CN113398030A - Osmanthus fragrans flower extract, preparation method thereof and cosmetic - Google Patents
Osmanthus fragrans flower extract, preparation method thereof and cosmetic Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/60—Sugars; Derivatives thereof
- A61K8/602—Glycosides, e.g. rutin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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- 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
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- 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
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- 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
- A61K2800/84—Products or compounds obtained by lyophilisation, freeze-drying
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- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
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Abstract
The invention provides an osmanthus fragrans extract, a preparation method thereof and cosmetics, and relates to the technical field of natural plant extraction. Mixing pretreated sweet osmanthus with a solvent, carrying out negative pressure extraction, then carrying out solid-liquid separation, concentrating supernatant obtained by the solid-liquid separation, adsorbing by using adsorption resin, eluting, concentrating obtained eluent, and then carrying out freeze drying to obtain a sweet osmanthus extract; the negative pressure extraction is adopted to reduce the boiling point of a mixed material formed by the sweet osmanthus and the solvent, so that the effective components with the thermosensitive property in the sweet osmanthus can be quickly and effectively extracted at a lower temperature, and the activity of the effective components can not be damaged; the obtained eluent is concentrated and then freeze-dried, so that the concentration of the active substances can be kept to the maximum extent. The osmanthus extract prepared by the preparation method contains active ingredients such as verbascoside and salidroside, and has high content of the active ingredients, light color and good stability.
Description
Technical Field
The invention relates to the technical field of natural plant extraction, and particularly relates to an osmanthus fragrans extract, a preparation method thereof and cosmetics.
Background
The osmanthus fragrans is one of ten traditional famous flowers in China, and is planted in Guizhou and other areas in a large scale. Researches show that the osmanthus fragrans is rich in various effective components such as verbascoside, salidroside and the like, and the osmanthus fragrans or the osmanthus fragrans extract can be used as a raw material of various products such as food, health care products and the like due to wide sources and proper cost of the osmanthus fragrans.
The sweet osmanthus extract is a substance extracted or processed by taking sweet osmanthus as a raw material. The different extraction modes lead the effective components or contents contained in the osmanthus fragrans extracts to be different. In the existing research on the extraction process (such as high-temperature extraction) of sweet osmanthus, only the yield of the extract is usually concerned, the obtained product has a darker color, and the application of the extract to subsequent products is easy to cause the unattractive color of the product. For example, patent CN103768152A discloses an extraction method of osmanthus fragrans phenylethanoid glycosides, which is to extract at high temperature under normal pressure to obtain osmanthus fragrans extract in which phenylethanoid total glycosides are verbascoside and isoverbascoside. However, the stability of active ingredients (acteoside, salidroside, etc.) in osmanthus fragrans is poor, and long-term heating may cause quality deterioration, such as inactivation of active substances, deepening of color, generation of unpleasant odor, and reduction of efficacy. In addition, the application of the osmanthus fragrans extract only focuses on the content of a single functional component in the osmanthus fragrans extract, and does not focus on other functional components, thereby causing resource waste.
In view of the above, the present invention is particularly proposed to solve at least one of the above technical problems.
Disclosure of Invention
The first objective of the present invention is to provide a preparation method of an osmanthus fragrans extract, so as to alleviate the above technical problems in the prior art.
The second purpose of the invention is to provide an osmanthus fragrans extract, which is prepared by adopting the preparation method.
The third purpose of the invention is to provide a cosmetic, which comprises the osmanthus fragrans extract.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a preparation method of an osmanthus extract, which comprises the following steps:
(a) mixing the pretreated sweet osmanthus with a solvent for negative pressure extraction to obtain an extracting solution; carrying out solid-liquid separation on the extracting solution to obtain supernatant;
(b) concentrating the supernatant, adsorbing by using adsorption resin, and then eluting to obtain an eluent;
concentrating the eluate, and freeze drying to obtain flos Osmanthi Fragrantis extract containing acteoside and salidroside.
Further, on the basis of the above technical solution of the present invention, in the step (a), the solvent includes water or an aqueous ethanol solution;
preferably, 10-20mL of solvent is used per gram of osmanthus fragrans.
Further, on the basis of the above technical scheme of the present invention, in the step (a), the pressure of the negative pressure extraction is-0.02 to-0.1 MPa;
preferably, the temperature of the negative pressure extraction is 30-60 ℃;
preferably, the times of negative pressure extraction are 1-3 times;
preferably, the time of each negative pressure extraction is 30-90 min.
Further, on the basis of the above technical scheme of the invention, in the step (a), the pressure of the negative pressure extraction is-0.04 to-0.06 MPa;
preferably, the temperature of the negative pressure extraction is 40-50 ℃;
preferably, the times of negative pressure extraction are 2-3 times;
preferably, the time of each negative pressure extraction is 60-90 min.
Further, on the basis of the above technical scheme of the present invention, in the step (a), the pretreatment comprises the steps of drying and then crushing the osmanthus flowers;
preferably, the solid-liquid separation mode comprises centrifugation;
preferably, the rotation speed of the centrifugation is 3000-.
Further, on the basis of the above technical solution of the present invention, in the step (b), the adsorption resin includes D101 macroporous adsorption resin or X-5 macroporous adsorption resin;
preferably, the eluent used for elution comprises water and ethanol water solution;
preferably, the volume fraction of the ethanol aqueous solution used for elution is 10-50%.
Further, in the step (b), the concentration is a concentration under reduced pressure, based on the above technical means of the present invention.
Further, on the basis of the technical scheme of the invention, in the step (b), the temperature of the freeze drying is-40 to-50 ℃;
preferably, the vacuum degree of the freeze drying is 20-60 Pa;
preferably, the freeze-drying time is 24 to 36 hours.
The invention also provides an osmanthus extract, which is prepared by adopting the preparation method of the osmanthus extract;
the sweet osmanthus extract contains verbascoside and salidroside;
preferably, the mass fraction of verbascoside in the sweet osmanthus flower extract is 30-50%, and the mass fraction of salidroside is 2-8%.
The invention also provides a cosmetic containing the osmanthus fragrans extract.
Compared with the prior art, the invention has the beneficial effects that:
(1) mixing the pretreated osmanthus with a solvent, carrying out negative pressure extraction, then carrying out solid-liquid separation, concentrating the supernatant obtained by the solid-liquid separation, then adopting adsorption resin to carry out adsorption and elution, concentrating the obtained eluent, and then carrying out freeze drying to obtain the osmanthus extract containing verbascoside and salidroside; the pretreated sweet osmanthus is subjected to negative pressure extraction with a solvent, so that the boiling point of a mixed material formed by the sweet osmanthus and the solvent is reduced, effective components with thermosensitive properties in the sweet osmanthus are quickly and effectively extracted at a lower temperature, and the activity of the effective components is not damaged; furthermore, the obtained eluent is concentrated and then freeze-dried, so that the concentration of verbascoside and salidroside can be kept to the maximum extent. In addition, the preparation method has simple process, low cost of the adopted raw materials, safety and no pollution to the environment, and is suitable for industrial mass production.
The osmanthus fragrans extract prepared by the preparation method of the osmanthus fragrans extract simultaneously contains active ingredients such as verbascoside and salidroside, has high content of the active ingredients, has light color and good stability, and provides a certain guarantee for the subsequent application of the osmanthus fragrans extract.
(2) The invention provides an osmanthus extract, which is prepared by adopting the preparation method of the osmanthus extract, the osmanthus extract has high content of active ingredients such as verbascoside, salidroside and the like, and the osmanthus extract has light color and good stability and is suitable for being applied to cosmetics.
(3) The invention provides a cosmetic, which comprises the osmanthus fragrans extract. In view of light color and good stability of the osmanthus fragrans extract, the osmanthus fragrans extract can play a very good and lasting skin brightening role when being applied to cosmetics, and the verbascoside and the salidroside in the osmanthus fragrans extract play a role together, so that the cosmetics have excellent effects of whitening, delaying aging, resisting oxidation and resisting ultraviolet rays.
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 process flow chart of a preparation method of an osmanthus fragrans extract according to an embodiment of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the 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 osmanthus fragrans extract prepared by the existing preparation method is dark in color, and when the osmanthus fragrans extract is used in subsequent products, the product color is not attractive, the content of active ingredients in the osmanthus fragrans extract is low, and the requirement of the product can be met only by adding more osmanthus fragrans extracts.
In order to solve the technical problems, the inventor discovers through a great deal of creative work that the osmanthus fragrans extract prepared by the existing method is deep in color and low in effective component content mainly because the high-temperature extraction method is adopted, the effective components with heat-sensitive properties in the osmanthus fragrans are easily damaged by the high-temperature extraction, and the extract obtained by the high-temperature extraction is deep in color, so that the obtained osmanthus fragrans extract is low in effective component content and deep in color. The present invention is proposed to solve this problem.
According to a first aspect of the present invention, there is provided a preparation method of an osmanthus extract, comprising the following steps:
(a) mixing the pretreated sweet osmanthus with a solvent for negative pressure extraction to obtain an extracting solution;
carrying out solid-liquid separation on the extracting solution to obtain supernatant;
(b) concentrating the supernatant, adsorbing by using adsorption resin, and then eluting to obtain an eluent;
concentrating the eluate, and freeze drying to obtain flos Osmanthi Fragrantis extract containing acteoside and salidroside.
Specifically, the step (a) of the present invention is to prepare the fresh osmanthus into a form suitable for extraction, and the typical but non-limiting step of the pretreatment may be drying and/or crushing, for example.
The negative pressure extraction is that vacuum decompression is adopted during extraction, so that the boiling point of a mixed material formed by the sweet osmanthus and a solvent is reduced, and the effective components with the thermosensitive property in the sweet osmanthus are quickly and effectively extracted at a lower temperature. Compared with the traditional extraction method (such as solvent high-temperature extraction), the negative pressure extraction can ensure that the effective components have higher extraction rate, and has the remarkable characteristics of short extraction time, low extraction temperature and easy operation. And the negative pressure extraction can be realized only by introducing a vacuum system on a conventional extractor, thereby avoiding the adoption of microwave extraction, ultrasonic extraction and supercritical CO2The new extraction methods such as extraction have the defects of expensive extraction equipment, small treatment capacity and the like.
Meanwhile, the extraction solution obtained by adopting negative pressure extraction has light color, so that the prepared osmanthus fragrans extract has light color, high content of effective components and good stability.
The negative pressure extraction is determined according to the specific condition of the mixed material formed by the sweet osmanthus and the solvent, wherein the adopted temperature, time, pressure and extraction times are required.
The number of times of negative pressure extraction is not limited to 1, and may be 2 or more. The times of negative pressure extraction are to ensure that the effective components in the osmanthus are fully extracted. And if multiple times of negative pressure extraction are carried out, combining the extracting solutions I obtained by each negative pressure extraction to obtain the extracting solution.
The pulverized osmanthus fragrans is a fine powder, insoluble in a solvent, and present in the form of a precipitate, and after extraction is completed, the osmanthus fragrans is separated from an extract liquid, so that the osmanthus fragrans is removed by solid-liquid separation (for example, filtration or centrifugation).
In the step (b), the supernatant is concentrated and then is absorbed by the absorption resin because the solvent content in the supernatant is high. The type of the adsorption resin is not particularly limited, and may be selected according to the effective components and content in the osmanthus fragrans.
After adsorption, elution treatment is carried out by eluent, and then freeze drying is carried out. Unlike conventional spray drying, low pressure drying and ultrasonic drying, vacuum freeze drying maximizes the concentration of the active.
Mixing the pretreated osmanthus with a solvent, carrying out negative pressure extraction, then carrying out solid-liquid separation, concentrating the supernatant obtained by the solid-liquid separation, then adopting adsorption resin to carry out adsorption and elution, concentrating the obtained eluent, and then carrying out freeze drying to obtain the osmanthus extract containing verbascoside and salidroside; the pretreated sweet osmanthus is subjected to negative pressure extraction with a solvent, so that the boiling point of a mixed material formed by the sweet osmanthus and the solvent is reduced, effective components with thermosensitive properties in the sweet osmanthus are quickly and effectively extracted at a lower temperature, and the activity of the effective components is not damaged; furthermore, the resulting eluate is concentrated and then freeze-dried, so that the concentration of the active substance can be retained to the maximum extent. In addition, the preparation method has simple process, low cost of the adopted raw materials, safety and no pollution to the environment, and is suitable for industrial mass production.
The osmanthus fragrans extract prepared by the preparation method of the osmanthus fragrans extract simultaneously contains active ingredients such as verbascoside and salidroside, has high content of the active ingredients, has light color and good stability, and provides a certain guarantee for the subsequent application of the osmanthus fragrans extract.
As an alternative embodiment of the present invention, in the step (a), the pretreatment includes a step of drying and then pulverizing the sweet osmanthus flower.
The pretreatment step is further limited, so that the extraction process is more favorable for the dissolution of effective components (acteoside and salidroside).
As an alternative embodiment of the present invention, in step (a), the solvent comprises water or an aqueous ethanol solution.
The water or ethanol water solution has good dissolving capacity for the effective components in the sweet osmanthus. By limiting the types of the solvents, the effective components in the osmanthus can be fully extracted. And the solvent is safe and environment-friendly and has no pollution to the environment.
As an optional embodiment of the present invention, in step (a), the ratio of the sweet osmanthus flower to the solvent is 1: (10-20), namely 10-20mL of solvent is used per gram of osmanthus fragrans. The typical but non-limiting feed-to-liquid ratio of osmanthus fragrans to solvent is 1: 10. 1: 12. 1: 14. 1: 15. 1: 16. 1: 18. 1: 20.
technological parameters such as pressure, temperature, times, extraction time and the like in the negative pressure extraction process have important influence on the extraction of effective components in the osmanthus fragrans.
As an alternative embodiment of the invention, the pressure of the negative pressure extraction in step (a) is between-0.02 and-0.1 MPa, preferably between-0.04 and-0.06 MPa.
Typical but non-limiting negative pressure extraction pressures are-0.02 MPa, -0.04MPa, -0.05MPa, -0.06MPa, -0.08MPa, -0.09MPa or-0.1 MPa. The pressure of the negative pressure extraction cannot be too high (higher than-0.02 MPa), so that a better extraction effect cannot be obtained, and the pressure of the negative pressure extraction cannot be too low (lower than-0.1 MPa), so that the technical realization is difficult, the equipment requirement is high, the cost is high, and the pressure of the negative pressure extraction needs to be limited within a specific numerical value range.
As an alternative embodiment of the present invention, the temperature of the negative pressure extraction in step (a) is 30-60 deg.C, preferably 40-50 deg.C.
Typical but non-limiting negative pressure extraction temperatures are 30 deg.C, 32 deg.C, 34 deg.C, 35 deg.C, 36 deg.C, 38 deg.C, 40 deg.C, 42 deg.C, 44 deg.C, 45 deg.C, 46 deg.C, 48 deg.C, 50 deg.C, 52 deg.C, 54 deg.C, 55 deg.C, 56 deg.C, 58 deg.C or 60 deg.C. The temperature of negative pressure extraction cannot be too high (higher than 60 ℃), which easily causes the color of the extracting solution to become dark, verbascoside and salidroside are inactivated, the temperature of negative pressure extraction cannot be too low (lower than 30 ℃), the extraction efficiency is low, and the temperature of negative pressure extraction needs to be limited in a specific numerical range.
As an alternative embodiment of the present invention, in the step (a), the number of times of negative pressure extraction is 1 to 3. Typical but non-limiting times of negative pressure extraction are 1, 2 and 3.
As an alternative embodiment of the present invention, in step (a), the time of each negative pressure extraction is 30-90 min.
Typical but non-limiting times for negative pressure extraction are 30min, 40min, 50min, 60min, 70min, 80min or 90 min. The time for the negative pressure extraction cannot be too short (less than 30min), which tends to result in insufficient extraction, and the time for the negative pressure extraction cannot be too long (more than 90min), which tends to result in loss of the active ingredient, so that the temperature for the negative pressure extraction needs to be limited to a specific value range.
As a preferred embodiment of the invention, in the step (a), the pressure of the negative pressure extraction is-0.04 to-0.06 MPa, the temperature of the negative pressure extraction is 40 to 50 ℃, the times of the negative pressure extraction are 2 to 3 times, and the time of each negative pressure extraction is 60 to 90 min.
By further limiting the process parameters of the negative pressure extraction, the extraction rate of the effective components in the osmanthus fragrans can be further improved.
As an alternative embodiment of the present invention, in step (a), the solid-liquid separation means comprises centrifugation.
As an alternative embodiment of the present invention, in step (a), the rotation speed of the centrifugation is 1000-. Typical but non-limiting centrifuges have a rotational speed of 1000r/min, 2000r/min, 3000r/min, 4000r/min, 5000r/min, 6000r/min, 7000r/min or 8000 r/min.
As an alternative embodiment of the present invention, in the step (b), the adsorption resin comprises a D101 macroporous adsorption resin or an X-5 macroporous adsorption resin.
The specific type of the adsorption resin is limited, so that the adsorption resin has good adsorption capacity for effective components in the supernatant after concentration.
In an alternative embodiment of the present invention, in the step (b), the eluent used for elution includes water and an aqueous ethanol solution. Here, the elution is performed with water and then with an aqueous ethanol solution.
As an alternative embodiment of the invention, the volume fraction of the aqueous ethanol solution used for elution is 10-50%. The aqueous ethanol solution typically, but not by way of limitation, is 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, or 50% by volume.
In an alternative embodiment of the present invention, in the step (b), the concentration is a concentration under reduced pressure.
As an alternative embodiment of the present invention, the temperature of the freeze-drying in step (b) is-40 to-50 ℃. Typical but non-limiting temperatures for freeze-drying are-40 ℃, -42 ℃, -44 ℃, -45 ℃, -46 ℃, -48 ℃ or-50 ℃.
As an optional embodiment of the invention, the vacuum degree of freeze drying is 20-60 Pa; typical but non-limiting pressures for freeze-drying are 20Pa, 30Pa, 40Pa, 50Pa or 60 Pa.
As an optional embodiment of the invention, the freeze drying time is 24-36 h. Typical but non-limiting times for freeze-drying are 24h, 25h, 26h, 28h, 30h, 32h, 34h or 36 h.
According to the second aspect of the invention, the invention also provides the osmanthus fragrans extract which is prepared by adopting the preparation method of the osmanthus fragrans extract;
the flos Osmanthi Fragrantis extract contains acteoside and salidroside.
The osmanthus fragrans extract prepared by the preparation method has high content of active ingredients such as verbascoside, salidroside and the like, and has light color and good stability.
As an optional implementation mode of the invention, the mass fraction of the verbascoside in the sweet osmanthus extract is 30-50%, and the mass fraction of the salidroside is 2-8%.
According to a third aspect of the invention, a cosmetic is also provided, which comprises the osmanthus fragrans extract.
In view of light color and good stability of the osmanthus fragrans extract, the osmanthus fragrans extract can play a very good and lasting skin brightening role when being applied to cosmetics, and the verbascoside and the salidroside in the osmanthus fragrans extract play a role together, so that the cosmetics have excellent effects of whitening, delaying aging, resisting oxidation and resisting ultraviolet rays.
The raw materials of the cosmetic can comprise other raw materials and/or auxiliary agents acceptable in the cosmetic field besides the sweet osmanthus extract, such as but not limited to moisturizer, thickener, chelating agent, emollient, neutralizer, preservative or skin conditioner and the like.
The form of the cosmetic preparation is not particularly limited, and includes, but is not limited to, cream, lotion, solution, film or spray form. The cosmetic can be in the form of skin cream, sunscreen cream, foundation, essence, cosmetic water, facial mask, spray, face cleaning milk, eye cream, etc.
The present invention will be further described with reference to specific examples and comparative examples.
Example 1
The embodiment provides a preparation method of an osmanthus fragrans extract, a process flow diagram is shown in fig. 1, and the preparation method comprises the following steps:
(a) mechanically crushing 1kg of dried sweet osmanthus obtained after drying, mixing with a solvent, and performing negative pressure extraction to obtain an extracting solution; wherein the solvent is water, and the ratio of the sweet osmanthus to the solvent is 1: 20, the pressure of negative pressure extraction is-0.06 MPa, the temperature of negative pressure extraction is 30 ℃, the time of negative pressure extraction is 60min, and the times of negative pressure extraction are 1;
centrifuging the extract to remove the precipitate to obtain a supernatant; the rotating speed of the centrifugation is 3000 r/min;
(b) concentrating the supernatant, adsorbing with D101 macroporous adsorbent resin, loading, and eluting with water and 30% ethanol water solution to obtain 10L eluate;
concentrating the eluate under reduced pressure until no alcohol smell exists, freeze drying at-40 deg.C for 24 hr under vacuum degree of 40Pa to obtain flos Osmanthi Fragrantis extract containing acteoside and salidroside.
Example 2
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 1 except that the temperature of the negative pressure extraction in step (a) is 40 ℃.
Example 3
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 1 except that the temperature of the negative pressure extraction in step (a) is 50 ℃.
Example 4
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 1 except that the temperature of the negative pressure extraction in step (a) is 60 ℃.
Example 5
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 1 except that the temperature of the negative pressure extraction in step (a) is 25 ℃.
Example 6
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 1 except that the temperature of the negative pressure extraction in step (a) is 65 ℃.
Example 7
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 3 except that the time for negative pressure extraction in step (a) is 30 min.
Example 8
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 3 except that the time for negative pressure extraction in step (a) is 90 min.
Example 9
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 3 except that the time for negative pressure extraction in step (a) is 120 min.
Example 10
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 3 except that the time for negative pressure extraction in step (a) is 20 min.
Example 11
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 3 except that the pressure of the negative pressure extraction in step (a) is-0.02 MPa.
Example 12
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 3 except that the pressure of negative pressure extraction in step (a) is-0.04 MPa.
Example 13
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 3 except that the pressure of the negative pressure extraction in step (a) is-0.08 MPa.
Example 14
This example provides a method for preparing an osmanthus fragrans extract, which is the same as example 3 except that the pressure of the negative pressure extraction in step (a) is-0.1 MPa.
Example 15
The embodiment provides a preparation method of an osmanthus fragrans extract, which comprises the following steps:
(a) mechanically pulverizing 1kg of dried flos Osmanthi Fragrantis, mixing with solvent for negative pressure extraction for 2 times, and combining the 2 obtained extractive solutions I to obtain extractive solution; wherein the solvent is water, and the ratio of the sweet osmanthus to the solvent is 1: 15, the pressure of negative pressure extraction is-0.08 MPa, the temperature of negative pressure extraction is 60 ℃, and the time of each negative pressure extraction is 60 min;
centrifuging the extract to remove the precipitate to obtain a supernatant; the rotating speed of the centrifugation is 3000 r/min;
(b) concentrating the supernatant, adsorbing with X-5 macroporous adsorbent resin, and eluting with water and 30% ethanol water solution to obtain 10L eluate;
concentrating the eluate under reduced pressure until no alcohol smell exists, and freeze drying at-40 deg.C for 24 hr under 40Pa to obtain flos Osmanthi Fragrantis extract containing acteoside and salidroside.
Example 16
The embodiment provides a preparation method of an osmanthus fragrans extract, which comprises the following steps:
(a) mechanically crushing 1kg of dried osmanthus fragrans flowers obtained after drying, mixing with a solvent for negative pressure extraction for 3 times, and combining the extracting solutions I obtained 3 times to obtain an extracting solution; wherein the solvent is water, and the ratio of the sweet osmanthus to the solvent is 1: 20, the pressure of negative pressure extraction is-0.08 MPa, the temperature of negative pressure extraction is 50 ℃, and the time of each negative pressure extraction is 60 min;
centrifuging the extract to remove the precipitate to obtain a supernatant; the rotating speed of the centrifugation is 3000 r/min;
(b) concentrating the supernatant, adsorbing with X-5 macroporous adsorbent resin, and eluting with water and 30% ethanol water solution to obtain 12L eluate;
concentrating the eluate under reduced pressure until no alcohol smell exists, and freeze drying at-40 deg.C for 24 hr under 40Pa to obtain flos Osmanthi Fragrantis extract containing acteoside and salidroside.
Example 17
The embodiment provides a preparation method of an osmanthus fragrans extract, which comprises the following steps:
(a) mechanically pulverizing 1kg of dried flos Osmanthi Fragrantis, mixing with solvent, and performing negative pressure extraction for 3 times, and combining the 3 obtained extractive solutions I to obtain extractive solution; wherein the solvent is a 30% ethanol water solution, and the feed-liquid ratio of the sweet osmanthus to the solvent is 1: 15, the pressure of negative pressure extraction is-0.06 MPa, the temperature of negative pressure extraction is 50 ℃, and the time of each negative pressure extraction is 60 min;
centrifuging the extract to remove the precipitate to obtain a supernatant; the rotating speed of the centrifugation is 3000 r/min;
(b) concentrating the supernatant, adsorbing with D101 macroporous adsorbent resin, loading, and eluting with water and 30% ethanol water solution to obtain 14L eluate;
concentrating the eluate under reduced pressure until no alcohol smell exists, and freeze drying at-40 deg.C for 24 hr under 40Pa to obtain flos Osmanthi Fragrantis extract containing acteoside and salidroside.
Example 18
The embodiment provides a preparation method of an osmanthus fragrans extract, which comprises the following steps:
(a) mechanically pulverizing 1kg of dried flos Osmanthi Fragrantis, mixing with solvent for negative pressure extraction for 2 times, and combining the 2 obtained extractive solutions I to obtain extractive solution; wherein the solvent is 40% ethanol water solution, and the feed-liquid ratio of the sweet osmanthus to the solvent is 1: 20, the pressure of negative pressure extraction is-0.06 MPa, the temperature of negative pressure extraction is 50 ℃, and the time of each negative pressure extraction is 60 min;
centrifuging the extract to remove the precipitate to obtain a supernatant; the rotating speed of the centrifugation is 3000 r/min;
(b) concentrating the supernatant, adsorbing with D101 macroporous adsorbent resin, loading, and eluting with water and 30% ethanol water solution to obtain 10L eluate;
concentrating the eluate under reduced pressure until no alcohol smell exists, and freeze drying at-40 deg.C for 24 hr under 40Pa to obtain flos Osmanthi Fragrantis extract containing acteoside and salidroside.
Example 19
The embodiment provides a preparation method of an osmanthus fragrans extract, which comprises the following steps:
(a) mechanically pulverizing 1kg of dried flos Osmanthi Fragrantis, mixing with solvent for negative pressure extraction for 2 times, and combining the 2 obtained extractive solutions I to obtain extractive solution; wherein the solvent is a 30% ethanol water solution, and the feed-liquid ratio of the sweet osmanthus to the solvent is 1: 10, the pressure of negative pressure extraction is-0.04 MPa, the temperature of negative pressure extraction is 40 ℃, and the time of each negative pressure extraction is 30 min;
centrifuging the extract to remove the precipitate to obtain a supernatant; the rotating speed of the centrifugation is 3000 r/min;
(b) concentrating the supernatant, adsorbing with D101 macroporous adsorbent resin, and eluting with water and 20% ethanol water solution to obtain 12L eluate;
concentrating the eluate under reduced pressure until no alcohol smell exists, and freeze drying at-40 deg.C for 24 hr under 40Pa to obtain flos Osmanthi Fragrantis extract containing acteoside and salidroside.
Example 20
The embodiment provides a preparation method of an osmanthus fragrans extract, which comprises the following steps:
(a) mechanically pulverizing 1kg of dried flos Osmanthi Fragrantis, mixing with solvent for negative pressure extraction for 2 times, and combining the 2 obtained extractive solutions I to obtain extractive solution; wherein the solvent is water, and the ratio of the sweet osmanthus to the solvent is 1: 10, the pressure of negative pressure extraction is-0.04 MPa, the temperature of negative pressure extraction is 40 ℃, and the time of each negative pressure extraction is 30 min;
centrifuging the extract to remove the precipitate to obtain a supernatant; the rotating speed of the centrifugation is 3000 r/min;
(b) concentrating the supernatant, adsorbing with X-5 macroporous adsorbent resin, and eluting with water and 20% ethanol water solution to obtain 10L eluate;
concentrating the eluate under reduced pressure until no alcohol smell exists, and freeze drying at-40 deg.C for 24 hr under 40Pa to obtain flos Osmanthi Fragrantis extract containing acteoside and salidroside.
Comparative example 1
The comparative example provides a preparation method of an osmanthus extract, which comprises the following steps:
(a) mechanically pulverizing 1kg of dried sweet osmanthus, adding 20 times of water, and extracting under normal pressure to obtain an extracting solution;
the remaining steps and process parameters were the same as in example 3.
Comparative example 2
The comparative example provides a preparation method of an osmanthus extract, which comprises the following steps:
(a) mechanically pulverizing 1kg of dried sweet osmanthus, adding 20 times of 30% ethanol, and extracting under normal pressure to obtain an extracting solution;
the remaining steps and process parameters were the same as in example 3.
Comparative example 3
The comparative example provides a preparation method of the osmanthus fragrans extract, except that the eluent is subjected to reduced pressure concentration in the step (b) and then is subjected to spray drying, the air inlet temperature of the spray drying is 180 ℃, the air outlet temperature of the spray drying is 90 ℃, and other steps and process parameters are the same as those in the example 3.
In order to verify the technical effects of the above examples and comparative examples, the following experimental examples were specifically set.
Experimental example 1
To examine the effect of the negative pressure extraction process parameters on the extract, the solid yield and the mass contents of verbascoside and salidroside in the extract obtained in step (a) of examples 1-14 were determined, and the specific results are shown in Table 1.
TABLE 1
Examples 2 to 6 are the control experiments of example 1. As can be seen from the data in Table 1, the yield of solid is increased with the increase of the negative pressure extraction temperature, the content of acteoside is increased and then decreased, the content of salidroside is gradually increased, and the color of the obtained extract is gradually deepened with the increase of the temperature. When the negative pressure extraction temperature is lower than 30 ℃ (example 5), the solid yield and the contents of verbascoside and salidroside are lower, and when the negative pressure extraction temperature is higher than 60 ℃ (example 6), the content of verbascoside is reduced, and the color of the extract is deepened.
Examples 7-10 are all control experiments of example 3. As can be seen from the data in Table 1, the yield of solid is gradually increased with the increase of the extraction time under negative pressure, the content of verbascoside and the content of salidroside are increased and then decreased, and the color of the extract begins to become dark after the extraction time exceeds 90 min. When the extraction time is less than 30min, the solid yield and the contents of verbascoside and salidroside are lower.
Examples 11-14 are all control experiments of example 3. As can be seen from the data in Table 1, the solid yield and the content of salidroside gradually increase with the increase of the negative pressure extraction pressure, and the content of verbascoside decreases after the negative pressure exceeds-0.06 MPa.
Experimental example 2
The quality of the osmanthus fragrans extracts prepared in the examples and the comparative examples and the mass content of verbascoside and salidroside in the osmanthus fragrans extracts are detected, and specific results are shown in table 2.
TABLE 2
As can be seen from the data in Table 2, the extraction under negative pressure can improve the yield of solid and the content of the active ingredients of osmanthus fragrans, namely verbascoside and salidroside, and the color of the extract is light. By adopting the freeze drying mode, the loss of functional components at high temperature can be avoided, and the deepening of the color of the osmanthus extract caused by spray drying at high temperature can be avoided.
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. The preparation method of the sweet osmanthus extract is characterized by comprising the following steps:
(a) mixing the pretreated sweet osmanthus with a solvent for negative pressure extraction to obtain an extracting solution;
carrying out solid-liquid separation on the extracting solution to obtain supernatant;
(b) concentrating the supernatant, adsorbing by using adsorption resin, and then eluting to obtain an eluent;
concentrating the eluate, and freeze drying to obtain flos Osmanthi Fragrantis extract containing acteoside and salidroside.
2. The preparation method of the osmanthus extract according to claim 1, wherein in the step (a), the solvent comprises water or an aqueous ethanol solution;
preferably, 10-20mL of solvent is used per gram of osmanthus fragrans.
3. The preparation method of osmanthus extract according to claim 1, wherein in the step (a), the pressure of the negative pressure extraction is-0.02 to-0.1 MPa;
preferably, the temperature of the negative pressure extraction is 30-60 ℃;
preferably, the times of negative pressure extraction are 1-3 times;
preferably, the time of each negative pressure extraction is 30-90 min.
4. The preparation method of osmanthus extract according to claim 3, wherein in the step (a), the pressure of the negative pressure extraction is-0.04 to-0.06 MPa;
preferably, the temperature of the negative pressure extraction is 40-50 ℃;
preferably, the times of negative pressure extraction are 2-3 times;
preferably, the time of each negative pressure extraction is 60-90 min.
5. The preparation method of the osmanthus extract according to claim 1, wherein in the step (a), the pretreatment comprises a step of drying and then crushing the osmanthus;
preferably, the solid-liquid separation mode comprises centrifugation;
preferably, the rotation speed of the centrifugation is 3000-.
6. The preparation method of the osmanthus extract according to any one of claims 1 to 5, wherein in the step (b), the adsorption resin comprises D101 macroporous adsorption resin or X-5 macroporous adsorption resin;
preferably, the eluent used for elution comprises water and ethanol aqueous solution;
preferably, the volume fraction of the ethanol aqueous solution used for elution is 10-50%.
7. The method for preparing an osmanthus extract according to any one of claims 1 to 5, wherein in the step (b), the concentration is a reduced pressure concentration.
8. The preparation method of the osmanthus extract according to any one of claims 1 to 5, wherein in the step (b), the temperature of the freeze drying is-40 to-50 ℃;
preferably, the vacuum degree of the freeze drying is 20-60 Pa;
preferably, the freeze-drying time is 24 to 36 hours.
9. An osmanthus extract, characterized by being prepared by the preparation method of the osmanthus extract according to any one of claims 1 to 8;
the sweet osmanthus extract contains verbascoside and salidroside;
preferably, the mass fraction of verbascoside in the sweet osmanthus flower extract is 30-50%, and the mass fraction of salidroside is 2-8%.
10. A cosmetic characterized by comprising the osmanthus extract according to claim 9.
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