraction effect is poor.
6. Samples 10-15 are the results of comparing the white oil with a kinematic viscosity of less than or equal to 30cSt with the white oil with a kinematic viscosity of greater than or equal to 30cSt, and the reason for selecting the white oil with a kinematic viscosity of less than or equal to 30cSt is illustrated by the difference of extraction effects.
7. Samples 16-18 are prepared by respectively extracting hydrogenated polydecene (30cSt, which meets the requirement of the invention that the kinematic viscosity is less than or equal to 30cSt) with ethanol, acetone and chloroform in a compounding way, and have good extraction effect.
8. Samples 19-21 are prepared by respectively extracting hydrogenated polydecene (46cSt, which does not meet the requirement of the invention that the kinematic viscosity is less than or equal to 30cSt) with ethanol, acetone and chloroform in a compounding manner, and the extraction effect is poor.
9. Samples 16-21 are similar to white oil and are the reason for selecting hydrogenated polydecene with a kinematic viscosity of 30cSt or less by comparing hydrogenated polydecene with a kinematic viscosity of 30cSt or more and comparing the results with the extraction effect. In addition, since both hydrogenated polydecene and hydrogenated polyisobutene are polymers, the description will be made by taking hydrogenated polydecene as an example.
10. Samples 22-24 are prepared by compounding and extracting polydimethylsiloxane (silicone oil, PMX200, 6cSt) with ethanol, acetone and chloroform respectively, and the silicone oil has a silicon chain structure and has poor dissolving effect on active ingredients of a carbon chain, so that the extraction effect is poor, and the DPPH clearance rate is very low; the poor compatibility also leads to poor stability, manifested as turbidity of the sample or precipitation (precipitation) of the active ingredient.
Through the above experiments, the solvent II preferred by the present invention comprises vegetable oil (samples 1 to 3), caprylic/capric triglyceride (samples 4 to 6), isostearyl isostearate (samples 7 to 9), white oil (samples 10 to 12) with a kinematic viscosity (40 ℃) of less than or equal to 30cSt, hydrogenated polyisobutene (which is an olefin polymer with hydrogenated polydecene, and only hydrogenated polydecene is taken as an example for experiments) with a kinematic viscosity (40 ℃) of less than or equal to 30cSt, and hydrogenated polydecene (samples 16 to 18) with a kinematic viscosity (40 ℃) of less than or equal to 30 cSt.
The second solvents used as comparative examples in the present invention include white oil (samples 13 to 15) having a kinematic viscosity (40 ℃) of not less than 30cSt, hydrogenated polydecene (samples 19 to 21) having a kinematic viscosity (40 ℃) of not less than 30cSt, and 6cSt polydimethylsiloxane PMX200 (samples 21 to 24).
According to the comparative experiments, vegetable oil, caprylic/capric triglyceride, isostearyl isostearate, white oil with the kinematic viscosity (40 ℃) of less than or equal to 30cSt, hydrogenated polyisobutene and hydrogenated polydecene all have good extraction effects by respectively carrying out compound extraction with the solvent I (ethanol, acetone and chloroform), and the product after extraction has good stability, so that the solvent II is suitable to be used as the solvent II of the invention and is matched with the solvent I to realize the extraction process of the invention. White oil with kinematic viscosity (40 ℃) of more than or equal to 30cSt, hydrogenated polyisobutene and hydrogenated polydecene are not suitable for being used as the second solvent of the invention because the extraction effect is not ideal due to the fact that the viscosity is increased and the mass transfer in the extraction process is not facilitated. The silicon oil (polydimethylsiloxane) has poor compatibility with carbon chain active ingredients in plants due to the structural difference, so that the extraction efficiency is low, and the stability of the extracted product is poor, so that the silicon oil (polydimethylsiloxane) is not suitable to be used as the solvent II.
Secondly, determining the extracted parameters of the invention
1. Second extraction temperature selection experiment: the second step is the synergistic extraction of the solvent and the solvent, so the extraction in the step is very important, and the extraction temperature in the second step directly influences the intersolubility degree and the extraction efficiency of the two solvents.
In this experiment, the first solvent is exemplified by ethanol, and the second solvent is exemplified by caprylic/capric triglyceride. The raw materials are exemplified by saffron.
The specific preparation process is as in experiment one, and the specific steps are as follows:
(1) coarse crushing: 10g of saffron crocus, and crushing to 40 meshes;
(2) high-temperature high-pressure treatment: treating at 100 deg.C under 0.10MPa for 30 min;
(3) and (3) drying: drying at 60 ℃ for 2 h;
(4) extracting for the first time: adding ethanol according to the feed-liquid ratio of 1:10m/m, mixing, and extracting at 80 deg.C for 1 h;
(5) and (3) second extraction: adding caprylic/capric triglyceride according to the feed-liquid ratio of 1:30m/m, wherein the extraction temperature is shown in Table 5, and stirring and extracting for 2 h;
(6) cooling to below 40 deg.C, and coarse-filtering with 60 mesh sieve to obtain filtrate;
(7) concentrating under reduced pressure at 60 deg.C until the solvent is completely removed;
(8) cooling to below 40 deg.C, and fine filtering to obtain clear filtrate.
TABLE 5
The extraction effect of the sample 25-30 is evaluated by DPPH clearance, and the experimental method is the DPPH free radical clearance experiment. The results are shown in FIG. 2. Therefore, the extraction efficiency is highest when the temperature of the extract is between 40 and 90 ℃, and is too low when the temperature is lower than 40 ℃ or higher than 90 ℃, and if poor temperature is adopted, the extraction rate can be improved only by prolonging the extraction time, so that the economic benefit of the extraction process on industrial application is influenced.
The stability test methods of the samples 25-30 are shown in stability comparison, and the results are shown in Table 6.
TABLE 6 comparison of stability of samples taken at different temperatures
The content of the part is to screen the technological parameters of the second extraction step, taking the temperature as an example, the DPPH and the stability of the product under the five temperature conditions of 30 ℃, 40 ℃, 60 ℃, 75 ℃, 90 ℃ and 95 ℃ are compared, the extraction effect (DPPH) and the stability at 40-90 ℃ are both better, the extraction effect at 30 ℃ is poor, the extraction effect at 95 ℃ is poor, the stability of the product is also poor due to overhigh temperature, discoloration and peculiar smell occur, therefore, the range of 40-90 ℃ is recommended to be adopted for the final extraction temperature, and the optimal extraction temperature is 75 ℃.
2. And (3) extracting the material-liquid ratio experiment for the second time: the second step is the synergic extraction of the solvent I and the solvent II, the extraction in the step is crucial, the extraction material-liquid ratio in the second step directly influences the intersolubility of the solvent I and the solvent II, and the extraction efficiency of the extraction is matched
In this experiment, the first solvent is exemplified by ethanol, and the second solvent is exemplified by caprylic/capric triglyceride. The raw materials are exemplified by saffron.
The specific preparation process is as in experiment one, and the specific steps are as follows:
(1) coarse crushing: 10g of saffron crocus, and crushing to 40 meshes;
(2) high-temperature high-pressure treatment: treating at 100 deg.C under 0.10MPa for 30 min;
(3) and (3) drying: drying at 60 ℃ for 2 h;
(4) extracting for the first time: adding ethanol according to the feed-liquid ratio of 1:10m/m, mixing, and extracting at 80 deg.C for 1 h;
(5) and (3) second extraction: the feed-liquid ratio is shown in Table 7, the caprylic capric triglyceride is added, the extraction temperature is 80 ℃, and the mixture is stirred and extracted for 2 hours;
(6) cooling to below 40 deg.C, and coarse-filtering with 60 mesh sieve to obtain filtrate;
(7) concentrating under reduced pressure at 60 deg.C until the solvent is completely removed;
(8) cooling to below 40 deg.C, and fine filtering to obtain clear filtrate.
TABLE 7
The extraction effect of the samples 31-36 is evaluated by DPPH clearance, the experimental method is shown in the DPPH free radical clearance experiment, and the result is shown in FIG. 3. Therefore, the extraction efficiency is high when the feed-liquid ratio is 1: 10-100, and the extraction efficiency is optimal when the feed-liquid ratio is 1: 10-50.
Thirdly, the extraction efficiency of the invention is compared with that of the prior art
The components of the plant extract are complex, and the analysis and quantification of the effective components of the extract are difficult, so that the extraction efficiency of the effective components is evaluated by detecting the antioxidant activity and the anti-inflammatory activity by a person skilled in the art, and the extract prepared by the process with good extraction efficiency has more excellent efficacy.
Antioxidant activity is generally evaluated using DPPH free radical scavenging experiments.
Anti-inflammatory activity is generally assessed experimentally by inhibiting hyaluronidase. Hyaluronidase is a participant of anaphylactic reaction, and researches show that hyaluronidase has strong correlation with inflammation and allergy, and a hyaluronidase in-vitro inhibition test is often used as a method for measuring the antiallergic activity. The antiallergic activity takes the hyaluronidase inhibition rate as an index, and the higher the hyaluronidase inhibition rate is, the stronger the antiallergic activity is.
Samples used for the following efficacy experiments:
sample 1 (prior art grease two extractions): weighing 10g of stigma croci Sativi, pulverizing to 40 mesh, treating at 100 deg.C under 0.10MPa for 30min, and drying at 60 deg.C for 2 hr; adding 100g of caprylic/capric triglyceride into the mixture at a feed-liquid ratio of 1:10(m/m), and stirring and extracting at 80 ℃ for 1 h; adding 300g of caprylic/capric triglyceride again at a feed-liquid ratio of 1:30(m/m), and stirring and extracting at 80 ℃ for 2 h; cooling to below 40 deg.C, filtering with filter plate having aperture of 10 μm, and fine filtering to clarify.
Sample 2 (prior art ethanol double extraction): weighing 10g of stigma croci Sativi, pulverizing to 40 mesh, treating at 100 deg.C under 0.10MPa for 30min, and drying at 60 deg.C for 2 hr; adding 100g of ethanol into the mixture according to the feed-liquid ratio of 1:10(m/m), and stirring and extracting for 1h at the temperature of 80 ℃; adding 300g of ethanol again according to the feed-liquid ratio of 1:30(m/m), and stirring and extracting for 2h at 80 ℃; concentrating under reduced pressure at 60 deg.C, filtering with filter plate having aperture of 10 μm, and fine filtering to clarify.
Sample 3 (two extractions with solvent one less polar than solvent two): weighing 10g of stigma croci Sativi, pulverizing to 40 mesh, treating at 100 deg.C under 0.10MPa for 30min, and drying at 60 deg.C for 2 hr; adding 300g of cyclohexane into the mixture according to the feed-liquid ratio of 1:10(m/m), and stirring and extracting the mixture for 1 hour at the temperature of 80 ℃; according to the formula of saffron: adding 900g of butanediol into butanediol at a ratio of 1:30(m/m), and stirring and extracting at 80 ℃ for 2 hours; cooling to below 40 deg.C, and filtering to obtain filtrate; concentrating under reduced pressure at 60 deg.C to remove cyclohexane; filtering with filter plate with aperture of 10 μm, and fine filtering to obtain the final product.
Sample 4: example 10.
DPPH radical scavenging experiment
(1) The experimental method comprises the following steps: taking 1mL of DPPH solution and 1mL of sample solution, fully oscillating and uniformly mixing, standing for 30min, and measuring the absorbance of the mixture by using a microplate reader at the wavelength of 517 nm.
DPPH free radical clearance calculation formula:
DPPH free radical clearance [ (B + C) -A ]/B100%
In the formula: a is the OD value of the sample solution mixed with the DPPH solution, B is the OD value of the absolute ethyl alcohol mixed with the DPPH solution, and C is the OD value of the absolute ethyl alcohol mixed with the sample solution.
TABLE 8 comparison of DPPH clearance for samples prepared by different procedures
| Sample name | Test concentration% | Clearance |
| Sample | ||
| 1 | 5 | 32 |
| |
5 | 50 |
| Sample 3 | 5 | 53 |
| Sample No. 4 | 5 | 86 |
(3) And (4) experimental conclusion:
the sample 1 is directly extracted by grease, and because the grease has large molecular weight, active ingredients in cells are not easy to extract through cell walls and cell membranes, the DPPH clearance rate is low.
Sample 3 was extracted with two solvents in two steps, but solvent one (in proportion to solvent two) was less polar, solvent two (in proportion to solvent two) was more polar, and solvent one was less interactive with cell membrane phospholipids, which was not conducive to the two solvents entering the cells to extract active ingredients, and destroyed the synergistic interaction between the two solvents, resulting in a lower extraction rate, and thus lower DPPH clearance.
Sample 4 is the extract prepared in example 10 of the present invention, and the time-to-feed-liquid ratio of the extract in sample 4 is the same as that in samples 1, 2 and 3, but the DPPH clearance is significantly higher than that in samples 1, 2 and 3, and is far better than the sum of the effects of samples 1 and 2. The inventors repeated the above experiments using extracts obtained in other embodiments of the present invention, and the results are the same as above, and are not repeated herein.
2. Experiment for inhibiting hyaluronidase
(1) The experimental method comprises the following steps: 0.1mL of 0.25mmol/L calcium chloride solution and 0.5mL of hyaluronidase solution are cultured for 20min at 37 ℃; adding 0.5mL of sample solution, and continuing to culture at 37 ℃ for 20 min; adding 0.5mL of hyaluronic acid sodium solution, keeping the temperature at 37 ℃ for 30min, and standing at normal temperature for 5 min; adding 0.1mL of 0.4mol/L sodium hydroxide solution and 0.5mL of acetylacetone solution, heating in a boiling water bath for 15min, and immediately cooling with ice water for 5 min; adding 1.0mL of Ellisib reagent, diluting with 3.0mL of absolute ethanol, standing for 20min for color development, and measuring the absorbance at 555nm by using a microplate reader.
The hyaluronidase inhibition rate calculation formula is as follows:
hyaluronidase inhibition [ (A-B) - (C-D) ]/(A-D) × 100%
In the formula: a is the absorbance of the control solution (the sample solution is replaced by acetic acid buffer solution), B is the absorbance of the control blank solution (the sample solution and the enzyme solution are replaced by acetic acid buffer solution), C is the absorbance value of the sample solution, and D is the absorbance of the sample blank solution (the enzyme solution is replaced by acetic acid buffer solution).
(2) And (5) comparing the sample with the extraction efficiency.
TABLE 9 comparison of hyaluronidase inhibition ratios for samples prepared by different processes
| Sample name | Test concentration% | Inhibition |
| Sample | ||
| 1 | 5 | 25 |
| |
5 | 43 |
| Sample 3 | 5 | 31 |
| Sample No. 4 | 5 | 72 |
(3) And (4) experimental conclusion:
the sample 1 is directly extracted by adopting grease, and the extraction efficiency is low, so the hyaluronidase inhibition rate is low.
Sample 3 is extracted by two-step double solvents, but the polarity of solvent 1 (compared with solvent 2) is weaker, the polarity of solvent 2 (compared with solvent 1) is stronger, the interaction between solvent 1 and cell membrane phospholipid is weak, so that the two solvents are not favorable for entering cells to extract active ingredients, the synergistic effect between the two solvents is damaged, the extraction rate is reduced, and the hyaluronidase inhibition rate is lower.
Sample 4 is the extract prepared in example 10 of the present invention, and the parameters of the extract time-to-feed-liquid ratio and the like of sample 4 are the same as those of samples 1, 2 and 3, but the hyaluronidase inhibition rate is obviously higher than that of samples 1, 2 and 3 and is far better than the sum of the effects of samples 1 and 2. The inventors repeated the above experiments using extracts obtained in other embodiments of the present invention, and the results are the same as above, and are not repeated herein.
Secondly, compared with the prior art, the stability of the extract obtained by the invention in oil type cosmetics is higher
1. Used for clarity comparison in oil type cosmetics
(1) The experimental method comprises the following steps: heating 3.0g of sample liquid and 27.0g of oil as common adjuvant of oil cosmetic to 50 deg.C, stirring for dissolving for 20min, standing, cooling for 1 hr, and observing the dissolution of sample in oil. The compatibility of the sample and the grease is good, and the dissolved sample is clear and transparent; if the sample is poorly compatible with the oil, the sample becomes cloudy after dissolution. Therefore, the solubility of the sample in the oil and fat can be characterized by the turbidity after the dissolution.
Turbidity is an optical property due to scattering of light by minute particles in a liquid, and the amount of scattered light increases as the turbidity increases. In the experiment, a HI93414 high-precision data type turbidity measuring instrument is adopted to detect the turbidity of the sample. Lower values of the measured values prove that lower turbidity proves better clarity and good product stability.
(2) And (5) comparing the sample with the extraction efficiency.
TABLE 10 comparison of turbidity of samples from different processes
And (4) experimental conclusion: as shown in the above table. Sample 1 is a fat extract by itself, and therefore the turbidity known in oil-type cosmetic accessories is excellent; sample 2 is an alcohol-soluble extract, and has poor compatibility with oils and fats, and therefore has high turbidity. The extraction solvent of sample 3 reverses the polarity of the first and second solvents of the present invention, so that the final product has stronger solvent polarity and poor compatibility with grease, and thus has high turbidity. Sample 4 is extracted by matching the solvent I and the solvent II, and the extraction process is optimized, so that the compatibility of the active ingredients of the extract and the oil which is a common auxiliary material of cosmetics is good, the turbidity is lower, the extract can be even better than the extract obtained by extracting the oil, and the stability and the compatibility of the extract in oil type cosmetics are very excellent. The inventors repeated the above experiments using extracts obtained in other embodiments of the present invention, and the results are the same as above, and are not repeated herein.
2. Oil stability test
(1) The experimental method comprises the following steps: mixing 10g of sample solution and 190g of caprylic/capric triglyceride, heating to about 50 ℃, stirring for dissolving for 20min, evenly dividing the prepared sample into five parts, respectively placing in dark (room temperature cassette), refrigeration (4 ℃ refrigerator), illumination (28 ℃ illumination incubator), heat (45 ℃ oven), and freezing (-15 ℃ refrigerator) under five conditions, and observing stability in 7 days, 14 days, and 30 days.
(2) And (5) comparing the sample with the extraction efficiency.
TABLE 11 comparison of oil stability of different process samples
(3) And (4) experimental conclusion: as shown in the above table.
The sample was found to have a small amount of sediment in the 130 day stability test and a slight off-flavor indicating sample deterioration. The sample stability test for 230 days shows that the sample has a large amount of precipitates, which indicates that the stability of the sample is poor. The sample was observed in the 330-day stability test, which showed a large amount of precipitation, indicating that the sample stability was poor. The 430-day stability test of the sample shows that the appearance is clear and transparent, and the smell is normal, which shows that the stability of the extract prepared by the invention is obviously superior to that of the samples 1, 2 and 3. The inventors repeated the above experiments using extracts obtained in other embodiments of the present invention, and the results are the same as above, and are not repeated herein.
3. Emulsion stability test
(1) The experimental method comprises the following steps: the prepared emulsion added with the sample is averagely divided into 5 parts, filled into a sterilized sample bottle, respectively placed under the five conditions of dark (in a room temperature cassette), refrigeration (in a refrigerator at 4 ℃), illumination (in an illumination incubator at 28 ℃), heating (in an oven at 45 ℃) and freezing (-in a refrigerator at 15 ℃), and the stability is observed on the 7 th day, the 14 th day and the 30 th day respectively.
(2) And (5) comparing the sample with the extraction efficiency.
Table 12 stability survey emulsion base formulations
The preparation process of the emulsion comprises the following steps:
(1) heating and boiling deionized water for about 5min, and cooling to 50-55 ℃;
(2) adding boiled deionized water into a beaker with a proper size and disinfected by 75% alcohol, and adding 1.2% AVC; adding 5% of prepared sample, mechanically stirring and emulsifying; adding 0.13% of preservative MTI, and stirring uniformly to obtain the finished product.
TABLE 13 comparison of emulsion stability for different process samples
(3) And (4) experimental conclusion: as can be seen from the above table, the sample became thin and flowable at 130 days, and both color and odor changed, indicating that the sample deteriorated and had poor stability at 130 days. The color and smell change phenomenon appears in both sample 2 and sample 330 days, which indicates that the product is deteriorated and has poor stability. The appearance color and smell of sample 4 of the present invention remained excellent and stable throughout. From the above experiments, it can be seen that the stability of the inventive samples after addition to the emulsion is significantly better than that of samples 1, 2 and 3. The inventors repeated the above experiments using extracts obtained in other embodiments of the present invention, and the results are the same as above, and are not repeated herein.
4. The extraction cost of the invention is compared with that of the prior art
According to the result of DPPH radical scavenging experiment in the above extraction efficiency experiment, it can be seen that the extraction efficiency of the present invention (sample 4) is much higher than that of direct extraction of oil (sample 1) and ethanol (sample 2) when the extraction conditions are the same (feed-to-liquid ratio, extraction temperature, extraction time).
TABLE 14 cost comparison of the present invention with the prior art industrial application
As can be seen from the above table, the extraction efficiency of the present invention is far superior to that of samples 1 and 2. If the same extraction efficiency as the present invention is to be achieved, the amount of raw material needs to be increased to twice the amount currently used. The raw material is increased and the extraction solvent is also required to be increased by times, the ethanol extraction in the prior art is at least one time more than the organic solvent in the invention, and if the raw material is increased to two times, the organic solvent is at least three times more than the organic solvent in the invention. Therefore, compared with the existing extraction process, the method has the advantages of low cost, less consumption of raw materials and extraction solvent, and lower cost in preparation, storage and transportation. And because the invention has reduced the consumption of organic solvent greatly, has avoided the cost of organic solvent recovery and discharge effectively, the more important thing has greatly reduced the risk to environmental pollution. Compared with the prior art, the invention has the advantages of cost saving, material reduction, energy consumption reduction and environmental protection, and is very suitable for the current energy-saving and emission-reducing industrial mass production.
Claims (29)
1. A method for extracting plant raw materials for cosmetic additives is characterized by comprising the following steps:
(1) extracting for the first time: weighing plant raw materials, mixing the raw materials and a solvent I according to a material-liquid ratio of 1: 10-100 m/m, and extracting at 40-90 ℃ for 0.5-2 h;
(2) and (3) second extraction: adding a second solvent according to the feed-liquid ratio of 1: 10-100 m/m, and extracting for 0.5-2 h at 40-90 ℃;
(3) removing the first solvent;
(4) fine filtering to obtain clear extract;
the first solvent is one or a mixture of ethanol, chloroform and acetone;
the second solvent is one or a mixture of more of white oil, hydrogenated polyisobutene, hydrogenated polydecene, caprylic/capric triglyceride, isostearyl isostearate and vegetable oil;
the kinematic viscosity of the white oil, the hydrogenated polyisobutene and the hydrogenated polydecene is less than or equal to 30cSt at 40 ℃.
2. The method for extracting a plant extract for cosmetic addition according to claim 1, wherein the ratio of the material to the liquid in the step (1) is 1:10 to 50 m/m.
3. The method for extracting a plant extract for cosmetic addition according to claim 1, wherein the ratio of the material to the liquid in the step (2) is 1:10 to 50 m/m.
4. The method for extracting a plant extract for cosmetic addition according to claim 1, wherein the step (3) is carried out by concentrating under reduced pressure at 40-80 ℃ until the solvent one is completely removed.
5. The method of extracting a plant extract for cosmetic addition according to claim 1, wherein the fine filtration in the step (4) is performed using a filter plate having a pore size of 0.2 to 10 μm.
6. The method of claim 1, further comprising a cooling step of cooling to a temperature below 40 ℃ before the fine filtration in step (4).
7. The method for extracting a plant extract for cosmetic addition according to any one of claims 1 to 6, further comprising 60 to 100 mesh coarse filtration between the step (2) and the step (3).
8. The method of extracting plant extract for cosmetic addition according to claim 7, further comprising a cooling step of cooling to below 40 ℃ before the preliminary filtration.
9. The method for extracting a plant material for cosmetic addition according to any one of claims 1 to 6, wherein the plant material is subjected to a pretreatment before the first extraction, and the pretreatment comprises the steps of:
(1) coarse crushing: crushing the raw materials to 20-60 meshes;
(2) high-temperature high-pressure treatment;
(3) and (5) drying.
10. The method for extracting a plant material for cosmetic addition according to claim 9, wherein the high-temperature high-pressure treatment conditions are: and (3) treating the coarsely crushed raw materials for 5-30 min under the conditions of 0.1-0.2 MPa and 100-130 ℃.
11. The method for extracting a plant material for cosmetic addition according to claim 9, wherein the drying is performed at 50 to 80 ℃ for 1 to 2 hours.
12. The method for extracting a plant material for cosmetic addition according to claim 7, wherein the plant material is subjected to a pretreatment before the extraction, and the pretreatment comprises the steps of:
(1) coarse crushing: crushing the raw materials to 20-60 meshes;
(2) high-temperature high-pressure treatment;
(3) and (5) drying.
13. The method for extracting a plant material for cosmetic addition according to claim 12, wherein the high-temperature high-pressure treatment conditions are: and (3) treating the coarsely crushed raw materials for 5-30 min under the conditions of 0.1-0.2 MPa and 100-130 ℃.
14. The method for extracting a plant material for cosmetic addition according to claim 12, wherein the drying is performed at 50 to 80 ℃ for 1 to 2 hours.
15. Use of the process according to any one of claims 1 to 6 for the preparation of a cosmetic additive.
16. Use of the process according to claim 7 for the preparation of cosmetic additives.
17. Use of the process according to claim 8 for the preparation of cosmetic additives.
18. Use of the process according to claim 9 for the preparation of cosmetic additives.
19. Use of the process according to claim 12 for the preparation of cosmetic additives.
20. A plant extract for cosmetics obtained by the method according to any one of claims 1 to 6.
21. A cosmetic plant extract obtained by the method of claim 7.
22. A cosmetic plant extract obtained by the method of claim 8.
23. A cosmetic plant extract obtained by the method of claim 9.
24. A cosmetic plant extract obtained by the method of claim 12.
25. A cosmetic composition comprising the plant extract for cosmetics according to claim 20 and a cosmetically acceptable excipient.
26. A cosmetic composition comprising the plant extract for cosmetics according to claim 21 and a cosmetically acceptable excipient.
27. A cosmetic composition comprising the plant extract for cosmetics according to claim 22 and a cosmetically acceptable excipient.
28. A cosmetic composition comprising the plant extract for cosmetics according to claim 23 and a cosmetically acceptable excipient.
29. A cosmetic comprising the plant extract for cosmetics according to claim 24 and a cosmetically acceptable excipient.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711194829.XA CN109512756B (en) | 2017-11-24 | 2017-11-24 | Method for extracting plant material for cosmetic additive and extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711194829.XA CN109512756B (en) | 2017-11-24 | 2017-11-24 | Method for extracting plant material for cosmetic additive and extract |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109512756A CN109512756A (en) | 2019-03-26 |
| CN109512756B true CN109512756B (en) | 2021-05-04 |
Family
ID=65768601
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711194829.XA Active CN109512756B (en) | 2017-11-24 | 2017-11-24 | Method for extracting plant material for cosmetic additive and extract |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109512756B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110090180B (en) * | 2019-03-29 | 2021-05-07 | 太和康美(北京)中医研究院有限公司 | Cosmetic lithospermum extract and preparation method thereof |
| CN112716844B (en) * | 2021-01-13 | 2023-04-07 | 贵州大隆药业有限责任公司 | Hand cream and preparation method thereof |
| CN114129499A (en) * | 2021-12-28 | 2022-03-04 | 猫头鹰(福州)日用品有限公司 | Preparation and application of plant mixed extract with anti-wrinkle and tightening effects |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1140557A (en) * | 1995-07-19 | 1997-01-22 | 孙占水 | Corn pollen extract and its preparing method |
| JP2004359664A (en) * | 2003-05-09 | 2004-12-24 | Kotobuki Chemical:Kk | Composition for skin care preparation for external use and skin care preparation for external use |
| CN105267092A (en) * | 2015-11-10 | 2016-01-27 | 广州丹奇日用化工厂有限公司 | Plant extract and preparation method and application thereof |
-
2017
- 2017-11-24 CN CN201711194829.XA patent/CN109512756B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1140557A (en) * | 1995-07-19 | 1997-01-22 | 孙占水 | Corn pollen extract and its preparing method |
| JP2004359664A (en) * | 2003-05-09 | 2004-12-24 | Kotobuki Chemical:Kk | Composition for skin care preparation for external use and skin care preparation for external use |
| CN105267092A (en) * | 2015-11-10 | 2016-01-27 | 广州丹奇日用化工厂有限公司 | Plant extract and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109512756A (en) | 2019-03-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104922056B (en) | A kind of fresh aloe juice gel and its preparation method and application | |
| CN109512756B (en) | Method for extracting plant material for cosmetic additive and extract | |
| CN107438427B (en) | Shampoo | |
| CN103356446B (en) | A kind of natural anti-aging skin care product containing black tea extract and preparation method thereof | |
| CN103627514A (en) | Method for extracting grape seed oil from grape seeds | |
| CN109512734B (en) | External plant extract and cosmetic with skin elasticity and gloss recovery effects and preparation method thereof | |
| KR100793019B1 (en) | Cosmetic composition containing an extract of Lespedeza bicolor Turcz., Glechoma hederacea var. longituba Nakai and Portulaca grandiflora Hooker for anti-oxidative and anti-inflammatory activity | |
| JP2015086189A (en) | Hyaluronidase inhibitors and external preparations for moisturizing, anti-aging or anti-inflammation of skin formulated therewith | |
| CN109512735B (en) | External plant extract with whitening and skin brightening effects, cosmetic and preparation method thereof | |
| CN109512891B (en) | External plant extract and cosmetic with effect of relieving senile skin chapping and itching and preparation method thereof | |
| CN110090180B (en) | Cosmetic lithospermum extract and preparation method thereof | |
| KR100817876B1 (en) | Isolation process for proanthocyanidin from the bark of pine tree | |
| JP2007238455A (en) | Humectant, cell activator and bleaching agent | |
| KR20150132754A (en) | A preparation method of an extract of Saliconia Herbacea L having antioxidant and antimicrobial activity | |
| KR101676292B1 (en) | Cosmetic composition comprising an mixed extract of tangle, okra and yam and manufacturing method thereof | |
| CN109512732B (en) | External plant extract and cosmetic with skin barrier repairing effect and preparation method thereof | |
| CN109512733B (en) | External plant extract and cosmetic with effects of nourishing and moistening hand skin and preparation method thereof | |
| CN109512755B (en) | External plant extract with nourishing, repairing, softening and hair brightening effects, head care product and preparation method thereof | |
| WO2004112813A1 (en) | Litchi sinensis extracts containing oligomeric proanthocyanidins | |
| KR20150132753A (en) | A preparation method of a leaf extract of Morus alba having antioxidant and antimicrobial activity | |
| JP4748962B2 (en) | Moisturizer, cell activator, whitening agent, and antioxidant | |
| JP2008024664A (en) | Hyaluronidase inhibitor | |
| CN107079935A (en) | A kind of preparation method of succulent special-purpose insecticide | |
| Haron | Enzymatic extraction of ficus deltoidea for better enhancement of extracted yield | |
| KR20230052731A (en) | Wrinkle improvement functional cosmetic composition using propolis supercritical extract mixed with propolis of different origins and supercritical extract residues and manufacturing method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |