CN116942544A - Tricholoma matsutake alcohol-containing microcapsule with anti-aging effect and preparation method and application thereof - Google Patents
Tricholoma matsutake alcohol-containing microcapsule with anti-aging effect and preparation method and application thereof Download PDFInfo
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- CN116942544A CN116942544A CN202311018303.1A CN202311018303A CN116942544A CN 116942544 A CN116942544 A CN 116942544A CN 202311018303 A CN202311018303 A CN 202311018303A CN 116942544 A CN116942544 A CN 116942544A
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- Prior art keywords
- tricholoma matsutake
- microcapsule
- alcohol
- matsutake alcohol
- tricholoma
- Prior art date
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Abstract
The invention relates to an anti-aging tricholoma matsutake alcohol microcapsule, a preparation method and application thereof. According to the invention, the complex enzyme enzymolysis and the water extraction method are combined, and then ultrasonic extraction is carried out, so that the yield of the tricholoma matsutake alcohol in the tricholoma matsutake can be greatly improved, and the method can well retain the tricholoma matsutake alcohol substances in the tricholoma matsutake; further microencapsulation of Tricholoma matsutake extract containing Tricholoma matsutake alcohol can improve oxidation stability of Tricholoma matsutake extract containing Tricholoma matsutake alcohol, and retain more active components of Tricholoma matsutake alcohol. The tricholoma matsutake alcohol microcapsule prepared by the invention can fully play the effects of eliminating free radicals and resisting aging of tricholoma matsutake alcohol, improve the effects of skin inflammation while resisting aging, has high purity of microcapsule components, good stability, convenient dispersion and direct addition, and simultaneously has higher activity. Meanwhile, after the emulsifier is adopted in the microcapsule prepared by the invention, the appearance of the microcapsule is more rich, waste is not generated in the preparation process, and the microcapsule is low in energy consumption, green, efficient and safe.
Description
Technical Field
The invention belongs to the technical field of cosmetics. More particularly, relates to a tricholoma matsutake alcohol-containing microcapsule with anti-aging effect, and a preparation method and application thereof.
Background
Tricholoma matsutake (Tricholoma matsutake (lto et lmai) Sing) is also called Tricholoma matsutake, matsutake Mushroom, etc., and Tricholoma matsutake of Tricholomataceae is mycorrhizal fungi exogenesis of trees such as Quercus matsutake, etc., and rare and precious natural medicinal fungi in the world are known as "king in fungi", and Chinese secondary endangered species are protected. Tricholoma matsutake is a fungus with homology of medicine and food, and contains abundant saccharide, amino acid and polypeptide, volatile substances, vitamins, minerals, and lipid substances, wherein Tricholoma matsutake polysaccharide, tricholoma matsutake polypeptide, and Tricholoma matsutake alcohol are main active substances of Tricholoma matsutake. The tricholoma matsutake has the pharmacological effects of resisting radiation, regulating immunity, whitening skin, resisting photoaging, resisting diabetes, resisting hypertension, regulating intestines and stomach, resisting oxidation, resisting cancer, resisting tumor and the like, and has high edible and medicinal values.
The skin is the largest organ of the human body, and the most important function is the barrier function, namely, the damage to the skin caused by external stimulus is prevented, and meanwhile, the water loss in the skin is prevented. With natural aging, progressive mitochondrial dysfunction occurs during aging, which increases ROS (reactive oxygen species) production, which can further lead to worsening mitochondrial function and overall cell damage. In the natural aging process, skin injury caused by ultraviolet radiation (UVB) is the most common, UVB can damage the dermis layer, collagen is damaged, elastic fiber is problematic, skin becomes loose, wrinkles appear, when photoaging is serious, the wrinkles appear on the skin and are difficult to recover through skin care products, expression lines are accumulated day by day, so that the skin is in an old state, and the expression lines are an important factor for the skin to be in an aging state.
The active ingredients of the cosmetics with the anti-aging effect at present mainly comprise retinol and derivatives thereof, bakuchiol, fermentation products of some natural products and the like. However, these ingredients are often poor in stability, large in skin irritation, and complicated in preparation process, which results in a problem of an increase in raw material cost. The tricholoma matsutake alcohol is an anticancer oxidation active substance in the tricholoma matsutake extract, only exists in the tricholoma matsutake body, not only has good antioxidant function, but also has strong anti-aging capability. The tricholoma matsutake alcohol is mainly obtained by extracting tricholoma matsutake, but the extraction rate of the tricholoma matsutake alcohol in the prior art is extremely low and is mostly below 0.05%. And the tricholoma matsutake alcohol is sensitive to light, heat and oxidizing agents and is easily damaged by oxidation, so that the application of the tricholoma matsutake extract in anti-aging products is affected. Based on the unstable and easily degradable property of the tricholoma matsutake alcohol, the prior art has a new tricholoma matsutake alcohol product which is used for extracting the tricholoma matsutake alcohol independently, and the application of the tricholoma matsutake alcohol is limited. In order to improve stability and yield of matsutake alcohol, there is a need to develop more and better methods for extracting and preparing matsutake alcohol products, providing more efficient anti-aging related natural products.
Disclosure of Invention
The invention aims to overcome the defects and the shortcomings of the traditional tricholoma matsutake alcohol product and provide the tricholoma matsutake alcohol-containing microcapsule with anti-aging effect, and the preparation method and the application thereof.
The invention aims to provide a microcapsule containing tricholoma matsutake alcohol with anti-aging effect.
Another object of the present invention is to provide a method for preparing a microcapsule containing matsutake alcohol.
It is a further object of the present invention to provide the use of tricholoma matsutake alcohol-containing microcapsules.
The above object of the present invention is achieved by the following technical scheme:
the invention provides a microcapsule containing tricholoma matsutake alcohol with anti-aging effect, wherein the core material of the microcapsule is tricholoma matsutake extract; the wall material is one of soybean protein isolate-maltodextrin, maltodextrin-acacia and soybean protein isolate-acacia; the emulsifier is one of soybean lecithin and soybean lecithin-tween-20.
According to the invention, the yield of the tricholoma matsutake alcohol in the tricholoma matsutake can be greatly improved by adopting the complex enzyme enzymolysis and combining a water extraction method and then carrying out ultrasonic extraction, and the method can well retain the tricholoma matsutake alcohol substances in the tricholoma matsutake; further microencapsulation of Tricholoma matsutake extract containing Tricholoma matsutake alcohol can improve oxidation stability of Tricholoma matsutake extract containing Tricholoma matsutake alcohol, and retain more active components of Tricholoma matsutake alcohol. The tricholoma matsutake alcohol microcapsule prepared by the invention can fully play the effects of eliminating free radicals and resisting aging of tricholoma matsutake alcohol, improve the effects of skin inflammation while resisting aging, and can be used for resisting skin aging, improving skin inflammation and repairing skin injury caused by UV radiation. Meanwhile, after the emulsifier is adopted by the microcapsule prepared by the invention, the appearance of the microcapsule is more rich, waste is not generated in the preparation process, and the microcapsule is low in energy consumption, green, efficient and safe.
Preferably, the core material: wall material: the mass ratio of the components of the emulsifier is 1: (0.8-2): (0.001-0.1).
More preferably, the core material: wall material: the mass ratio of the components of the emulsifier is 1: (1-1.5): (0.005-0.1).
Further preferably, the core material: wall material: the mass ratio of the components of the emulsifier is 1:1.5: (0.005-0.1).
Preferably, the mass ratio of the components in the wall material is 1: (1-2).
More preferably, the wall material comprises the following components in percentage by mass: (1-1.5).
Further preferably, the wall material component is soy protein isolate and maltodextrin.
Preferably, when the emulsifier is soybean lecithin-tween-20, the mass ratio of the emulsifier is (1-1.5): 1
More preferably, the mass ratio of soybean lecithin-tween-20 is 1.5:1.
preferably, the matsutake alcohol extract of the core material is matsutake alcohol-containing matsutake extract.
The tricholoma matsutake alcohol is an active ingredient extracted from tricholoma matsutake grown in mountain, and is a specific ingredient in tricholoma matsutake, IUPAC name: 1-octen-3-ol (1-octen-3-ol) is a main component in the flavor of Tricholoma matsutake, and belongs to polycyclic hydroxyl diterpenoid compounds, and is composed of multiple cyclic structures. The tricholoma matsutake alcohol has good edible and medicinal values, has high antioxidant activity, has good effects of diminishing inflammation and delaying aging, and can improve immunity, resist tumor, reduce blood lipid and the like.
The invention provides a preparation method of tricholoma matsutake alcohol microcapsule, which comprises the following steps:
s1, preparing a tricholoma matsutake alcohol extract: taking dried matsutake, crushing and sieving, and mixing the materials according to a feed liquid ratio of 1:10-80 (g: mL), adding deionized water to obtain Tricholoma matsutake solution, performing enzymolysis with complex enzyme, performing ultrasonic extraction, separating supernatant, concentrating and collecting precipitate, and washing precipitate to obtain supernatant precipitate to obtain Tricholoma matsutake extract containing Tricholoma matsutake alcohol;
s2, preparing a wall material solution and an emulsifying agent;
s3, adding the tricholoma matsutake extract containing the tricholoma matsutake alcohol into the wall material solution, uniformly stirring, adding an emulsifying agent for emulsification, and performing spray drying to obtain the microcapsule containing the tricholoma matsutake alcohol.
Preferably, the feed liquid ratio in step S1 is 1:50 (g: mL).
Preferably, the complex enzyme enzymolysis in step S1 is: adjusting the pH to 7, adding a complex enzyme: trypsin, pectase and cellulase, wherein the addition amount of the compound enzyme is 3-5% of the volume of the extracted Tricholoma matsutake solution, the enzymolysis time is 90-180min, and the enzymolysis temperature is 10-60 ℃.
More preferably, the mass ratio of the trypsin, the pectase and the cellulase is 1:1:1, the enzymolysis temperature is 35 ℃, and the enzymolysis time is 120min.
Preferably, the ultrasonic extraction in step S1 is: the ultrasonic power is 200-500W, the extraction temperature is 60-80 ℃, and the extraction time is 1-3h.
More preferably, the ultrasonic power is 250W, the extraction temperature is 60 ℃, and the extraction time is 3h.
Preferably, in the step S2, maltodextrin and soy protein isolate are used as wall materials, and the mass ratio is 1: (1-1.5).
As a most preferred embodiment, the present invention provides a specific preparation method of tricholoma matsutake alcohol microcapsule:
(1) Preparation of the antler extract: preparing Cheng Songrong decoction pieces with dried Tricholoma matsutake, pulverizing decoction pieces to obtain Tricholoma matsutake powder, and sieving with 80 mesh sieve. Taking a certain amount of matsutake Mushroom powder, adding distilled water in a mass ratio of 1:50 (g: mL) to deionized water, adjusting pH to 7 and temperature to 35 ℃, adding trypsin, pectase and cellulase accounting for 3.5% of the mass (g) of the solution (the mass ratio is 1:1:1), performing enzymolysis for 120min, and performing ultrasonic water bath at 60 ℃ and 250W for 3h. Centrifuging at 6000r/min for 0min, separating to obtain supernatant, rotary evaporating, and concentrating to 1/3 of original volume. The precipitate was then collected, precipitate 1: slowly adding 95% ethanol with volume 3 times of that of the concentrated extract, and standing at 4deg.C for 12 hr; and centrifuging at 4000r/min for 0min, and collecting precipitate. Precipitation 2: adding 80% ethanol into the supernatant obtained by washing the precipitate 1, and standing at the temperature of 4 ℃ for 3 hours. Obtaining supernatant precipitate. Mixing the two precipitates to obtain Tricholoma matsutake extract.
(2) Preparing tricholoma matsutake alcohol microcapsules: the wall materials adopted in the embodiment are soy protein isolate and maltodextrin, and the mass ratio is 1:1.5; the emulsifying agent is soybean lecithin and tween-20, and the mass ratio is 1.5:1. taking the tricholoma matsutake extract prepared by the steps as a core material, and according to the core material: wall material: the mass ratio of the emulsifier is 1:1.5:0.0075. weighing a certain amount of soybean protein isolate and maltodextrin, dissolving in water at 60deg.C, maintaining the temperature of the mixed solution at about 60deg.C, and stirring for 20min. Slowly adding Tricholoma matsutake extract containing Tricholoma matsutake alcohol, stirring for 15min, and emulsifying with emulsifying machine at 6500r/min to obtain emulsion. And then drying the prepared emulsion by controlling proper flow through a peristaltic pump, wherein the air outlet temperature is about 90 ℃, and simultaneously collecting microcapsule products through the outlet of a cyclone separator of a spray dryer to obtain the tricholoma matsutake alcohol microcapsule.
The invention also provides application of the tricholoma matsutake alcohol-containing microcapsule in resisting aging, improving skin inflammation and repairing skin injury caused by UV radiation, or in preparing a product for resisting skin aging, improving skin inflammation and repairing skin injury caused by UV radiation.
Furthermore, the invention also provides an anti-aging skin care product containing the tricholoma matsutake alcohol microcapsule, wherein the product is cream, emulsion or essence, and the product also contains a preparation which is used together with skin care and is conventional in the field.
Preferably, the product is a face cream, and comprises the following components in percentage by mass: the matsutake alcohol microcapsule provided by the invention comprises 0.4wt% of ceramide 0.4wt%, lecithin 2.0wt%, phytosterol 0.5wt%, polyol 6.5wt%, chelating agent 0.3wt%, thickener 3wt%, emulsifier 3.5wt%, emollient 19.0wt%, fatty alcohol 5wt%, skin conditioner 2wt%, antioxidant 0.01wt%, preservative 0.01wt%, essence 1.0wt% and deionized water to 100.0wt%; wherein the lecithin is one or more selected from lecithin, hydrogenated lecithin and hydroxylated lecithin.
Preferably, the product is emulsion and contains the following components in percentage by mass: the tricholoma matsutake alcohol microcapsule provided by the invention comprises 1.0wt% of glycerin 30.0wt%, sorbitol stearate 5.0wt%, sucrose cocoate 2.0wt%, dioctyl carbonate 4.0wt%, paraffin 3.0wt%, citric acid 3.0wt%, vitamin C0.1wt%, sodium stearate 1.0wt% and deionized water to 100.0wt%.
Preferably, the product is essence, and contains the following components in percentage by mass: 6.0 weight percent of tricholoma matsutake alcohol microcapsule and 40.0 weight percent of butanediol; deionized water to 100.0wt%.
The invention has the following beneficial effects:
the invention provides a microcapsule containing tricholoma matsutake alcohol with anti-aging effect and a preparation method and application thereof, and the microcapsule containing tricholoma matsutake alcohol is subjected to enzymolysis by adopting complex enzyme, combined with a water extraction method and then subjected to ultrasonic extraction, so that the yield of the tricholoma matsutake alcohol in the tricholoma matsutake can be greatly improved, and the method can well retain the tricholoma matsutake alcohol substances in the tricholoma matsutake; further microencapsulation of Tricholoma matsutake extract containing Tricholoma matsutake alcohol can improve oxidation stability of Tricholoma matsutake extract containing Tricholoma matsutake alcohol, and retain more active components of Tricholoma matsutake alcohol. The tricholoma matsutake alcohol microcapsule prepared by the invention can fully play the effects of eliminating free radicals and resisting aging of tricholoma matsutake alcohol, improve the effects of skin inflammation while resisting aging, and can be used for resisting skin aging, improving skin inflammation and repairing skin injury caused by UV radiation. Meanwhile, after the emulsifier is adopted by the microcapsule prepared by the invention, the appearance of the microcapsule is more rich, waste is not generated in the preparation process, and the microcapsule is low in energy consumption, green, efficient and safe.
The invention provides more methods for improving the extraction efficiency and the extraction efficacy of specific active ingredients in the tricholoma matsutake extract, provides a basis for preparing products with good quality and good effect and simultaneously provides a thought for the application of volatile active ingredients such as tricholoma matsutake alcohol in anti-aging products.
Drawings
FIG. 1 is a graph showing the results of an in vitro transdermal performance test.
Detailed Description
The invention is further illustrated in the following drawings and specific examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Reagents and materials used in the following examples are commercially available unless otherwise specified.
The tricholoma matsutake decoction pieces adopted by the invention are derived from Shangri-La of Yunnan, are obtained by slicing and drying fruiting bodies of fresh tricholoma matsutake into medicinal materials, and are subjected to liquid nitrogen freezing treatment to obtain ultrathin slices with the thickness of 1-5 mu m.
Tween-20 and soybean lecithin used in the following experiments were all obtained fromFor analytically pure grade; soy protein isolate was purchased from Rui He source power suppliers, food grade; maltodextrin was purchased from the commercial company, inc. of the public welfare, food grade.
EXAMPLE 1 preparation of Tricholoma matsutake alcohol extract
In the embodiment, a large number of optimization experiments are used for screening the tricholoma matsutake alcohol extraction method, so that the extraction method and the parameter steps thereof have a large influence on the extraction yield of the tricholoma matsutake alcohol. The invention adopts a complex enzyme method combined with a water extraction method for extraction, and single factor condition optimization shows that the complex enzyme adopts trypsin, pectase and cellulase, the mass ratio of the complex enzyme is 1:1:1, the enzymolysis time is 120min, the enzymolysis temperature is 35 ℃, the addition amount of the complex enzyme is 3.5 percent of the volume of the extracted tricholoma matsutake solution, and the extraction rate of tricholoma matsutake alcohol is highest; the conditions for enzymolysis are as follows: the enzymolysis time is 90-180min, the enzymolysis temperature is 10-60 ℃, the adding amount of the compound enzyme is 3-5% of the volume of the extracted tricholoma matsutake solution, and the specific extraction method is as follows:
preparing Cheng Songrong decoction pieces with dried Tricholoma matsutake, pulverizing decoction pieces to obtain Tricholoma matsutake powder, and sieving with 80 mesh sieve. Taking a certain amount of matsutake Mushroom powder, adding distilled water, mixing with deionized water at a ratio of 1:50 (g: mL), adjusting pH to 7, and temperature to 35deg.C, adding trypsin, pectase and cellulase (at a mass ratio of 1:1:1) accounting for 3.5% of the matsutake Mushroom solution mass (g), performing enzymolysis for 120min, and performing ultrasonic water bath at 60deg.C and 250W for 3 hr. Centrifuging at 6000r/min for 0min, separating to obtain supernatant, rotary evaporating, and concentrating to 1/3 of original volume.
The precipitate was then collected, precipitate 1: slowly adding 95% ethanol with volume 3 times of that of the concentrated extract, and standing at 4deg.C for 12 hr; and centrifuging at 4000r/min for 0min, and collecting precipitate.
Precipitation 2: adding 80% ethanol into the supernatant obtained by washing the precipitate 1, and standing at the temperature of 4 ℃ for 3 hours. Obtaining supernatant precipitate. Mixing the two precipitates to obtain Tricholoma matsutake extract.
The parameter conditions of the extraction method are adjusted according to the above extraction steps, and the adjustment parameters of different extraction methods are shown in the following table 1, and the matsutake mushroom extracts are prepared respectively.
TABLE 1 extraction conditions and methods for obtaining the extraction yield of Tricholoma matsutake alcohol
And then ultraviolet spectroscopic calibration method is adopted to calibrate the content of the effective substances (the extraction rate of the tricholoma matsutake alcohol), and meanwhile, the extraction rates of the tricholoma matsutake alcohol prepared in the subsequent comparative example 1 and comparative example 2 are measured (namely, the conventional extraction method in the field). Tricholoma matsutake alcohol content% (g/g) =absorbance standard curve corresponds to amount x dilution/extract sample mass x 100%.
The results of the extraction rate of the tricholoma matsutake alcohol are shown in table 1, and the tricholoma matsutake alcohol content extracted by the combination of the complex enzyme method and the water method is obviously higher than that of the conventional water extraction method and alcohol extraction method. Meanwhile, the parameter conditions of the extraction method are optimized, and the extraction processes such as feed-liquid ratio, time and extraction temperature are changed to perform comparison, so that the tricholoma matsutake alcohol can be better obtained only by extraction under specific conditions, and the yield is higher; the extraction time is not enough, so the extraction time is more than 1h, the ultrasonic power, the extraction temperature and the like can influence the extraction effect, and the optimal extraction conditions are as follows: the ratio of the feed liquid is 1:10-80, the ultrasonic power is 200-500W, the extraction temperature is 60-80 ℃, and the extraction time is 1-3h.
EXAMPLE 2 preparation of Tricholoma matsutake alcohol microcapsules
The matsutake extract prepared in example 1 was used as a core material, and extraction was performed using the above-mentioned optimum parameters. The materials subjected to microencapsulation were then screened, the tricholoma matsutake extract was embedded using different wall materials and emulsifier combinations as shown in table 2 below, the tricholoma matsutake extract containing tricholoma matsutake alcohol as the core material was slowly added to the wall materials, and then the emulsifier was added for emulsification. After stirring, emulsifying by an emulsifying machine under the condition of 6500r/min to ensure that the emulsification is complete. And then drying the prepared emulsion by controlling proper flow through a peristaltic pump, wherein the air outlet temperature is about 90 ℃, and simultaneously collecting microcapsule products through the outlet of a cyclone separator of a spray dryer to obtain the tricholoma matsutake alcohol microcapsule.
TABLE 2 arrangement of different wall materials and emulsifiers
The wall material combinations of the above Table 2 were combined with the Tricholoma matsutake extract, and the ratio of the wall material to the emulsifier was optimized by measuring the embedding rate. The microencapsulation effect is measured by the embedding rate: embedding rate= (1-oil content of microcapsule surface/total oil content of microcapsule) ×100%. Microcapsule surface oil content: accurately weighing 4.5g of the product prepared after microencapsulation, adding 20mL of petroleum ether, shaking for dissolving, filtering, repeating for 2 times, combining filtrates, volatilizing the total filtrate at room temperature, and weighing. Determination of total oil of microcapsules: accurately weighing 4.5g of the product prepared after microencapsulation, mashing the microcapsules, fully dissolving the microcapsules by using normal hexane as a solvent, and measuring the total oil content of the microcapsule product by using a Soxhlet extraction method.
The statistical results are shown in table 3 below, and show that the isolated soy protein is obtained under conditions that maintain the extraction process of the matsutake extract unchanged: the mass ratio of maltodextrin is 1:1.5, soybean lecithin: the mass ratio of tween-20 is 1.5:1. wall material: the mass ratio of the emulsifying agent is 1: at 0.0075, the entrapment rate of Tricholoma matsutake extract reaches the optimum level. The reason is that the film forming speed is increased along with the increase of the wall material quantity, so that the loss of the core material is reduced, and the microcapsule efficiency is improved, but if the proportion of the core material to the wall material is continuously reduced, the efficiency is reduced, and the reason is that the wall material quantity is too high, the drying speed is reduced, the loss of the core material is increased, and meanwhile, the diffusion loss of some core materials during embedding can reduce the microcapsule inclusion rate. The embedding effect of the combination of the soybean protein isolate and the maltodextrin is obviously superior to that of other compositions, and the soybean protein isolate has good film forming property and emulsifying property, so that a smooth film is formed on the surface of the microcapsule in the drying process, and meanwhile, the maltodextrin covers the surface of the protein film, so that the thickness, strength and density of the microcapsule are increased, and the diffusion and migration of the surfaces of a core material and a wall material and the compactness of the microcapsule are relatively reduced. The influence of the increase of the proportion of the isolated soy protein still needs to be further verified by experiments.
TABLE 3 influence of different wall Material and emulsifier combinations on the encapsulation efficiency of microcapsules
| Case (B) | Embedding rate% | Case (B) | Embedding rate% |
| Case 1 | 64.51 | Case 7 | 80.56 |
| Case 2 | 75.62 | Case 8 | 77.39 |
| Case 3 | 84.44 | Case 9 | 60.01 |
| Case 4 | 79.62 | Case 10 | 61.23 |
| Case 5 | 62.53 | Case 11 | 70.75 |
| Case 6 | 72.14 | Case 12 | 65.33 |
The mass ratio of the core material to the wall material has an influence on the microencapsulation efficiency of the tricholoma matsutake alcohol: the wall material adopts soybean protein isolate and maltodextrin with the proportion of 1:1.5, the total solid content of the emulsion is 16.67%, the emulsification temperature is 60 ℃, and the core wall ratios are respectively 1:0.8, 1:1. 1:1.25, 1:1.5,1:2, the influence of the mass ratio of the core material to the wall material on the microencapsulation efficiency was further studied, and the specific proportions and measurement results are shown in table 4 below. The results show that the mass ratio of core/wall material is 1:0.8 is reduced to 1: in the process of 1.5, the microencapsulation efficiency is gradually improved, and the mass ratio of the core material to the wall material is 1: the efficiency is highest at 1.5.
TABLE 4 influence of core to wall mass ratio on the efficiency of microencapsulation of matsutake alcohol
| Core/wall mass ratio | Embedding rate% |
| 1：0.8 | 76.02 |
| 1：1 | 78.96 |
| 1：1.125 | 82.03 |
| 1：1.5 | 84.44 |
| 1：2 | 76.35 |
The total solid content of the emulsion (namely the dosage of the emulsifier) has an influence on the microencapsulation efficiency of the tricholoma matsutake alcohol: the mass of the core material and the wall material is 1:1.5, the wall material adopts soybean protein isolate and maltodextrin with the proportion of 1:1. the effect of the total solid content of the emulsion on the microencapsulation efficiency was further studied at 60 ℃ under the conditions that the total solid content of the emulsion was 13.33%,15%,16.67%,18% and 20%, respectively, and the specific proportions and measurement results are shown in table 5 below. As can be seen from Table 5, the embedding rate increased with increasing emulsion concentration, and reached the highest when the total solids were 16.67%. The reason is that the increase of the concentration of the emulsion reduces the water content in the emulsion, accelerates the film forming speed of liquid drops in the vacuum drying process, and is beneficial to the formation of microcapsule walls and the increase of the density of the microcapsule walls. However, if the emulsion concentration is further increased, the packing rate is reduced because the emulsion curing concentration is too high, which results in too thick emulsion, which is unfavorable for forming microcapsule film, the drying speed is slow, and even coking phenomenon occurs.
TABLE 5 influence of the total solids content of the emulsion on the efficiency of microencapsulation of matsutake alcohol
| Total solids content | Embedding rate% |
| 13.33 | 65.32 |
| 15 | 72.32 |
| 16.67 | 80.03 |
| 18 | 78.63 |
| 20 | 75.41 |
In summary, only by adopting specific wall materials, emulsifying agents, mass ratio of core materials to wall materials and total solid content of emulsion, the microencapsulation efficiency can be further improved, and the embedding efficiency of the tricholoma matsutake alcohol extract can be improved.
EXAMPLE 3 Tricholoma matsutake alcohol microcapsule
(1) Preparing tricholoma matsutake extract: preparing Cheng Songrong decoction pieces with dried Tricholoma matsutake, pulverizing decoction pieces to obtain Tricholoma matsutake powder, and sieving with 80 mesh sieve. Taking a certain amount of matsutake Mushroom powder, adding distilled water, wherein the ratio of the mass of the sample to the deionized water is 1:50 (g: mL), adjusting the pH to 7, the temperature to 35 ℃, adding trypsin, pectase and cellulase accounting for 3.5% of the mass (g) of the solution (the mass ratio is 1:1:1), performing enzymolysis for 120min, and performing ultrasonic water bath at 60 ℃ and 250W for 3h. Centrifuging at 6000r/min for 0min, separating to obtain supernatant, rotary evaporating, and concentrating to 1/3 of original volume. The precipitate was then collected, precipitate 1: slowly adding 95% ethanol with volume 3 times of that of the concentrated extract, and standing at 4deg.C for 12 hr; and centrifuging at 4000r/min for 0min, and collecting precipitate. Precipitation 2: adding 80% ethanol into the washing supernatant, precipitating with ethanol at 4deg.C for 3 hr. Obtaining supernatant precipitate. Mixing the two precipitates to obtain Tricholoma matsutake extract containing Tricholoma matsutake alcohol.
(2) Preparing tricholoma matsutake alcohol microcapsules: the wall materials adopted in the embodiment are soy protein isolate and maltodextrin, and the mass ratio is 1:1.5; the emulsifying agent is soybean lecithin and tween-20, and the mass ratio is 1.5:1. taking the tricholoma matsutake extract prepared by the steps as a core material. According to the core material: wall material: the mass ratio of the emulsifier is 1:1.5:0.0075. weighing a certain amount of soybean protein isolate and maltodextrin, dissolving in water at 60deg.C, maintaining the temperature of the mixed solution at about 60deg.C, and stirring for 20min. Slowly adding Tricholoma matsutake extract containing Tricholoma matsutake alcohol, stirring for 15min, and emulsifying with emulsifying machine at 6500r/min to obtain emulsion. And then drying the prepared emulsion by controlling proper flow through a peristaltic pump, wherein the air outlet temperature is about 90 ℃, and simultaneously collecting microcapsule products through the outlet of a cyclone separator of a spray dryer to obtain the tricholoma matsutake alcohol microcapsule.
EXAMPLE 4 Tricholoma matsutake alcohol microcapsule
(1) Preparation of the antler extract: preparing Cheng Songrong decoction pieces with dried Tricholoma matsutake, pulverizing decoction pieces to obtain Tricholoma matsutake powder, and sieving with 80 mesh sieve. Taking a certain amount of matsutake Mushroom powder, adding distilled water, wherein the ratio of the mass of the sample to the deionized water is 1:50 (g: mL), adjusting the pH to 7, the temperature to 35 ℃, adding trypsin, pectase and cellulase accounting for 3.5% of the mass (g) of the solution (the mass ratio is 1:1:1), performing enzymolysis for 120min, and performing ultrasonic water bath at 60 ℃ and 250W for 3h. Centrifuging at 6000r/min for 0min, separating to obtain supernatant, rotary evaporating, and concentrating to 1/3 of original volume. The precipitate was then collected, precipitate 1: slowly adding 95% ethanol with volume 3 times of that of the concentrated extract, and standing at 4deg.C for 12 hr; and centrifuging at 4000r/min for 0min, and collecting precipitate. Precipitation 2: adding 80% ethanol into the washing supernatant, precipitating with ethanol at 4deg.C for 3 hr. Obtaining supernatant precipitate. Mixing the two precipitates to obtain Tricholoma matsutake extract containing Tricholoma matsutake alcohol.
(2) Preparing tricholoma matsutake alcohol microcapsules: the wall materials adopted in the embodiment are soy protein isolate and maltodextrin, and the mass ratio is 1:1.5; the emulsifying agent is soybean lecithin and tween-20, and the mass ratio is 1.5:1. taking the tricholoma matsutake extract prepared by the steps as a core material. According to the core material: wall material: the mass ratio of the emulsifier is 1:1.5:0.005. weighing a certain amount of soybean protein isolate and maltodextrin, dissolving in water at 60deg.C, maintaining the temperature of the mixed solution at about 60deg.C, and stirring for 20min. Slowly adding Tricholoma matsutake extract containing Tricholoma matsutake alcohol, stirring for 15min, and emulsifying with emulsifying machine at 6500r/min to obtain emulsion. And then drying the prepared emulsion by controlling proper flow through a peristaltic pump, wherein the air outlet temperature is about 90 ℃, and simultaneously collecting microcapsule products through the outlet of a cyclone separator of a spray dryer to obtain the tricholoma matsutake alcohol microcapsule.
EXAMPLE 5 Tricholoma matsutake alcohol microcapsule
(1) Preparation of the antler extract: preparing Cheng Songrong decoction pieces with dried Tricholoma matsutake, pulverizing decoction pieces to obtain Tricholoma matsutake powder, and sieving with 80 mesh sieve. Taking a certain amount of matsutake Mushroom powder, adding distilled water, wherein the ratio of the mass of the sample to the deionized water is 1:50 (g: mL), adjusting the pH to 7, the temperature to 35 ℃, adding trypsin, pectase and cellulase accounting for 3.5% of the mass (g) of the solution (the mass ratio is 1:1:1), performing enzymolysis for 120min, and performing ultrasonic water bath at 60 ℃ and 250W for 3h. Centrifuging at 6000r/min for 0min, separating to obtain supernatant, rotary evaporating, and concentrating to 1/3 of original volume. The precipitate was then collected, precipitate 1: slowly adding 95% ethanol with volume 3 times of that of the concentrated extract, and standing at 4deg.C for 12 hr; and centrifuging at 4000r/min for 0min, and collecting precipitate. Precipitation 2: adding 80% ethanol into the washing supernatant, precipitating with ethanol at 4deg.C for 3 hr. Obtaining supernatant precipitate. Mixing the two precipitates to obtain Tricholoma matsutake extract containing Tricholoma matsutake alcohol.
(2) Preparing tricholoma matsutake alcohol microcapsules: the wall materials adopted in the embodiment are soy protein isolate and maltodextrin, and the mass ratio is 1:1.5; the emulsifying agent is soybean lecithin and tween-20, and the mass ratio is 1.5:1. taking the tricholoma matsutake extract prepared by the steps as a core material. According to the core material: wall material: the mass ratio of the emulsifier is 1:1.5:0.01. weighing a certain amount of soybean protein isolate and maltodextrin, dissolving in water at 60deg.C, maintaining the temperature of the mixed solution at about 60deg.C, and stirring for 20min. Slowly adding Tricholoma matsutake extract containing Tricholoma matsutake alcohol, stirring for 15min, and emulsifying with emulsifying machine at 6500r/min to obtain emulsion. And then drying the prepared emulsion by controlling proper flow through a peristaltic pump, wherein the air outlet temperature is about 90 ℃, and simultaneously collecting microcapsule products through the outlet of a cyclone separator of a spray dryer to obtain the tricholoma matsutake alcohol microcapsule.
Comparative example 1 preparation of Tricholoma matsutake extract by aqueous extraction
Adding distilled water into the same processed Tricholoma matsutake slices as in example 1 at a feed liquid ratio of 1:10, heating in water bath at 80deg.C for 2 hr, extracting for 2 times, filtering, lyophilizing, and pulverizing to obtain Tricholoma matsutake water extract.
Comparative example 2 alcohol extraction method for preparing Tricholoma matsutake extract
The pine mushroom slices treated in the same way as in the example 1 are added with 75% ethanol solution according to a feed liquid ratio of 1:10, heated and extracted for 2 hours in a water bath at 80 ℃ for 2 times, and then filtered by suction and steamed by rotary evaporation to obtain the pine mushroom alcohol extract.
Comparative example 3
The preparation method of the tricholoma matsutake extract is the same as that of example 3, and the only difference is that the mass ratio of the core material to the wall material is 1:3, and no emulsifier.
Comparative example 4
The preparation method of the tricholoma matsutake extract is the same as that of example 3, except that the subsequent microencapsulation is not adopted.
Test example 1 inhibition of non-enzymatic glycosylation reaction by Tricholoma matsutake alcohol microcapsules
To 100ml of phosphate buffer solution of 0.2mol/L at pH=7.4, 19.82g of glucose, 0.4024g of bovine serum albumin and 0.39g of sodium azide were added, and the mixture was mixed to form a reaction solution. Taking a plurality of test tubes, sequentially adding 4mL of reaction solution and the tricholoma matsutake extracting solutions with different concentrations into each test tube (the tricholoma matsutake alcohol microcapsule adopts examples 3-5, the tricholoma matsutake alcohol microcapsule prepared by reference example 3 of the extracts 2-5 in comparative examples 1-3 and the tricholoma matsutake extracting solution containing the tricholoma matsutake alcohol of comparative example 4), and dissolving and mixing the tricholoma matsutake extract into an ethanol solution with 50% volume fraction by using absolute ethanol with analytical grade so that the total volume of the solutions in all the test tubes is 5mL. And the initial fluorescence values of all the samples are measured by adopting a fluorescence spectrophotometer, then all the test tubes are placed in a water bath at 37 ℃ and kept away from light for 7d, the fluorescence values of the samples in all the test tubes are measured, and after all the test tubes are kept away from light for 7d in the water bath at 37 ℃, the fluorescence values are measured. The test conditions were: excitation wavelength is 370nm, and slit is 5nm; the emission wavelength ranges from 380 nm to 500nm, and the slits are 5nm; the light source voltage is 700V. The inhibition ratio was calculated using the obtained fluorescence data, and the calculation formula was IR (inhibition ratio) =1-F (1-5) /F6, (F is notFluorescence value of the same tube).
The measurement results of the non-enzymatic glycosylation reaction are shown in Table 6 below, and there is a close relationship between the non-enzymatic glycosylation and the oxidation reaction, which is a middle and late stage of the non-enzymatic glycosylation reaction, and promotes the oxidation reaction at the same time. The data in each group in Table 6 show that the stability of the tricholoma matsutake alcohol can be obviously improved after microencapsulation treatment, and the tricholoma matsutake alcohol microcapsule prepared by the invention has better antioxidant activity, can effectively inhibit non-enzymatic glycosylation reaction, and has a certain dose-dependent effect; wherein the tricholoma matsutake alcohol microcapsule treated in the embodiment 3 has better non-enzymatic glycosylation inhibition activity, and the inhibition rates respectively reach 38.45%, 63.48% and 86.87%. The microcapsule treatment effectively improves the stability of the tricholoma matsutake alcohol, and the stability of the polycyclic hydroxyl diterpenoid compound has positive effect on scavenging free radicals; the tricholoma matsutake alcohol microcapsule with larger specific surface area can provide a plurality of sites combined with free radicals, shield or stop the free radicals, effectively inhibit oxidation reaction initiated by the free radicals, and finally improve the non-enzymatic glycosylation inhibition effect.
TABLE 6 inhibition of non-enzymatic glycosylation by Tricholoma matsutake alcohol microcapsules
Test example 2 action of Tricholoma matsutake alcohol microcapsules on scavenging free radicals
Measuring DPPH free radical scavenging ability of Tricholoma matsutake extract microcapsule, taking several test tubes, adding 2mL of 0.1mmol of DPPH solution into each test tube, placing the test tubes in ice water bath in the dark, and sequentially adding Tricholoma matsutake alcohol microcapsule with different concentrations (Tricholoma matsutake alcohol microcapsule adopts examples 3-5, tricholoma matsutake alcohol microcapsule prepared from extracts 2-5 in comparative examples 1-3 and 1 and reference example 3, and Tricholoma matsutake extract containing Tricholoma matsutake alcohol in comparative example 4) and absolute ethanol, so that total volume of the solutions in each test tube is 4mL. After reaction in the dark for 30min, the absorbance of each sample at 517nm was measured by an ultraviolet-visible spectrophotometer using absolute ethyl alcohol as a reference.
The measurement results of the free radical scavenging effect are shown in the following table 7, and show that the tricholoma matsutake alcohol microcapsule prepared by the invention has better free radical scavenging effect, the DPPH free radical scavenging rate is 24.34-93.37% within the polysaccharide concentration of 0.2-1 mg/m L, the scavenging rate increases with the increase of the concentration, and the obvious dose-effect relationship exists.
TABLE 7 scavenging action of Tricholoma matsutake alcohol microcapsules on free radicals
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Test example 3 protection of Tricholoma matsutake alcohol microcapsules against oxidative stress and inflammation
Oxidative stress and inflammation are major factors causing photodamage to the skin. Further study was performed by enzyme-linked immunosorbent assay (enzyme-linked immunosorbent assay, ELISA) by taking blank, model, and Tricholoma matsutake microcapsules of example 3 and setting different concentrations of treatments: skin tissue of mice treated with three concentration treatment groups of 1% low concentration (L), 5% medium concentration (M) and 10% high concentration (H), and vitamin E group was set as a positive control (the amounts of the treatment groups were the same). The skin tissue of the treated mice was homogenized, and the supernatant was obtained, and IL-1β, IL-6, COX-2, and TNF- α levels in the skin tissue homogenates were measured.
The results are shown in Table 8 below, and show that inflammatory factors IL-6 and TNF- α are significantly increased (P < 0.01) in the skin of the model group and IL-1β, COX-2 also have an upward trend under UVB induction compared to the blank group. Notably, example 3 microcapsules were able to significantly reduce IL-1 β in skin (P < 0.05), to significantly reduce IL-6 in skin to (63.34 ±44.14) pg/mL (P < 0.05), to significantly reduce COX-2 to (2.53±1.22) ng/mL (P < 0.05), and to significantly reduce tnfα to (4.95±3.39) pg/mL (P < 0.01) compared to the blank. Vitamin E was able to significantly reduce COX-2 and TNF- α levels (P < 0.05) compared to the model group. The microcapsule group of example 3 showed a decrease in IL-1β, IL-6, TNF- α, COX-2, but no statistical difference compared to the vitamin E group.
TABLE 8 influence of test substances on inflammatory factors in UVB-induced photo-aged skin of ICR mice
Note that: # indicates significant differences between groups.
In conclusion, the results show that the tricholoma matsutake alcohol microcapsule provided by the invention can obviously reduce the levels of oxidative stress and inflammatory factors IL-1 beta, IL-6, COX-2 and TNF-alpha, has positive correlation with the administration concentration, avoids causing skin photodamage, and has good protection effect on the skin damage of mice induced by UVB radiation.
Test example 4 in vitro transdermal Performance test
In order to compare the transdermal properties of the tricholoma matsutake alcohol microcapsules, the samples of examples 3, 4 and 5 were tested for transdermal properties by using the tricholoma matsutake extract prepared in comparative example 1 as a control group (without microencapsulation), and the residual amounts of the tricholoma matsutake extract in the horny layer, the active epidermis and the dermis after 24 hours of permeation were measured.
As shown in FIG. 1, the sample of example 3 showed higher levels of the extract of Tricholoma matsutake in the stratum corneum, the active epidermis and the dermis than the control group, and no Tricholoma matsutake extract was detected in the receiving solution, indicating that the Tricholoma matsutake extract was present in each layer of skin, and was mainly present in the active epidermis and the dermis. And the skin transmittance of the sample of example 3 was optimized.
Example 6 anti-aging skin care product
Based on the research, the invention also provides an anti-aging skin care product containing the tricholoma matsutake alcohol microcapsule, namely a facial cream, which comprises the following components in percentage by mass: example 3 Tricholoma matsutake alcohol microcapsule 0.4wt%, ceramide 0.4wt%, lecithin 2.0wt%, phytosterol 0.5wt%, polyol 6.5wt%, chelating agent 0.3wt%, thickener 3wt%, emulsifier 3.5wt%, emollient 19.0wt%, fatty alcohol 5wt%, skin conditioner 2wt%, antioxidant 0.01wt%, preservative 0.01wt%, essence 1.0wt%, deionized water to 100.0wt%; wherein the lecithin is one or more selected from lecithin, hydrogenated lecithin and hydroxylated lecithin.
Example 7 anti-aging skin care product
The embodiment provides an anti-aging skin care product-emulsion containing tricholoma matsutake alcohol microcapsules, which comprises the following components in percentage by mass: example 3 Tricholoma matsutake alcohol microcapsule 1.0wt%, glycerin 30.0wt%, sorbitol stearate 5.0wt%, sucrose cocoate 2.0wt%, dioctyl carbonate 4.0wt%, paraffin 3.0wt%, citric acid 3.0wt%, vitamin C0.1wt%, sodium stearate 1.0wt%, deionized water to 100.0wt%.
Example 8 anti-aging skin care product
The embodiment provides an anti-aging skin care product containing tricholoma matsutake alcohol microcapsules, namely essence, which comprises the following components in percentage by mass: example 3 Tricholoma matsutake alcohol microcapsule 6.0wt%, butylene glycol 40.0wt%; deionized water to 100.0wt%.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. A microcapsule containing tricholoma matsutake alcohol with anti-aging effect is characterized in that the core material of the microcapsule is tricholoma matsutake extract; the wall material is one of soybean protein isolate-maltodextrin, maltodextrin-acacia and soybean protein isolate-acacia; the emulsifier is one of soybean lecithin and soybean lecithin-tween-20.
2. The microcapsule according to claim 1, wherein the core material: wall material: the mass ratio of the emulsifier is 1: (0.8-2): (0.001-0.01).
3. The microcapsule according to claim 1, wherein the mass ratio of the components in the wall material is 1: (1-2).
4. A microcapsule according to claim 3, wherein the emulsifier is soybean lecithin and tween-20 in a mass ratio of (1-1.5): 1.
5. the microcapsule of claim 1, wherein the tricholoma matsutake extract is tricholoma matsutake extract containing tricholoma matsutake alcohol.
6. The method for preparing the tricholoma matsutake alcohol microcapsule according to any one of claims 1 to 5, comprising the following steps:
s1, preparing a tricholoma matsutake alcohol extract: taking dried matsutake, crushing and sieving, and mixing the materials according to a feed liquid ratio of 1:10-80 (g: mL), adding deionized water to obtain Tricholoma matsutake solution, performing enzymolysis with complex enzyme, performing ultrasonic extraction, separating supernatant, concentrating and collecting precipitate, and washing precipitate to obtain supernatant precipitate to obtain Tricholoma matsutake extract containing Tricholoma matsutake alcohol;
s2, preparing a wall material solution and an emulsifying agent;
s3, adding the tricholoma matsutake extract containing the tricholoma matsutake alcohol into the wall material solution, uniformly stirring, adding an emulsifying agent for emulsification, and performing spray drying to obtain the microcapsule containing the tricholoma matsutake alcohol.
7. The preparation method according to claim 6, wherein the complex enzyme enzymolysis in step S1 is: adjusting the pH to 7, adding a complex enzyme: trypsin, pectase and cellulase, the mass ratio of the complex enzyme is 1:1:1, the adding amount of the compound enzyme is 3-5% of the volume of the extracted tricholoma matsutake solution, the enzymolysis time is 90-180min, and the enzymolysis temperature is 10-60 ℃.
8. The method according to claim 6, wherein the ultrasonic extraction conditions in step S1 are: the ultrasonic power is 200-500W, the extraction temperature is 60-80 ℃, and the extraction time is 1-3h.
9. The preparation method according to claim 6, wherein in the step S2, maltodextrin and soy protein isolate are used as the wall materials, and the mass ratio is 1: (1-1.5).
10. Use of the tricholoma matsutake alcohol-containing microcapsule according to any one of claims 1-5 for anti-aging, improving skin inflammation, repairing skin damage caused by UV radiation, or for the preparation of a product for anti-aging, improving skin inflammation, repairing skin damage caused by UV radiation.
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| CN115669945A (en) * | 2022-10-24 | 2023-02-03 | 上海艾斯顿医疗科技有限公司 | Liposome-coated polypeptide with neurotrophic effect, and preparation method and application thereof |
| CN116421482A (en) * | 2023-04-20 | 2023-07-14 | 稀物集(广州)生物科技有限公司 | Composition containing tricholoma matsutake extract with anti-aging effect and application thereof |
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| CN101744847A (en) * | 2009-12-10 | 2010-06-23 | 浙江大山合菇业有限公司 | Agaricus compound polysaccharide capsule preparation method |
| CN101768614A (en) * | 2010-03-05 | 2010-07-07 | 浙江省农业科学院 | Method for efficiently extracting polysaccharide and polyphenol from agaricus blazei |
| KR20130027117A (en) * | 2011-09-07 | 2013-03-15 | 한불화장품주식회사 | Cosmetic composition using microcapsules containing fermented herb medicine extracts |
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