CN113797146A - Dendrobium stem extract and preparation method and application thereof - Google Patents
Dendrobium stem extract and preparation method and application thereof Download PDFInfo
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- CN113797146A CN113797146A CN202111311512.6A CN202111311512A CN113797146A CN 113797146 A CN113797146 A CN 113797146A CN 202111311512 A CN202111311512 A CN 202111311512A CN 113797146 A CN113797146 A CN 113797146A
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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
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9794—Liliopsida [monocotyledons]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—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
Abstract
The invention relates to the field of cosmetic application, in particular to a dendrobium nobile lindl extract and a preparation method and application thereof, comprising the following steps: (a) taking the crushed dendrobium nobile lindl raw material, carrying out reflux extraction by using an organic solvent, and carrying out solid-liquid separation to obtain filter residue; (b) extracting the filter residue in the step (a) in water bath, filtering and concentrating under reduced pressure to obtain crude extract; (c) and (c) eluting the crude extract obtained in the step (b) by using a macroporous adsorption resin column, collecting eluent, and concentrating under reduced pressure to obtain the dendrobium nobile extract. The dendrobium nobile extract prepared by the method disclosed by the invention is remarkable in antioxidant activity, has a good moisturizing effect, can be used as an effect additive in the field of cosmetics, and has a wide application prospect.
Description
Technical Field
The invention relates to the field of cosmetic application, and in particular relates to a dendrobium nobile lindl extract and a preparation method and application thereof.
Background
With the continuous development of the cosmetic industry, skin care cosmetics become essential products in life of people at present, and the skin care effect of the skin care cosmetics is generally reflected in the aspects of moisture retention, aging resistance and the like. At present, the theory of free radicals is a research hotspot of an anti-aging mechanism. The effective free radical scavenger has the effects of scavenging excessive free radicals and delaying skin aging. However, the existing products or substances with the ability of scavenging free radicals in the market often have the problems of low activity, single free radical scavenging ability and the like, and if the problems can be solved, the method has great significance for the cosmetic industry.
Dendrobium nobile is a traditional and famous traditional Chinese medicine in China, is an orchid plant, is flat and cylindrical, and is famous like a head ornament. Modern pharmacological studies show that dendrobium nobile lindl has the effects of resisting aging, oxidation and tumors, enhancing the immunity of organisms, reducing blood sugar and the like. In the quality standard of dendrobium nobile recorded in the pharmacopoeia of the people's republic of China 2020 edition, the quality of dendrobium nobile is mainly identified by detecting the content of dendrobine in addition to the appearance and shape and microscopic identification. The dendrobium nobile lindl contains not only alkaloid represented by dendrobine, but also components such as polysaccharides, flavonoids, phenols and the like, has great development and utilization potential, and can be applied to the field of cosmetics. However, the existing extraction methods for various active ingredients in dendrobium nobile lindl mainly comprise a hot water extraction method, a microwave-assisted extraction method, a water extraction and alcohol precipitation polysaccharide, an enzyme-assisted extraction method and the like, and the separation technology for active substances mainly adopts a step-by-step alcohol precipitation method, a silica gel column chromatography method and the like, so that the problems that the content of impurities in the extract is high, or the separation method is not beneficial to scale enlargement and the like exist.
Accordingly, the present invention is directed to a method for manufacturing a semiconductor device.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of dendrobium nobile lindl extract, the dendrobium nobile lindl extract prepared by the method has low impurity content, remarkable antioxidant activity, good moisturizing effect and simple preparation method, and the technical problems that the extraction or separation method of dendrobium nobile lindl in the prior art is not beneficial to enlarging the production scale and the prepared extract has high impurity content are solved.
The second purpose of the invention is to provide the dendrobium nobile lindl extract prepared by the preparation method of the dendrobium nobile lindl extract.
The third objective of the present invention is to provide an application of dendrobium nobile lindl extract in the preparation of cosmetic products, so as to solve the technical problems that products or substances with free radical scavenging ability in the prior art have low activity and only have single free radical scavenging ability.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
in a first aspect, the invention provides a preparation method of dendrobium nobile lindl extract, which comprises the following steps:
(a) carrying out reflux extraction on the crushed dendrobium nobile by using an organic solvent, and carrying out solid-liquid separation after extraction to obtain filter residue;
in some embodiments of the invention, the filter residue is dried after the filter residue is obtained.
And the filter residue is dried and then subjected to water bath extraction, so that the extraction efficiency is improved.
Preferably, in the step (a), each gram of dendrobium nobile lindl is subjected to reflux extraction by using 5-15 mL of solvent;
preferably, the reflux extraction is performed at least 3 times;
preferably, the step of reflux extraction specifically includes: each gram of dendrobium nobile is extracted by refluxing with 10-15mL, 10-15mL and 5-10mL of organic solvents in sequence;
preferably, the organic solvent comprises at least one of ethyl acetate, petroleum ether, and absolute ethanol;
preferably, the organic solvent is ethyl acetate;
preferably, the time of each reflux extraction is 30-60min, and more preferably 40 min.
(b) Carrying out solid-liquid separation after extracting the filter residue obtained in the step (a) in a water bath, and concentrating the liquid obtained by separation to obtain a crude extract;
preferably, in the step (b), the temperature of the water bath extraction is 90-100 ℃;
preferably, in the water bath extraction process, the mass of water is 10-20 times of that of the filter residue;
preferably, the number of times of the water bath extraction is at least 2;
preferably, the water bath extraction step specifically includes: sequentially extracting the filter residue with water with the mass of 15-20 times and 10-15 times of the filter residue in a water bath at 90-100 ℃;
preferably, the water bath extraction is performed at atmospheric pressure;
preferably, in the step (b), the mass concentration of the crude extract is 0.1-1.0 g/mL, more preferably 0.3-0.6 g/mL based on the crude drug amount of dendrobium nobile lindl.
(c) Eluting the crude extract obtained in the step (b) by adopting a macroporous adsorption resin column, collecting eluent, and concentrating to obtain the dendrobium nobile extract;
preferably, in step (c), the macroporous adsorbent resin column is of type D101;
preferably, standing for adsorption for 0.5-4h before elution;
preferably, in step (c), the crude extract is eluted sequentially with water and ethanol;
preferably, the ethanol comprises 15% ethanol solution by volume fraction, 30% ethanol solution by volume fraction and absolute ethanol;
preferably, the step of eluting specifically comprises: eluting each gram of the crude extract by using 10-20g of macroporous adsorption resin and sequentially using 9-20mL of water, 15-30mL of ethanol solution with the volume fraction of 15%, 30-60mL of ethanol solution with the volume fraction of 30% and 15-30mL of absolute ethanol;
preferably, in the step (c), the mass concentration of the dendrobium nobile lindl extract is 0.2-2.0 g/mL, more preferably 0.4-1.0 g/mL based on the crude drug of dendrobium nobile lindl.
In a second aspect, the invention provides a dendrobium nobile lindl extract prepared by a preparation method of the dendrobium nobile lindl extract.
In a third aspect, the invention provides an application of dendrobium nobile lindl extract prepared by the preparation method in preparing cosmetic products.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the dendrobium nobile lindl extract provided by the invention has the advantages of simple and convenient extraction, separation and purification process, easy enlargement of production scale and contribution to development and utilization of dendrobium nobile lindl resources.
(2) The dendrobium nobile lindl extract prepared by the specific preparation method of the dendrobium nobile lindl extract has remarkable antioxidant activity and good moisturizing performance.
(3) The dendrobium nobile lindl extract prepared by the specific preparation method of the dendrobium nobile lindl extract can be used as an efficacy additive to be applied to the field of cosmetics, so that the prepared cosmetics have good skin care effect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a graph showing the results of the antioxidant activity test in the test examples of the present invention.
FIG. 2 is a graph showing the results of testing the moisturizing efficacy of Dendrobium nobile Lindl extract in the test examples of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The invention provides a preparation method of dendrobium nobile lindl extract, which comprises the following steps:
(a) and carrying out reflux extraction on the crushed dendrobium nobile by using an organic solvent, and carrying out solid-liquid separation after extraction to obtain filter residue.
The dendrobium nobile lindl is a traditional and rare traditional Chinese medicine in China, and the modern medical science and the traditional Chinese medicine pharmacological research show that the dendrobium nobile lindl has obvious effects on improving the human body immunity, resisting aging, tonifying the internal organs and consumptive diseases and the like.
In a preferred embodiment of the present invention, in step (a), 5 to 15mL (e.g. 5, 8, 10, 15mL) of solvent is used for reflux extraction per gram of dendrobium nobile lindl;
in a preferred embodiment of the invention, the number of reflux extractions is at least 3, such as 3, 4, 5;
in a preferred embodiment of the present invention, the step of reflux extraction specifically comprises: each gram of dendrobium nobile is extracted by refluxing with 10-15mL, 10-15mL and 5-10mL of organic solvents in sequence;
in a preferred embodiment of the present invention, the organic solvent used comprises at least one of ethyl acetate, petroleum ether, absolute ethanol;
in a preferred embodiment of the invention, the organic solvent used is ethyl acetate;
in a preferred embodiment of the invention, the time of each reflux extraction is 30-60 min; can also be selected from 35min, 40min, 45min, 50min or 55 min;
in a preferred embodiment of the invention, the time for each reflux extraction is 40 min.
The ethyl acetate is colorless transparent liquid, has low toxicity and sweet taste, has pungent odor when the concentration is higher, is easy to volatilize, has air-sensitive feeling, and can absorb moisture to slowly hydrolyze the ethyl acetate to form acidic reaction. Can be mixed with chloroform, ethanol, acetone and diethyl ether, and dissolved in water. Ethyl acetate is used in a wide variety of applications, such as: can be used as an extractant for the production of medicines, organic acids and other products; can be used as extractant to extract many compounds (phosphorus, tungsten, arsenic, cobalt) from aqueous solution; can be used as organic solvent, and as standard substance for calibrating thermometer when used for separating saccharides.
Petroleum ether is a colorless transparent liquid, mainly a mixture of pentane and hexane. Is insoluble in water, and is soluble in most organic solvents such as absolute ethanol, benzene, chloroform, oils, etc. Mainly used for solvent and grease treatment, specifically: can be used as organic solvent and chromatographic solvent; can be used as an organic high-efficiency solvent, a medicine extracting agent, a fine chemical synthesis auxiliary agent and the like; can also be used for organic synthesis and chemical raw materials.
The absolute ethanol refers to ethanol water solution with higher purity. In general, an ethanol solution with a concentration of 99.5% is referred to as absolute ethanol, and absolute ethanol is a mixture of ethanol and water, can be miscible with water at any ratio, and can be miscible with many organic solvents such as ether, chloroform, glycerol, and the like. The absolute ethyl alcohol can be widely used in various aspects such as medicine, paint, sanitary products, cosmetics, grease and the like.
(b) Carrying out solid-liquid separation after extracting the filter residue obtained in the step (a) in a water bath, and concentrating the liquid obtained by separation to obtain a crude extract;
in a preferred embodiment of the invention, the temperature of the water bath extraction is 90-100 ℃; optionally 92 deg.C, 94 deg.C, 96 deg.C or 98 deg.C;
in the preferred embodiment of the invention, in the water bath extraction process, the mass of water is 10-20 times of the mass of filter residue; it is also possible to choose 12 times, 15 times or 18 times.
In a preferred embodiment of the invention, the number of water bath extractions is at least 2, such as 2, 3, 4;
in a preferred embodiment of the present invention, the water bath extraction step specifically comprises: sequentially extracting the filter residue with water with the mass of 15-20 times and 10-15 times of the filter residue in a water bath at 90-100 ℃; wherein the temperature can also be 92 ℃, 94 ℃, 96 ℃ or 98 ℃;
in a preferred embodiment of the invention, the water bath extraction is carried out at atmospheric pressure;
in a preferred embodiment of the invention, the mass concentration of the crude extract is 0.1-1.0 g/mL, and can be selected from 0.2g/mL, 0.4g/mL, 0.6g/mL or 0.8g/mL based on the crude drug of dendrobium nobile lindl; more preferably 0.3-0.6 g/mL, i.e. the initial mass of dendrobium per mL of solution is 0.3-0.6 g.
In the prior art, the extraction methods of various active ingredients in dendrobium nobile lindl mainly comprise a hot water extraction method, an ultrasonic auxiliary extraction method, a microwave auxiliary extraction method, a water extraction and alcohol precipitation polysaccharide, an enzyme auxiliary extraction method and the like, and the separation technology of active substances mainly adopts a step alcohol precipitation method, a macroporous adsorption resin column chromatography method, a silica gel column chromatography method and the like, so that the problems of high impurity content of extract, unfavorable scale expansion of the separation method and the like exist. According to the invention, the organic solvent is extracted in advance by the method of preparing the polysaccharide by firstly treating the polysaccharide with the organic solvent and then extracting the polysaccharide with water, so that the water-soluble polysaccharide component is dissolved out favorably, and the difficulty in later separation is reduced. Moreover, the organic solvent part can be studied for efficacy in other directions, and the utilization rate of rare plants is improved.
(c) Eluting the crude extract obtained in the step (b) by adopting a macroporous adsorption resin column, collecting eluent, and concentrating to obtain the dendrobium nobile extract.
The macroporous adsorption resin is a macromolecular adsorption resin which does not contain exchange groups and has a macroporous structure, has a good macroporous network structure and a larger specific surface area, and can selectively adsorb organic matters in an aqueous solution through physics. The D101 type macroporous adsorption resin is an adsorbent of a nonpolar polymer, is used for adsorbing and retaining polysaccharide substances with relatively small polarity and phenolic hydroxyl structures, and simultaneously optimizes elution conditions by virtue of the porous structure of the polysaccharide substances to separate the polysaccharide components with different molecular weights and phenolic hydroxyl structures with different quantities so as to obtain the components with good antioxidant activity and moisturizing activity.
In a preferred embodiment of the present invention, the macroporous adsorbent resin column is of type D101;
in a preferred embodiment of the invention, the adsorption is carried out for 0.5 to 4 hours by standing before elution; 1h, 2h or 3h can also be selected.
In a preferred embodiment of the present invention, the crude extract is eluted with water and ethanol in this order;
in a preferred embodiment of the present invention, the ethanol comprises a 15% volume fraction ethanol solution, a 30% volume fraction ethanol solution and anhydrous ethanol; eluting each gram of the crude extract by using 10-20g of macroporous adsorption resin and sequentially using 9-20mL of water, 15-30mL of ethanol solution with the volume fraction of 15%, 30-60mL of ethanol solution with the volume fraction of 30% and 15-30mL of absolute ethanol;
in a preferred embodiment of the invention, the mass concentration of the dendrobium nobile lindl extract is 0.2-2.0 g/mL based on the crude dendrobium nobile lindl amount, namely the mass of the dendrobium nobile lindl corresponding to each mL of solution is 0.2-2.0 g; more preferably 0.4 to 1.0 g/mL.
The dendrobium nobile active site prepared by the preparation method disclosed by the invention is remarkable in antioxidant activity, has a good moisturizing effect, and can be used as an effect type additive in the field of cosmetics. In addition, the preparation process is easy to enlarge scale, and is beneficial to the development and utilization of dendrobium nobile resources.
Example 1
The embodiment provides a preparation method of dendrobium nobile lindl extract, which comprises the following steps:
performing reflux extraction on the crushed dendrobium nobile for 3 times by using 10mL, 10mL and 5mL of ethyl acetate in turn according to per gram of dendrobium nobile, extracting for 40min each time, performing solid-liquid separation after extraction to obtain filter residue, sequentially extracting the filter residue for 2 times by using deionized water with the mass 15 times and 10 times of the obtained filter residue in a water bath at 90 ℃ under normal pressure, performing solid-liquid separation after extraction, concentrating the separated liquid to obtain a water extract of the dendrobium nobile, preparing the water extract into a crude extraction liquid with the concentration of 0.5g/mL according to the mass of the dendrobium nobile, loading the crude extraction liquid on a pretreated D101 type macroporous resin column, standing and adsorbing for 2h after loading, and sequentially eluting by using 11mL of water, 18mL of an ethanol solution with the volume fraction of 15%, 35mL of an ethanol solution with the volume fraction of 30% and 18mL of absolute ethanol according to per gram of the crude extraction liquid, and monitoring and collecting the eluent by adopting full wavelength, concentrating the eluent, and preparing a solution with the concentration of 0.4g/mL in terms of the crude drug amount of the dendrobium nobile lindl by using deionized water to obtain the dendrobium nobile lindl extract.
Example 2
The preparation method of the dendrobium nobile lindl extract provided in this example is basically the same as that of example 1, except that ethyl acetate is replaced by petroleum ether.
Example 3
The preparation method of the dendrobium nobile lindl extract provided in this example is basically the same as that of example 1, except that ethyl acetate is replaced by absolute ethyl alcohol.
Example 4
The preparation method of the dendrobium nobile lindl extract provided by the embodiment comprises the following steps:
performing reflux extraction on the crushed dendrobium nobile lindl for four times by using ethyl acetate of 15mL, 12mL, 8mL and 5mL in turn according to each gram of dendrobium nobile lindl, extracting for 50min each time, performing solid-liquid separation after extraction to obtain filter residue, extracting the filter residue for 3 times by using deionized water of which the mass is 20 times, 15 times and 10 times of the mass of the obtained filter residue in water bath at 100 ℃ in turn under normal pressure, performing solid-liquid separation after extraction, concentrating the separated liquid to obtain a water extract of the dendrobium nobile lindl, preparing the water extract into a crude extract with the concentration of 0.3g/mL according to the crude drug of the dendrobium nobile lindl, putting the crude extract on a pretreated D101 type macroporous resin column, standing for adsorption for 2.5h, and eluting by using water of 20mL, ethanol solution of which the volume fraction is 15% of 30mL, ethanol solution of which the volume fraction is 60mL and absolute ethanol of 30mL of each gram of the crude extract in turn, and monitoring and collecting the eluent by adopting full wavelength, concentrating the eluent, and preparing a solution with the concentration of 0.6g/mL in terms of the crude drug amount of the dendrobium nobile lindl by using deionized water to obtain the dendrobium nobile lindl extract.
Example 5
The preparation method of the dendrobium nobile lindl extract provided by the embodiment comprises the following steps:
performing reflux extraction on the crushed dendrobium nobile lindl for four times by using ethyl acetate of 15mL, 10mL, 8mL and 5mL in turn according to each gram of dendrobium nobile lindl, extracting for 45min each time, performing solid-liquid separation after extraction to obtain filter residue, extracting the filter residue for 3 times by using deionized water of which the concentration is 20 times, 15 times and 10 times of the obtained filter residue in water bath at the temperature of 95 ℃ in turn under normal pressure, performing solid-liquid separation after extraction, concentrating the separated liquid to obtain a water extract of the dendrobium nobile lindl, preparing the water extract into a crude extraction liquid with the concentration of 0.6g/mL according to the crude drug amount of the dendrobium nobile lindl, loading the crude extraction liquid on a pretreated D101 type macroporous resin column, standing and adsorbing for 3h after loading, and eluting by using water of 9mL, an ethanol solution of which the volume fraction is 15% according to each gram of the crude extraction liquid, an ethanol solution of which the volume fraction is 30% and absolute ethanol of 15mL in turn, and monitoring and collecting the eluent by adopting full wavelength, concentrating the eluent, and preparing a solution with the concentration of 0.8g/mL in terms of the crude drug amount of the dendrobium nobile lindl by using deionized water to obtain the dendrobium nobile lindl extract.
Comparative example 1
The preparation method of the dendrobium nobile lindl extract provided by the comparative example comprises the following steps:
extracting crushed dendrobium nobile lindl with deionized water 15 times, 10 times and 10 times of the mass of filter residue for 5 times in a water bath at 90 ℃ under normal pressure, carrying out solid-liquid separation after extraction, concentrating the separated liquid to obtain a dendrobium nobile lindl water extract, preparing the water extract into a crude extraction liquid with the concentration of 0.5g/mL based on the dendrobium nobile lindl crude drug amount by using the deionized water, loading the crude extraction liquid on a pretreated D101 type macroporous resin column, standing and adsorbing for 2h after loading, sequentially adopting 11mL of water, 18mL of ethanol solution with the volume fraction of 15%, 35mL of ethanol solution with the volume fraction of 30% and 18mL of absolute ethanol for elution based on each gram of the crude extraction liquid, collecting eluent by adopting full-wavelength monitoring, preparing a solution with the concentration of 0.4g/mL based on the dendrobium nobile lindl crude drug amount by using the deionized water after concentration, obtaining the dendrobium nobile lindl extract.
Comparative example 2
Performing reflux extraction on the crushed dendrobium nobile for 5 times by using 10mL, 5mL and 5mL of ethyl acetate in turn according to per gram of dendrobium nobile, extracting for 40min each time, performing solid-liquid separation after extraction, concentrating the separated liquid, adding deionized water to prepare a crude extract with the concentration of 0.5g/mL according to the original dendrobium nobile content, loading the crude extract on a pretreated D101 type macroporous resin column, standing and adsorbing for 2h after sampling, based on per gram of crude extract, sequentially adopting 11mL of water, 18mL of ethanol solution with the volume fraction of 15%, 35mL of ethanol solution with the volume fraction of 30% and 18mL of absolute ethyl alcohol for elution, and monitoring and collecting the eluent by adopting full wavelength, concentrating the eluent, and preparing a solution with the concentration of 0.4g/mL in terms of the crude drug amount of the dendrobium nobile lindl by using deionized water to obtain the dendrobium nobile lindl extract.
Test example 1
The extraction efficiency of the antioxidant active substances in the dendrobium nobile is compared by adopting a DPPH method and taking the antioxidant activity as an index in each example and comparative example. The results are shown in Table 1.
TABLE 1 comparison of extraction efficiencies for each group
Test example 2
Performing antioxidant activity detection on the dendrobium nobile extract prepared in the embodiment 1, specifically, performing antioxidant activity detection on each group of dendrobium nobile extract by taking a 100 mu M Trolox solution as a positive control and adopting a DPPH method; detecting the free radical scavenging capacity of the dendrobium nobile extracts by using 100 mu M Trolox solution as a reference and using an ABTS method; the free radical scavenging ability of the dendrobium nobile extracts in each group was determined by ORAC method with 10 μ M Trolox as control, and the results are shown in FIG. 1.
As can be seen from fig. 1, the dendrobium nobile lindl extract has very significant antioxidant activity.
And the semi-clearance concentration (IC50) of the extract of dendrobium nobile lindl prepared in example 1 was measured for its antioxidant activity by DPPH method and ABTS method, and the results are shown in table 2.
TABLE 2 anti-oxidant activity results of Dendrobium nobile extract
As can be seen from the data in table 2, the dendrobium nobile lindl extract has very significant antioxidant activity.
Test example 3
Respectively weighing a proper amount of glycerin, butanediol and sodium alginate, dissolving by using deionized water, and preparing into a solution with the mass fraction of 2% for later use. Taking the dendrobium nobile lindl extract solution prepared in the embodiment 1, and preparing the solution with the mass fraction of 2% by using deionized water for later use. The deionized water was used as a control, and the moisturizing abilities of the glycerin, the butanediol, the sodium alginate and the dendrobium stem extract solution under the condition of the relative humidity of 43% were measured by a weighing method, and the results are shown in fig. 2.
As can be seen from FIG. 2, the dendrobium nobile lindl extract has good moisturizing ability.
Test example 4
The total polysaccharide content in the dendrobium nobile extract prepared in each example and comparative example of the present invention was determined according to the method for detecting the total polysaccharide content under dendrobium huoshanense item in the dendrobium nobile standard recorded in the 'chinese pharmacopoeia' 2020 edition, and the results are shown in table 3.
TABLE 3 Total polysaccharide content in the Dendrobium nobile extract
| Numbering | Total polysaccharidesContent (%) |
| Example 1 | 41.6％ |
| Example 2 | 38.2％ |
| Example 3 | 57.5％ |
| Example 4 | 28.7％ |
| Example 5 | 26.5％ |
| Comparative example 1 | 18.7％ |
| Comparative example 2 | 10.5％ |
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of dendrobium nobile lindl extract is characterized by comprising the following steps:
(a) carrying out reflux extraction on the crushed dendrobium nobile by using an organic solvent, and carrying out solid-liquid separation after extraction to obtain filter residue;
(b) carrying out solid-liquid separation after extracting the filter residue obtained in the step (a) in a water bath, and concentrating the liquid obtained by separation to obtain a crude extract;
(c) eluting the crude extract obtained in the step (b) by adopting a macroporous adsorption resin column, collecting eluent, and concentrating to obtain the dendrobium nobile extract.
2. The method for preparing dendrobium nobile lindl extract according to claim 1, characterized in that in step (a), each gram of dendrobium nobile lindl is extracted by refluxing with 5-15 mL of solvent;
preferably, the reflux extraction is performed at least 3 times;
preferably, the step of reflux extraction specifically includes: each gram of dendrobium nobile is extracted by refluxing with 10-15mL, 10-15mL and 5-10mL of organic solvents in sequence;
preferably, the organic solvent comprises at least one of ethyl acetate, petroleum ether, and absolute ethanol;
preferably, the organic solvent is ethyl acetate.
3. The method for preparing dendrobium nobile lindl extract according to claim 2, characterized in that in step (a), the time of each reflux extraction is 30-60 min; preferably 40 min.
4. The method for preparing dendrobium nobile lindl extract according to claim 1, wherein in the step (b), the temperature of the water bath extraction is 90-100 ℃;
preferably, in the water bath extraction process, the mass of water is 10-20 times of that of the filter residue;
preferably, the number of times of the water bath extraction is at least 2;
preferably, the water bath extraction step specifically includes: sequentially extracting the filter residue with water with the mass of 15-20 times and 10-15 times of the filter residue in a water bath at 90-100 ℃;
preferably, the water bath extraction is performed at atmospheric pressure.
5. The method for preparing a dendrobium nobile lindl extract according to claim 1, wherein in step (b), the mass concentration of the crude extract is 0.1-1.0 g/mL based on the crude dendrobium nobile lindl.
6. The method for preparing dendrobium nobile lindl extract according to claim 1 wherein in step (c), the macroporous adsorbent resin column is D101 type;
preferably, the adsorption is carried out for 0.5 to 4 hours at rest before the elution.
7. The method for preparing dendrobium nobile lindl extract according to claim 1, characterized in that in step (c), water and ethanol are adopted to elute the crude extract in sequence;
preferably, the ethanol comprises 15% ethanol solution by volume fraction, 30% ethanol solution by volume fraction and absolute ethanol;
preferably, the step of eluting specifically comprises: and each gram of the crude extract is eluted by sequentially adopting 9-20mL of water, 15-30mL of ethanol solution with the volume fraction of 15%, 30-60mL of ethanol solution with the volume fraction of 30% and 15-30mL of absolute ethanol.
8. The method according to claim 1, wherein in step (c), the concentration of the dendrobium nobile lindl extract is 0.2-2.0 g/mL in terms of the crude drug content of dendrobium nobile lindl.
9. The dendrobium nobile lindl extract prepared by the method for preparing the dendrobium nobile lindl extract according to any one of claims 1 to 8.
10. The dendrobium nobile lindl extract prepared by the method for preparing the dendrobium nobile lindl extract according to any one of claims 1 to 8, or the application of the dendrobium nobile lindl extract according to claim 9 in preparing cosmetic products.
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