CN112438935A - Hemerocallis fulva leaf extracting solution and preparation method and application thereof - Google Patents
Hemerocallis fulva leaf extracting solution and preparation method and application thereof Download PDFInfo
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- CN112438935A CN112438935A CN202011454292.8A CN202011454292A CN112438935A CN 112438935 A CN112438935 A CN 112438935A CN 202011454292 A CN202011454292 A CN 202011454292A CN 112438935 A CN112438935 A CN 112438935A
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- hemerocallis fulva
- hemerocallis
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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]
- A61K8/9794—Liliopsida [monocotyledons]
-
- 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
- A61K8/67—Vitamins
- A61K8/676—Ascorbic acid, i.e. vitamin C
-
- 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
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening 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
- A61K2800/74—Biological properties of particular ingredients
- A61K2800/78—Enzyme modulators, e.g. Enzyme agonists
- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- 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
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Dermatology (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Engineering & Computer Science (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Cosmetics (AREA)
Abstract
The invention belongs to the technical field of cosmetics, and particularly relates to a hemerocallis fulva leaf extracting solution as well as a preparation method and application thereof. The preparation method of the hemerocallis fulva leaf extracting solution comprises the following steps: processing the dry hemerocallis fulva leaf powder by adopting an ultrasonic-ethanol synergistic extraction method to obtain a hemerocallis fulva leaf dry powder ultrasonic treatment liquid, and carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to obtain a hemerocallis fulva leaf extracting solution. The method fills the blank of extracting the hemerocallis fulva leaves, solves the problem that the hemerocallis fulva leaves cannot be effectively utilized in the prior art, and improves the additional value of the hemerocallis fulva planting. The hemerocallis fulva leaf extracting solution prepared by the method disclosed by the invention can effectively play a role in high antioxidation, moisturizing and skin firming effects when being applied to the hemerocallis fulva leaf lotion.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a hemerocallis fulva leaf extracting solution as well as a preparation method and application thereof.
Background
Toning lotion is one of the most fluid liquids in all cosmetics, and has the effects of supplementing and maintaining the moisture of the skin stratum corneum, softening the stratum corneum and keeping the normal function of the stratum corneum, and from this viewpoint, the toning lotion is also called emollient water. Since the 90 s of the 21 st century, the lotion still has the main effects of moisturizing and moistening skin, but the effect of the lotion is far beyond the range and is expanded to have the effects of resisting oxidation, resisting aging, astringing, sterilizing, cleaning, regulating sebum secretion, whitening, peeling dead skin (aged cuticle) and the like. The advantage and trend of cosmetics are that natural plant extract is added into the cosmetics as cosmetic raw material. Natural plant cosmetics are popular with consumers due to the characteristics of nature, mildness, no irritation, high safety and the like, and the natural plant cosmetics are a necessary trend for the development of the cosmetics.
Hemerocallis fulva (scientific name) is a plant of the genus Hemerocallis of the family Liliaceae, and has been used as an edible and medicinal crop in the east Asia for a thousand years. Hemerocallis fulva is used as a medicine and food dual-purpose flower, and roots, stems, leaves and flowers of the Hemerocallis fulva can be used as medicines, and buds of the Hemerocallis fulva can be used as golden day vegetables. The hemerocallis fulva has various biological activities and has wide application in health preservation and medical treatment. The diversity of biological activities of hemerocallis fulva is closely related to the natural components they are rich in. It has been found that hemerocallis contain various bioactive substances such as flavones, lactams, carotenoids, alkaloids, steroids, and the like. Research results at home and abroad show that the hemerocallis contain various flavonoids such as quercetin, rutin, isorhamnetin, kaempferol and the like, the research on the extraction process of the flavone in the hemerocallis and the analysis and detection of the antioxidant effect are favorable for developing flavone resources in the hemerocallis leaves, and the application of the flavone resources in the field of cosmetics can greatly improve the economic value of the hemerocallis.
In recent years, studies on hemerocallis have focused on the development and utilization of hemerocallis flowers, and studies on the extraction process and efficacy of hemerocallis leaves and lotions prepared based on active ingredients extracted from hemerocallis leaves have not been reported at present.
Disclosure of Invention
The preparation method of the hemerocallis fulva leaf extracting solution can well extract effective components in the hemerocallis fulva leaves and apply the effective components to the astringent, so that a large number of mature leaves generated in the growing process of the hemerocallis fulva are effectively utilized, and the additional value of the hemerocallis fulva planting is improved.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a preparation method of a hemerocallis fulva leaf extracting solution, which comprises the following steps:
processing the dry hemerocallis fulva leaf powder by adopting an ultrasonic-ethanol synergistic extraction method to obtain a hemerocallis fulva leaf dry powder ultrasonic treatment liquid;
and carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to obtain a hemerocallis fulva leaf extracting solution.
Preferably, the mass to ethanol volume ratio of the hemerocallis fulva leaf dry powder is 1 g: 20-60 mL.
Preferably, the ultrasonic power is 100-200W, the temperature is 40-80 ℃, the time is 20-60 min, and the frequency is 30-50 kHz during the ultrasonic-ethanol synergistic extraction.
Preferably, the particle size of the dry hemerocallis fulva leaf powder is 40-60 meshes.
The hemerocallis fulva leaf extracting solution prepared by the preparation method in the technical scheme is provided by the invention.
The invention provides application of the hemerocallis fulva leaf extracting solution in toning lotion.
The invention also provides day lily leaf lotion which comprises the following components: the hemerocallis fulva leaf extracting solution, sodium hyaluronate, vitamin C and water.
Preferably, the day lily leaf lotion comprises the following components in percentage by mass: 15-25% of hemerocallis fulva leaf extracting solution, 0.01-0.03% of sodium hyaluronate, 0.005-0.015% of vitamin C and the balance of water.
The invention provides a preparation method of day lily leaf toning lotion in the technical scheme, which comprises the following steps:
mixing the hemerocallis fulva leaf extracting solution, sodium hyaluronate, vitamin C and water to obtain a mixed solution;
and filtering the mixed solution by using a filter membrane to obtain the day lily leaf toning lotion.
Preferably, the pore size of the filter membrane is 0.22 μm, and the temperature of the mixing is room temperature.
According to the preparation method of the hemerocallis fulva leaf extracting solution, the effective components in the hemerocallis fulva leaf dry powder are extracted by an ultrasonic-ethanol synergistic extraction method, and finally, the impurity part and the effective components are separated by suction filtration to obtain the hemerocallis fulva leaf extracting solution. The method effectively fills the blank of the extraction of the hemerocallis fulva leaves, solves the problem that the hemerocallis fulva leaves in the prior art cannot be effectively utilized, and improves the additional value of the hemerocallis fulva planting.
In addition, the invention also provides application of the hemerocallis fulva leaf extracting solution in the astringent, and the astringent takes the hemerocallis fulva leaf extracting solution, sodium hyaluronate, vitamin C and water as components. The day lily leaf lotion provided by the invention takes the day lily leaf extracting solution as a main component, so that the obtained lotion has the characteristics of being mild, not irritating and high in safety, the flavone content in the day lily leaf extracting solution is high, the effect of high antioxidation is achieved, and the effects of resisting free radicals and inhibiting tyrosinase can be further improved by matching with vitamin C, so that the formation of color spots is inhibited, the original color spots are lightened, and the skin color is brightened; the day lily leaf toning lotion provided by the invention takes the sodium hyaluronate as a component, so that the obtained toning lotion has strong lubricating feeling and film-forming property, and the sodium hyaluronate can permeate into the epidermis layer of skin to promote the supply of skin nutrition and the excretion of waste, thereby playing the roles of high oxidation resistance, moisture retention and skin tightening.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a rutin standard curve;
FIG. 2 shows DPPH clearance of day lily leaf lotion prepared in examples 1 and 2, and commercial muscle water, Job's tears water, and 10 μ g/mL vitamin C solution;
FIG. 3 is a graph showing the total flavone content of the dry powder of leaves of Hemerocallis fulva of example 5;
FIG. 4 is a graph showing the total flavone content of the dry powder of leaves of Hemerocallis fulva of example 6;
FIG. 5 is a graph showing the total flavone content of the dry powder of leaves of Hemerocallis fulva of example 7.
Detailed Description
The invention provides a preparation method of a hemerocallis fulva leaf extracting solution, which comprises the following steps:
processing the dry hemerocallis fulva leaf powder by adopting an ultrasonic-ethanol synergistic extraction method to obtain a hemerocallis fulva leaf dry powder ultrasonic treatment liquid;
and carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to obtain a hemerocallis fulva leaf extracting solution.
The method adopts an ultrasonic-ethanol synergistic extraction method to treat dry hemerocallis fulva leaf powder to obtain an ultrasonic treatment solution of the dry hemerocallis fulva leaf powder. In the present invention, the volume ratio of the dry hemerocallis fulva leaf powder to ethanol is preferably 1 g: 20-60 mL, more preferably 1 g: 40-60 mL, more preferably 1 g: 50 mL. In the invention, the power of ultrasound during the ultrasound-ethanol synergistic extraction is preferably 100-200W, more preferably 125-175W, and more preferably 150W; the temperature is preferably 40-80 ℃, more preferably 50-70 ℃, and more preferably 60 ℃; the time is preferably 20-60 min, more preferably 30-50 min, and even more preferably 40 min; the frequency is preferably 30 to 50kHz, more preferably 35 to 45kHz, and even more preferably 40 kHz. The method utilizes an ultrasonic-ethanol synergistic extraction method to extract effective components in dried hemerocallis fulva leaves, wherein ultrasonic extraction is to extract the effective components of plants by utilizing ultrasonic cavitation, and the ultrasonic extraction method can simplify the operation process, shorten the extraction time, improve the extraction yield and further ensure the content of the effective active components in the final extracting solution; the ethanol is a good solvent for the total flavonoids, the total flavonoids can be effectively extracted, and the ethanol is used for extraction, so that the obtained extracting solution is easy to concentrate and dry, and the damage of the complicated purification process to the effective components of the hemerocallis fulva leaves is avoided. The method utilizes an ultrasonic-ethanol synergistic extraction method to extract the active substances in the hemerocallis fulva leaves, so that the active ingredients in the hemerocallis fulva leaves can be fully extracted, and meanwhile, the decomposition of the active substances is effectively avoided. Furthermore, the method utilizes the specific mass-to-volume ratio of the dry hemerocallis fulva leaf powder to the ethanol, ultrasonic power, temperature and time, so that the poor extraction effect caused by poor ultrasonic degree is avoided, and the active substances are prevented from being damaged caused by overhigh ultrasonic degree.
In the invention, the particle size of the dry hemerocallis fulva leaf powder is preferably 40-60 meshes, and more preferably 50 meshes; the dry hemerocallis fulva leaf powder is preferably obtained by crushing dry hemerocallis fulva leaves. In the invention, the dried hemerocallis fulva leaves are preferably sieved after being crushed to obtain dry hemerocallis fulva leaf powder, and the number of the sieved meshes is preferably 40-60 meshes, and more preferably 50 meshes. In the crushing process, the uniform dry hemerocallis fulva leaf powder with high refining degree can be obtained by limiting the number of the sieved screens, and the effective components of the dry hemerocallis fulva leaf powder can be fully extracted in the extraction process through ultrasonic-ethanol synergistic extraction, so that the utilization rate of the hemerocallis fulva leaves is improved.
In the invention, the preparation method of the dried hemerocallis fulva leaves is preferably obtained by vacuum freeze-drying or natural sunlight drying of fresh hemerocallis fulva leaves. According to the invention, the fresh hemerocallis fulva leaves are treated by selecting a natural sunlight drying mode, so that the preparation cost can be reduced, the purchase of instruments and equipment is reduced, and the transportation cost is reduced; the method for treating the fresh hemerocallis fulva leaves by selecting a vacuum freeze-drying mode can avoid the damage of the drying process to the effective active ingredients of the hemerocallis fulva leaves, and improve the oxidation resistance of the hemerocallis fulva leaf extracting solution. When dried hemerocallis fulva leaves are prepared by vacuum freeze-drying, the vacuum drying conditions preferably include: vacuum-drying at-50 deg.C for 18h by using vacuum freeze dryer.
According to the technical scheme, the active substances in the hemerocallis fulva leaves can be extracted, the blank of extracting the hemerocallis fulva leaves is effectively filled, and the problem that the hemerocallis fulva leaves cannot be effectively utilized in the prior art is solved. Moreover, the hemerocallis leaves are a byproduct in the cultivation of hemerocallis, special cultivation is not needed, the hemerocallis are peeled off regularly, the regeneration of the hemerocallis is not influenced, the hemerocallis has wider sources compared with hemerocallis flowers and hemerocallis tender buds, and the additional value of the hemerocallis planting is improved.
After obtaining the hemerocallis fulva leaf dry powder ultrasonic treatment liquid, carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to obtain a hemerocallis fulva leaf extracting solution. In the present invention, the suction filtration may be performed by a suction filtration operation known to those skilled in the art, and preferably, a vacuum filtration is used as the suction filtration; the method separates the fiber from the liquid part in the hemerocallis fulva leaf extracting solution in the suction filtration process, so that the clarification of the hemerocallis fulva leaf extracting solution is ensured.
The invention also provides the hemerocallis fulva leaf extracting solution prepared by the preparation method in the technical scheme. In the present invention, the effective component of the hemerocallis fulva leaf extract is preferably total flavonoids. In the invention, the content of total flavonoids extracted from the dry hemerocallis fulva leaf powder is preferably more than 18mg/g, and more preferably 20-22 mg/g. By adopting the method provided by the invention, the total flavone of the hemerocallis fulva leaves can be extracted to the maximum extent through an optimized process, and the hemerocallis fulva leaf extracting solution with higher total flavone content is obtained.
The invention also provides application of the hemerocallis fulva leaf extracting solution in toning lotion.
The invention also provides day lily leaf lotion which comprises the following components: the hemerocallis fulva leaf extracting solution, the sodium hyaluronate, the vitamin C and the water in the technical scheme. The day lily leaf extracting solution is used as a component, so that the obtained lotion has the characteristics of being mild, not irritating and high in safety, and the day lily leaf extracting solution is high in flavone content and has a high anti-oxidation effect. The cosmetic lotion has the advantages that the sodium hyaluronate is used as the component, so that the obtained cosmetic lotion has strong lubricating feeling and film-forming property, and the sodium hyaluronate can permeate into the epidermis layer of the skin to promote the supply of skin nutrition and the excretion of waste, thereby playing the roles of high oxidation resistance, moisture retention and skin tightening. In the invention, the vitamin C has oxidation resistance, and can be matched with the hemerocallis fulva leaf extract to further improve the effects of resisting free radicals and inhibiting tyrosinase and brighten skin color. In the invention, the DPPH clearance of the day lily leaf toning lotion is preferably 90% or more, and more preferably 91.88-93.69%.
The hemerocallis fulva leaf cosmetic water provided by the invention preferably comprises 15-25% of hemerocallis fulva leaf extracting solution, more preferably 18-22% of hemerocallis fulva leaf extracting solution, and more preferably 20% of hemerocallis fulva leaf extracting solution. The method utilizes the hemerocallis fulva leaf extracting solution with a specific mass percentage, so that the problems that the hemerocallis fulva leaf extracting solution has low content and cannot play an antioxidation effect, and the raw material waste caused by the high content of the hemerocallis fulva leaf extracting solution and the unobvious improvement degree of the antioxidation effect are avoided.
The day lily leaf lotion provided by the invention preferably comprises 0.01-0.03% of sodium hyaluronate, more preferably 0.015-0.025%, and even more preferably 0.02% by mass. According to the invention, the sodium hyaluronate with a specific mass percentage is utilized, so that the problems that the content of the sodium hyaluronate is high, the viscosity of the lotion is high, the original effect of easy flowing cannot be kept are solved, the problem that the lotion cannot be effectively maintained on the surface of the skin due to too low content of the sodium hyaluronate, the smoothness and the film forming degree are low, and the problem that effective components cannot be ensured to permeate into the epidermis layer of the skin are solved.
The day lily leaf cosmetic water provided by the invention preferably comprises 0.005-0.015 per thousand of vitamin C, more preferably 0.007-0.013 per thousand of vitamin C, and even more preferably 0.01 per thousand of vitamin C. According to the invention, the vitamin C with a specific mass percentage is utilized, so that the problems that the content of the vitamin C is low, the vitamin C cannot generate a synergistic effect with the hemerocallis fulva leaf extracting solution, the antioxidant effect cannot be further improved, the content of the vitamin C is high, the improvement degree of the antioxidant effect is not obvious, and the raw material waste is caused are avoided.
The day lily leaf lotion provided by the invention further comprises the balance of water, and the water is preferably deionized water.
The invention also provides a preparation method of the hemerocallis fulva leaf lotion, which comprises the following steps:
mixing the hemerocallis fulva leaf extracting solution, sodium hyaluronate, vitamin C and water to obtain a mixed solution;
and filtering the mixed solution by using a filter membrane to obtain the day lily leaf toning lotion.
The preparation method comprises the step of mixing a hemerocallis fulva leaf extracting solution, sodium hyaluronate, vitamin C and water to obtain a mixed solution. In the invention, the hemerocallis fulva leaf extracting solution is obtained by the preparation method in the technical scheme. In the present invention, the mixing is preferably performed under stirring conditions, the mixing temperature is preferably room temperature, and the present invention has no special requirement on the specific parameters of the stirring, and the stirring method known to those skilled in the art can be adopted. The stirring temperature is limited to room temperature, so that the decomposition of effective substances cannot occur in the stirring process, and the content of the effective active ingredients of the hemerocallis fulva leaf toning lotion is ensured.
After the mixed solution is obtained, the mixed solution is filtered by using a filter membrane to obtain the day lily leaf toning lotion. In the present invention, the pore size of the filter is preferably 0.22. mu.m. The method utilizes the filter membrane for filtration, and can further remove impurities and microorganisms in the hemerocallis fulva leaf toning lotion and the hemerocallis fulva leaf extracting solution, so that the safety of the hemerocallis fulva leaf toning lotion is improved.
For further illustration of the present invention, the following detailed description will be made of the preparation method and application of the extract of hemerocallis fulva leaves provided by the present invention with reference to the accompanying drawings and examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Cleaning and airing fresh hemerocallis fulva leaves, drying by using a vacuum freeze dryer, crushing the obtained hemerocallis fulva leaves into fine powder, and sieving the fine powder with a 50-mesh sieve to obtain dry hemerocallis fulva leaf powder;
adding the obtained dry hemerocallis fulva leaf powder into ethanol, wherein the mass to volume ratio of the hemerocallis fulva leaf powder to the ethanol is 1 g: 50mL, and after uniformly stirring, carrying out ultrasonic treatment for 40min under the conditions of power of 150W, frequency of 40kHz and temperature of 60 ℃ to obtain an ultrasonic treatment solution of dry hemerocallis fulva leaf powder;
carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to obtain a hemerocallis fulva leaf extracting solution;
mixing the hemerocallis fulva leaf extracting solution, sodium hyaluronate, vitamin C and deionized water at room temperature to obtain a mixed solution; the ingredients by weight percentage are as follows: 20% of hemerocallis fulva leaf extracting solution, 0.02% of sodium hyaluronate, 0.01% of vitamin C and the balance of deionized water;
and filtering the mixed solution by using a filter membrane with the diameter of 0.22 mu m to obtain the day lily leaf toning lotion.
Example 2
Cleaning fresh hemerocallis fulva leaves, airing, carrying out sun-drying treatment by utilizing natural sunlight, crushing the obtained hemerocallis fulva leaves into fine powder, and sieving the fine powder with a 50-mesh sieve to obtain dry hemerocallis fulva leaf powder;
adding the obtained dry hemerocallis fulva leaf powder into ethanol, wherein the mass to volume ratio of the hemerocallis fulva leaf powder to the ethanol is 1 g: 50mL, and after uniformly stirring, carrying out ultrasonic treatment for 40min under the conditions of power of 150W, frequency of 40kHz and temperature of 60 ℃ to obtain an ultrasonic treatment solution of dry hemerocallis fulva leaf powder;
carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to obtain a hemerocallis fulva leaf extracting solution;
mixing the hemerocallis fulva leaf extracting solution, sodium hyaluronate, vitamin C and deionized water at room temperature to obtain a mixed solution; the ingredients by weight percentage are as follows: 20% of hemerocallis fulva leaf extracting solution, 0.02% of sodium hyaluronate, 0.01% of vitamin C and the balance of deionized water;
and filtering the mixed solution by using a filter membrane with the diameter of 0.22 mu m to obtain the day lily leaf toning lotion.
Example 3
Cleaning and airing fresh hemerocallis fulva leaves, drying by using a vacuum freeze dryer, crushing the obtained hemerocallis fulva leaves into fine powder, and sieving the fine powder with a 50-mesh sieve to obtain dry hemerocallis fulva leaf powder;
adding the obtained dry hemerocallis fulva leaf powder into ethanol, wherein the mass to volume ratio of the hemerocallis fulva leaf powder to the ethanol is 1 g: 50mL, and after uniformly stirring, carrying out ultrasonic treatment for 40min under the conditions of power of 150W, frequency of 40kHz and temperature of 60 ℃ to obtain an ultrasonic treatment solution of dry hemerocallis fulva leaf powder;
carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to obtain a hemerocallis fulva leaf extracting solution;
mixing the hemerocallis fulva leaf extracting solution, sodium hyaluronate, vitamin C and deionized water at room temperature to obtain a mixed solution; the ingredients by weight percentage are as follows: 15% of hemerocallis fulva leaf extracting solution, 0.02% of sodium hyaluronate, 0.01% of vitamin C and the balance of deionized water;
and filtering the mixed solution by using a filter membrane with the diameter of 0.22 mu m to obtain the day lily leaf toning lotion.
Example 4
Cleaning and airing fresh hemerocallis fulva leaves, drying by using a vacuum freeze dryer, crushing the obtained hemerocallis fulva leaves into fine powder, and sieving the fine powder with a 50-mesh sieve to obtain dry hemerocallis fulva leaf powder;
adding the obtained dry hemerocallis fulva leaf powder into ethanol, wherein the mass to volume ratio of the hemerocallis fulva leaf powder to the ethanol is 1 g: 50mL, and after uniformly stirring, carrying out ultrasonic treatment for 40min under the conditions of power of 150W, frequency of 40kHz and temperature of 60 ℃ to obtain an ultrasonic treatment solution of dry hemerocallis fulva leaf powder;
carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to obtain a hemerocallis fulva leaf extracting solution;
mixing the hemerocallis fulva leaf extracting solution, sodium hyaluronate, vitamin C and deionized water at room temperature to obtain a mixed solution; the ingredients by weight percentage are as follows: 25% of hemerocallis fulva leaf extracting solution, 0.02% of sodium hyaluronate, 0.01% of vitamin C and the balance of deionized water;
and filtering the mixed solution by using a filter membrane with the diameter of 0.22 mu m to obtain the day lily leaf toning lotion.
Example 5
Cleaning and airing fresh hemerocallis fulva leaves, drying by using a vacuum freeze dryer, crushing the obtained hemerocallis fulva leaves into fine powder, and sieving the fine powder with a 50-mesh sieve to obtain dry hemerocallis fulva leaf powder;
adding the obtained dry hemerocallis fulva leaf powder into ethanol, wherein the mass to volume ratio of the hemerocallis fulva leaf powder to the ethanol is 1 g: 50mL, and after uniformly stirring, respectively carrying out ultrasonic treatment for 40min under the conditions that the power is 150W, the frequency is 40kHz, and the temperature is 40 ℃, 50 ℃, 60 ℃, 70 ℃ and 80 ℃ respectively to obtain an ultrasonic treatment solution of the dry hemerocallis fulva leaf powder;
and (4) carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to respectively obtain hemerocallis fulva leaf extracting solution.
Example 6
Cleaning and airing fresh hemerocallis fulva leaves, drying by using a vacuum freeze dryer, crushing the obtained hemerocallis fulva leaves into fine powder, and sieving the fine powder with a 50-mesh sieve to obtain dry hemerocallis fulva leaf powder;
adding the obtained dry hemerocallis fulva leaf powder into ethanol, wherein the mass to volume ratio of the hemerocallis fulva leaf powder to the ethanol is 1 g: 50mL, and after uniformly stirring, respectively carrying out ultrasonic treatment on the hemerocallis fulva dry powder for 20min, 30min, 40min, 50min and 60min under the conditions that the power is 150W, the frequency is 40kHz and the temperature is 60 ℃ to obtain an ultrasonic treatment solution of the hemerocallis fulva dry powder;
and respectively carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to obtain a hemerocallis fulva leaf extracting solution.
Example 7
Cleaning and airing fresh hemerocallis fulva leaves, drying by using a vacuum freeze dryer, crushing the obtained hemerocallis fulva leaves into fine powder, and sieving the fine powder with a 50-mesh sieve to obtain dry hemerocallis fulva leaf powder;
adding the obtained dry hemerocallis fulva leaf powder into ethanol, wherein the mass ratio of the dry hemerocallis fulva leaf powder to the volume ratio of the ethanol is 1 g: 20mL, 1 g: 30mL, 1 g: 40mL, 1 g: 50mL, 1 g: 60mL, and after uniformly stirring, carrying out ultrasonic treatment for 40min under the conditions of power of 150W, frequency of 40kHz and temperature of 60 ℃ to obtain an ultrasonic treatment solution of dry hemerocallis fulva leaf powder;
and respectively carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to obtain a hemerocallis fulva leaf extracting solution.
Effect example 1 measurement of Total Flavonoids content in Hemerocallis leaf extract
Drawing a standard curve: accurately weighing constant weight rutin 5.0mg, dissolving with 60% ethanol, and diluting to 50mL to obtain standard solution with concentration of 0.1 mg/mL. Accurately measuring rutin standard solution 0, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, placing in 10mL colorimetric tube, adding 5% NaNO20.3mL, shake, stand for 6 min; adding 10% Al (NO)3)30.3mL, shake, stand for 6 min;adding 4mL of 10% NaOH, diluting to constant volume with 60% ethanol, and mixing; the first cuvette was used as a blank control and absorbance was measured at 510nm after development for 15 min. Drawing a standard curve with mass concentration (mg/mL) as abscissa and absorbance as ordinate as shown in FIG. 1, and obtaining a regression equation of y-11.047 x +0.0041 (R)2＝0.9999)。
The calculation formula of the total flavone content is shown as formula I:
m1cv/m, formula I;
in the formula I, m1The content (mg/g) of the total flavone of the hemerocallis fulva leaf dry powder, and c is the concentration (mg/mL) of the total flavone of the hemerocallis fulva leaf extracting solution; v is the volume (mL) of the extract of hemerocallis fulva leaves; m is the mass of dry hemerocallis fulva leaf powder. In the invention, the volume constant volume of the hemerocallis fulva leaf extracting solution is 100mL, namely v in the formula I is 100 mL.
And (3) total flavone content determination: 1mL of the extract solution of hemerocallis fulva leaf obtained in example 1 and 1mL of the extract solution of hemerocallis fulva leaf obtained in example 2 were transferred to a 10mL colorimetric tube, and the contents of the extracts were measured by the method for preparing a calibration curve. The flavonoid concentrations in the extract of Hemerocallis fulva leaf of example 1 and the extract of Hemerocallis fulva leaf of example 2 were 0.22mg/mL and 0.18mg/mL, respectively, as calculated by fitting the equation in FIG. 1. The content of total flavonoids extracted from the dry hemerocallis fulva leaf powder was calculated according to the calculation formula of total flavonoids in the dry hemerocallis fulva leaf powder, and the result shows that the content of total flavonoids extracted from the hemerocallis fulva leaf powder obtained in examples 1 and 2 respectively reaches 22mg/g and 18 mg/g.
Effect example 2 measurement of antioxidant Properties of day lily leaf toning lotion by DPPH method
And (4) determining the DPPH free radical clearance effect by utilizing an improved Nagai method, and judging the oxidation resistance of the day lily leaf toning lotion.
Weighing 2mg of DPPH powder, dissolving the DPPH powder in 50mL of absolute ethyl alcohol, carrying out ultrasonic treatment for 20-30 minutes, measuring the absorbance at 517nm, and controlling the absorbance to be 1.2-1.3 to obtain DPPH solution; adding the day lily leaf cosmetic water into the DPPH solution and the absolute ethyl alcohol with the same volume respectively, standing the mixture at room temperature in a dark place for 30min, and measuring the absorbance at 517nm respectively. And simultaneously measuring the absorbance at 517nm after the mixed solution of the DPPH solution and the absolute ethyl alcohol which are mixed in equal volume is placed for 30min in a dark room temperature.
And calculating the DPPH free radical clearance rate according to the measured absorbance, wherein the calculation formula is shown as a formula II:
in the formula II, A1And A10Respectively adding equal volume of DPPH solution and anhydrous ethanol into day lily leaf astringent, standing in dark at room temperature for 30min, and keeping the absorbance at 517 nm;
Axis a mixed solution obtained by mixing a DPPH solution and absolute ethyl alcohol in equal volume, and the mixed solution is placed in a dark place at room temperature for 30min and then the absorbance is measured at 517 nm.
The DPPH clearance of the day lily leaf lotion obtained in example 1 and example 2, and the commercially available muscle water, coix seed water and vitamin C solution of 10 μ g/mL were measured by the above-mentioned measurement method, and the measurement results are shown in table 1 and fig. 2:
TABLE 1 DPPH clearance of four lotions
As can be seen from the results in table 1 and fig. 2, the DPPH removal rate of the day lily leaf lotion prepared in example 1 is slightly higher than that of the day lily leaf lotion prepared in example 2, and the DPPH removal rates of the day lily leaf lotions prepared in examples 1 and 2 are all higher than those of muscle water, coix seed water and 10 μ g/mL vitamin C solution. Therefore, the DPPH radical scavenging ability of the day lily leaf lotion prepared in examples 1 and 2 is higher than that of the lotion containing only 10 μ g/mL of vitamin C and other lotions on the market, and it can be seen that the day lily leaf lotion prepared from freeze-dried day lily leaves has slightly better anti-oxidation effect than that of the day lily leaf lotion prepared from day lily leaves dried in the natural sunlight.
The DPPH clearance of the day lily leaf cosmetics obtained in example 3 and example 4 was measured by the above measurement method, and compared with example 1, the measurement results are shown in table 2:
TABLE 2 DPPH removal Rate of Hemerocallis leaf lotions obtained in examples 1 to 3
As can be seen from the DPPH clearance results of the hemerocallis leaves toning lotion obtained in table 2, the weight percentage of the hemerocallis leaves extract in the hemerocallis leaves toning lotion of example 3 is 15%, compared with that of example 1 in which the weight percentage of the hemerocallis leaves extract is 20%, the oxidation resistance effect is significantly reduced; example 4 the content of the extract solution of leaves of hemerocallis fulva in the hemerocallis fulva leaf cosmetic water is 25% by mass, and the oxidation resistance effect is slightly improved compared with example 1 in which the content of the extract solution of leaves of hemerocallis fulva is 20% by mass. Therefore, the day lily leaf extract is limited to 15-25% by mass, so that the day lily leaf lotion has high oxidation resistance, and is further limited to 20%, and the oxidation resistance effect of the day lily leaf extract is ensured and is not wasted.
Effect example 3
The total flavonoids in the dry powders of daylily leaves of examples 5, 6 and 7 were measured by the method of effect example 1, as shown in fig. 3, 4 and 5.
As can be seen from FIGS. 3 to 5, the weight-to-ethanol volume ratio of the dry hemerocallis fulva leaf powder is defined as 1 g: 20-60 mL of the hemerocallis fulva leaf extract with high content of total flavonoids can be obtained by extracting the total flavonoids in the hemerocallis fulva leaf dry powder to the maximum extent at the ultrasonic treatment temperature of 40-80 ℃ for 20-60 min. The best extraction conditions of the hemerocallis fulva leaf extract are as follows: the temperature is 60 ℃, the time is 40min, and the ratio of material to liquid is 1 g: 50 mL.
Effect example 4 sensory evaluation of Hemerocallis leaf toning lotion
Clinical experimental evaluation was performed on the day lily leaf lotion obtained in example 1 and example 2.
The clinical experimental conditions were: 40 female volunteers aged 20 to 45 years were divided into 2 experimental groups according to age and skin level, and evaluated from the perspective of appearance, spreadability, skin feel when applied, stickiness, and absorption rate using the day lily leaf lotion obtained in example 1 and example 2, respectively. Sensory evaluation tables of day lily leaves lotions of example 1 and example 2 are shown in table 3 below:
TABLE 3 sensory evaluation Table for Hemerocallis fulva leaf toning lotion
| Evaluation item | Evaluation criteria | Example 1 | Example 2 |
| Appearance form | Dislike-like (1-5 points) | 3.4±0.22 | 3.3±0.25 |
| Spreadability | Poor-good (1-5) points | 3.1±0.34 | 3.2±0.19 |
| Skin feel when applying | Poor-good (1-5) points | 3.5±0.15 | 3.4±0.34 |
| Sticky feeling | Presence-absence (1-5) of | 3.8±0.11 | 3.8±0.23 |
| Absorption rate | Slow-fast (1-5) points | 3.5±0.27 | 3.6±0.15 |
| Integral fraction | Poor-good (1-5) points | 3.7±0.16 | 3.5±0.21 |
As can be seen from the sensory evaluation table of the day lily leaf lotions in table 3, the day lily leaf lotions obtained in example 1 and example 2 did not have much difference in sensory scores in appearance, spreadability, skin feel at application, stickiness, and absorption speed, and example 1 was slightly higher than example 2 in the overall score.
From the experimental results, the day lily leaf lotion provided by the invention has a high oxidation resistance effect and can achieve the effects of moisturizing and tightening skin. In addition, according to the method for extracting the hemerocallis fulva leaves, provided by the invention, the fresh hemerocallis fulva leaves are treated in a natural sunlight drying mode, so that the preparation cost can be reduced, the purchase of instruments and equipment is reduced, and the transportation cost is reduced; the fresh hemerocallis fulva leaves are treated in a vacuum freeze-drying mode, so that the damage to the effective active ingredients of the hemerocallis fulva leaves in the drying process can be avoided, and the oxidation resistance of the hemerocallis fulva leaf extracting solution is improved; the natural extracting solution of the hemerocallis fulva leaves is applied to the cosmetics, so that the additional value of the hemerocallis fulva planting can be effectively improved, and waste is turned into wealth; the selection of the preparation method provides an effective idea for the industrial production of the hemerocallis fulva leaves.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are within the scope of the present invention.
Claims (10)
1. The preparation method of the hemerocallis fulva leaf extracting solution is characterized by comprising the following steps of:
processing the dry hemerocallis fulva leaf powder by adopting an ultrasonic-ethanol synergistic extraction method to obtain a hemerocallis fulva leaf dry powder ultrasonic treatment liquid;
and carrying out suction filtration on the hemerocallis fulva leaf dry powder ultrasonic treatment liquid to obtain a hemerocallis fulva leaf extracting solution.
2. The preparation method according to claim 1, wherein the mass to volume ratio of the dry hemerocallis fulva leaf powder to ethanol is 1 g: 20-60 mL.
3. The preparation method according to claim 1, wherein the ultrasonic power is 100-200W, the temperature is 40-80 ℃, the time is 20-60 min, and the frequency is 30-50 kHz.
4. The method according to claim 1, wherein the dry hemerocallis fulva leaf powder has a particle size of 40-60 mesh.
5. An extract of leaves of Hemerocallis fulva prepared by the method according to any one of claims 1 to 4.
6. The use of an extract of hemerocallis fulva leaves of claim 5 in a cosmetic lotion.
7. The day lily leaf lotion is characterized by comprising the following components: the daylily leaf extract of claim 5, sodium hyaluronate, vitamin C and water.
8. The day lily leaf lotion according to claim 7, wherein the day lily leaf lotion comprises the following components in percentage by mass: 15-25% of hemerocallis fulva leaf extracting solution, 0.01-0.03% of sodium hyaluronate, 0.005-0.015% of vitamin C and the balance of water.
9. The method for preparing day lily leaf toning lotion according to any one of claims 7 to 8, comprising the following steps:
mixing the hemerocallis fulva leaf extracting solution, sodium hyaluronate, vitamin C and water to obtain a mixed solution;
and filtering the mixed solution by using a filter membrane to obtain the day lily leaf toning lotion.
10. The method as claimed in claim 9, wherein the pore size of the filter membrane is 0.22 μm, and the temperature of the mixing is room temperature.
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| CN113875860A (en) * | 2021-10-20 | 2022-01-04 | 上海应用技术大学 | Hemerocallis fulva leaf tea beverage rich in flavone and preparation method thereof |
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