CN113057917A - Abelmoschus manihot anti-aging composition and preparation method and application thereof - Google Patents

Abelmoschus manihot anti-aging composition and preparation method and application thereof Download PDF

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CN113057917A
CN113057917A CN202110255490.XA CN202110255490A CN113057917A CN 113057917 A CN113057917 A CN 113057917A CN 202110255490 A CN202110255490 A CN 202110255490A CN 113057917 A CN113057917 A CN 113057917A
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CN113057917B (en
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张利春
黄丽翠
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Guangzhou Meizihe Cosmetics Co ltd
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Guangdong Chuangmei Anti Aging Research Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • A61K8/9728Fungi, e.g. yeasts
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9794Liliopsida [monocotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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Abstract

The invention discloses an anti-aging Abelmoschus manihot composition and a preparation method and application thereof. The anti-aging composition is mainly prepared by extracting the following Chinese medicinal materials in parts by weight: 30-50 parts of abelmoschus manihot, 10-20 parts of rhodiola rosea and 1-10 parts of lemon. The anti-aging composition disclosed by the invention can be used as an active additive to be applied to cosmetics to prepare the cosmetics with anti-aging effect. Consumer use tests prove that the skin care product added with the anti-aging composition can improve the water content of skin, reduce the water loss of the skin, improve the elasticity of the skin, effectively remove facial wrinkles and fine lines and show good anti-aging effect.

Description

Abelmoschus manihot anti-aging composition and preparation method and application thereof
Technical Field
The invention relates to the field of cosmetics, and particularly relates to an abelmoschus manihot anti-aging composition and a preparation method and application thereof.
Background
The skin is the largest organ of the human body and ages with age. There are reports in the literature that women begin to wrinkle around 30 years of age, develop color spots, and subsequently become loose, rough, dull, and have deeper wrinkles, etc. Skin aging is almost accompanied by the second half of each person, which negatively affects the work and life of people, and thus how to delay aging is one of the research focuses on cosmetics.
For the above-mentioned anti-aging cosmetics, plant-derived anti-aging raw materials have been superior in skin irritation or safety and more acceptable to consumers than chemically synthesized anti-aging raw materials. In recent years, researchers find that some plants or Chinese herbal medicines contain antioxidant ingredients and have the effects of resisting free radicals, promoting skin metabolism and delaying body aging, but in practical application, the anti-wrinkle and anti-aging effects are not obvious. Therefore, it is necessary to research a brand-new pure natural skin care composition which has good crease-resistant anti-aging effect and good stability and is specially used for cosmetic addition.
Abelmoschus manihot (Hibiscus manihot L.) is an annual herbaceous plant of Abelmoschus genus of Malvaceae family, and is prepared from bark of Ulmus davidiana, Hibiscus manihot, Abelmoschus manihot or glutinous drynaria. The wild abelmoschus manihot is nearly endangered and dead, is discovered by a researchers in Tang Yixiong of Chinese academy of agricultural sciences in the North Prochensinensis area 8 months earlier than 2003, and is mostly planted in the market at present. Abelmoschus manihot recorded in Ben Cao gang mu has effects of clearing heat, cooling blood and removing toxic substance, and can be used for treating dyspepsia, anorexia, traumatic injury, etc. Modern pharmacological research proves that the Abelmoschus manihot has high medicinal value, has the strongest health-care medicinal function in more than 200 Abelmoschus plants, and has obvious effects of diminishing inflammation, easing pain, clearing away summer heat, reducing blood fat, resisting tumors, resisting oxidation, regulating immunity and the like.
The Abelmoschus manihot has rich active ingredients and extremely high content of bioflavonoids, and also comprises unsaturated fatty acid, volatile oil, organic acid, organic polysaccharide, alkaloid, protein, vitamin, polysaccharide gum, plant fiber and the like, and trace elements necessary for human bodies are also rich. Abelmoschus manihot has a good application prospect in the field of cosmetics, however, reports on the aspect are few.
Disclosure of Invention
In view of the above, the invention provides an anti-aging composition of abelmoschus manihot, wherein the effective components of the anti-aging composition are mainly extracted from abelmoschus manihot and other plants.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an anti-aging composition which is mainly prepared by extracting the following Chinese medicinal materials in parts by weight: 30-50 parts of abelmoschus manihot, 10-20 parts of rhodiola rosea and 1-10 parts of lemon.
In some embodiments of the invention, the anti-aging composition is mainly prepared by extracting the following Chinese medicinal materials in parts by weight: 40 parts of abelmoschus manihot, 15 parts of rhodiola rosea and 5 parts of lemon.
In some embodiments, the anti-aging composition can also be prepared by extracting the following traditional Chinese medicinal materials in parts by weight: 15 parts of ganoderma atrum, 7 parts of aloe and 5 parts of liquorice.
The invention relates to Abelmoschus manihot flower, which is flower of Abelmoschus manihot (L.) medic of Abelmoschus of Malvaceae, and has the effects of clearing heat, cooling blood and removing toxic substance.
The rhodiola rosea related by the invention is dry roots and rhizomes of rhodiola crenulata of Crassulaceae. Rhodiola root is sweet and bitter in taste, neutral in nature, and enters lung and heart meridians. Has the functions of benefiting qi, activating blood circulation, dredging meridian and relieving asthma.
The lemon related to the invention is the pericarp of a lemon of a citrus plant of rue family of dicotyledonous plants. Lemon peel is slightly bitter in taste and warm in nature, and recorded in Guangxi TCM J-Zhi (records of Guangxi TCM J-Zhi) it "moving qi, dispelling phlegm and invigorating stomach".
The ganoderma atrum cap is kidney-shaped, the upper surface of the ganoderma atrum cap is reddish brown, and the ganoderma atrum cap has cloud-shaped, annular patterns and lacquer-shaped luster. Is warm in nature and light in taste, is called as the best product in ganoderma lucidum, and has the medicinal effects of strengthening brain, diminishing inflammation, promoting urination, tonifying kidney and the like on the health care of human bodies.
The aloe related by the invention is aloe vera, is one of a few edible species in aloe, and the product is widely applied to the fields of food, beauty treatment, health care, medicine and the like. Aloe has been reported to have skin-astringing, softening, moisturizing, anti-inflammatory, and skin-caring effects.
The licorice root of the present invention is the dried root and rhizome of licorice of Leguminosae. Licorice root, radix Glycyrrhizae is sweet in flavor and neutral in nature. Enter heart, lung, spleen and stomach meridians. The functions are as follows: regulating the middle warmer, relieving urgency, moistening lung, removing toxic substance, and harmonizing the effects of the other drugs.
In some embodiments of the present invention, there is also provided a method for preparing the anti-aging composition, comprising the steps of:
(1) cutting lemon peel, transferring into a chromatographic column, packing the column, compacting, and eluting with ethanol water solution to obtain an eluent;
(2) adding water into the eluent to obtain a mixed solution;
(3) drying Abelmoschus manihot and radix Rhodiolae, pulverizing, adding appropriate amount of mixed solution, soaking, transferring into chromatography column, packing, compacting, and eluting with the mixed solution obtained in step (3) to obtain extractive solution;
(4) centrifuging the extractive solution, collecting supernatant, adding dipropylene glycol, mixing, and rotary evaporating to remove ethanol.
In some embodiments of the invention, the volume fraction of the aqueous ethanol solution of step (1) is from 90 to 95%; the flow rate of elution is 1-2BV/h, and the collection amount of the eluent is 1-2 BV.
In some embodiments of the invention, the volume fraction of ethanol in the mixture of step (2) is 60-80%.
In some embodiments of the invention, the soaking time in step (3) is 6 to 12 hours; the flow rate of elution is 1-2BV/h, and the collection amount of the eluent is 2-3 BV.
In some embodiments of the invention, dipropylene glycol is added in step (4) in an amount of 40-60% by weight of the supernatant.
In some embodiments of the present invention, ganoderma atrum, aloe and licorice are further added in step (3).
The anti-aging composition prepared by the embodiment of the invention can be used as an additive to be applied to cosmetics, and the cosmetics can be cream, emulsion, essence, facial mask and toner according to dosage forms.
The technical scheme provided by the embodiment of the invention has the following beneficial effects: the anti-aging composition provided by the embodiment of the invention can be used as an active additive to be applied to cosmetics to prepare the cosmetics with anti-aging effect. Consumer use tests prove that the skin care product added with the anti-aging composition can improve the water content of skin, reduce the water loss of the skin, improve the elasticity of the skin, effectively remove facial wrinkles and fine lines and show good anti-aging effect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art are briefly introduced below.
FIG. 1, change in water content of stratum corneum after 8 weeks of using anti-aging emulsion;
FIG. 2, change in TEWL values after 8 weeks of use of the anti-aging emulsion;
FIG. 3 is a graph of the change in skin elasticity after 8 weeks of use of the anti-aging lotion;
FIG. 4, change in skin wrinkle score after 8 weeks of using anti-aging lotion;
FIG. 5 comparison of change in eye wrinkles in volunteers using anti-aging lotion 8 weeks.
Detailed Description
The invention discloses an anti-aging Abelmoschus manihot composition, and a preparation method and application thereof, and can be realized by appropriately improving process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the art that the techniques of this invention can be modified and applied without departing from the spirit and scope of the invention by making changes or appropriate alterations and combinations to the methods and applications described herein.
The raw materials and reagents used in the anti-aging composition and the application formula provided by the invention can be purchased from the market.
The invention is further illustrated by the following examples:
example 1
A preparation method of an anti-aging composition comprises the following steps:
(1) cutting 1kg of lemon peel, transferring into a chromatographic column, filling the column, compacting, eluting with 90% ethanol water solution by volume fraction at the flow rate of 2BV/h to obtain 1BV eluent;
(2) adding water into the eluent to obtain a mixed solution with the volume fraction of ethanol being 80%;
(3) drying 50kg of Abelmoschus manihot and 10kg of rhodiola rosea, crushing, adding a proper amount of mixed solution, and soaking for 6 hours, wherein the liquid level is slightly higher than the materials; then transferring into a chromatographic column, filling the column, compacting, eluting with the mixed solution obtained in the step (3), and controlling the flow rate at 2BV/h to obtain 2BV extracting solution;
(4) centrifuging the extracting solution, collecting supernatant, and adding dipropylene glycol, wherein the addition amount of the dipropylene glycol is 40% of the weight of the supernatant; mixing, and rotary evaporating to remove ethanol.
Example 2
A preparation method of an anti-aging composition comprises the following steps:
(1) cutting 10kg of lemon peel, transferring into a chromatographic column, filling the column, compacting, eluting with 95% ethanol water solution by volume fraction at the flow rate of 1BV/h to obtain 2BV eluent;
(2) adding water into the eluent to obtain a mixed solution with the volume fraction of ethanol being 60%;
(3) drying 30kg of Abelmoschus manihot and 20kg of rhodiola rosea, crushing, adding a proper amount of mixed solution, and soaking for 12 hours, wherein the liquid level is slightly higher than the materials; then transferring into a chromatographic column, filling the column, compacting, eluting with the mixed solution obtained in the step (3), and controlling the flow rate at 1BV/h to obtain 3BV extracting solution;
(4) centrifuging the extracting solution, collecting supernatant, and adding dipropylene glycol, wherein the addition amount of dipropylene glycol is 60% of the weight of the supernatant; mixing, and rotary evaporating to remove ethanol.
Example 3
A preparation method of an anti-aging composition comprises the following steps:
(1) cutting 5kg of lemon peel, transferring into a chromatographic column, filling the column, compacting, eluting with 92% ethanol water solution by volume fraction at the flow rate of 1.5BV/h to obtain 1.5BV eluent;
(2) adding water into the eluent to obtain a mixed solution with the volume fraction of ethanol being 70%;
(3) drying 40kg of Abelmoschus manihot and 15kg of rhodiola rosea, crushing, adding a proper amount of mixed solution, and soaking for 8 hours, wherein the liquid level is slightly higher than the materials; then transferring into a chromatographic column, filling the column, compacting, eluting with the mixed solution obtained in the step (3), and controlling the flow rate at 1.5BV/h to obtain 2.5BV extracting solution;
(4) centrifuging the extracting solution, collecting supernatant, and adding dipropylene glycol, wherein the addition amount of dipropylene glycol is 50% of the weight of the supernatant; mixing, and rotary evaporating to remove ethanol.
Example 4
A preparation method of an anti-aging composition comprises the following steps:
(1) cutting 5kg of lemon peel, transferring into a chromatographic column, filling the column, compacting, eluting with 92% ethanol water solution by volume fraction at the flow rate of 1.5BV/h to obtain 1.5BV eluent;
(2) adding water into the eluent to obtain a mixed solution with the volume fraction of ethanol being 70%;
(3) drying Abelmoschus manihot 40kg, radix Rhodiolae 15kg, Ganoderma atrum 15kg, Aloe 7kg, and Glycyrrhrizae radix 5kg, pulverizing, adding appropriate amount of mixed solution, soaking for 8 hr, wherein the liquid level is slightly higher than the materials; then transferring into a chromatographic column, filling the column, compacting, eluting with the mixed solution obtained in the step (3), and controlling the flow rate at 1.5BV/h to obtain 2.5BV extracting solution;
(4) centrifuging the extracting solution, collecting supernatant, and adding dipropylene glycol, wherein the addition amount of dipropylene glycol is 50% of the weight of the supernatant; mixing, and rotary evaporating to remove ethanol.
Comparative example 1
A preparation method of an anti-aging composition comprises the following steps:
(1) drying 30kg of Abelmoschus manihot and 20kg of rhodiola rosea, crushing, adding a proper amount of mixed solution, and soaking for 12 hours, wherein the liquid level is slightly higher than the materials; then transferring into a chromatographic column, filling the column, compacting, eluting with 60% ethanol water solution by volume fraction, and controlling the flow rate at 1BV/h to obtain 3BV extracting solution;
(2) cutting 10kg of lemon peel, transferring into a chromatographic column, filling the column, compacting, eluting with 95% ethanol water solution by volume fraction at the flow rate of 1BV/h to obtain 2BV eluent;
(3) mixing the extracting solution obtained in the step (1) and the eluent obtained in the step (2), centrifuging, collecting supernate, and adding dipropylene glycol, wherein the addition amount of the dipropylene glycol is 60% of the weight of the supernate; mixing, and rotary evaporating to remove ethanol.
Comparative example 2
A preparation method of an anti-aging composition comprises the following steps:
(1) cutting 5kg of lemon peel, transferring into a chromatographic column, filling the column, compacting, eluting with 95% ethanol water solution by volume fraction at the flow rate of 1BV/h to obtain 2BV eluent;
(2) centrifuging the eluent, collecting supernatant, and adding dipropylene glycol, wherein the addition amount of the dipropylene glycol is 60% of the weight of the supernatant; mixing, and rotary evaporating to remove ethanol.
Comparative example 3
A preparation method of an anti-aging composition comprises the following steps:
(1) drying 40kg of Abelmoschus manihot, crushing, adding a proper amount of mixed solution, and soaking for 12 hours, wherein the liquid level is slightly higher than the materials; then transferring into a chromatographic column, filling the column, compacting, eluting with 60% ethanol water solution by volume fraction, and controlling the flow rate at 1BV/h to obtain 3BV extracting solution;
(2) centrifuging the extracting solution, collecting supernatant, and adding dipropylene glycol, wherein the addition amount of dipropylene glycol is 60% of the weight of the supernatant; mixing, and rotary evaporating to remove ethanol.
Comparative example 4
A preparation method of an anti-aging composition comprises the following steps:
(1) drying 15kg of rhodiola rosea, crushing, adding a proper amount of mixed solution, and soaking for 12 hours, wherein the liquid level is slightly higher than the materials; then transferring into a chromatographic column, filling the column, compacting, eluting with 60% ethanol water solution by volume fraction, and controlling the flow rate at 1BV/h to obtain 3BV extracting solution;
(2) centrifuging the extracting solution, collecting supernatant, and adding dipropylene glycol, wherein the addition amount of dipropylene glycol is 60% of the weight of the supernatant; mixing, and rotary evaporating to remove ethanol.
Test 1 measurement of Total Flavonoids content
The test principle is as follows: the flavone mother nucleus contains basic oxygen atom, generally has phenolic hydroxyl group, can generate yellow complex with aluminum ions, and is added with sodium nitrite and sodium hydroxide to make the solution be red in alkaline solution, the solution has maximum absorption at 510nm, and the color reaction is stable within 60 min. Rutin is used as a reference substance, aluminum nitrate is used as a color developing agent for colorimetric determination of flavonoids, the absorbance and the concentration of the rutin are in a linear relationship, and the content of the total flavonoids is determined by adopting a spectrophotometry.
Instruments and reagents: an ultraviolet-visible spectrophotometer; electronic balance (0.1 mg); 60% (V/V) ethanol solution; 5% sodium nitrite solution; 10% aluminum nitrate solution.
Preparing a rutin standard solution: 20.8mg of rutin is weighed, and the volume is determined to be 25ml volumetric flask by 60 percent ethanol to be used as standard solution.
And (3) preparing a standard curve: precisely measuring rutin standard solution 0.0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL and 6.0mL, respectively placing in 25mL volumetric flasks, adding water to 6mL, adding sodium nitrite solution 1mL, shaking, standing for 6min, adding aluminum nitrate solution 1mL, shaking, standing for 6min, adding sodium hydroxide solution 10mL, adding water to scale, shaking, standing for 15min, preparing blank liquid without adding aluminum nitrate solution according to the steps, adjusting to zero as blank, measuring absorbance at the wavelength of 510nm, drawing a standard curve by taking the absorbance as ordinate and the concentration as abscissa, and performing linear fitting to obtain a standard curve equation Y =100.02X-0.4165, wherein R is R2=0.9996。
Preparation of a sample: precisely measuring a proper amount of sample (V), placing the sample in a 25mL (V1) volumetric flask, and adding a 60% ethanol solution to fix the volume to the scale. Accurately sucking 5mL (V2) of the solution, placing the solution in another 25mL volumetric flask, adding 1mL of water, adding 1mL of sodium nitrite solution, shaking up, placing for 6min, adding 1mL of aluminum nitrate solution, shaking up, placing for 6min, adding 10mL of sodium hydroxide solution, adding water to the scale, shaking up, and placing for 15min to serve as a test solution. Meanwhile, a blank solution is prepared according to the steps without adding an aluminum nitrate solution and is used as a blank for zero adjustment.
Measurement of the sample: absorbing the test solution, measuring the absorbance at the wavelength of 510nm by taking the blank solution as a reference, and calculating the content (A) of the total flavonoids in the test solution according to the standard curve. And if the absorbance of the test solution exceeds the absorbance of the highest concentration of the standard curve, properly diluting the test solution and then measuring.
The content (X) of total flavonoids in the sample is calculated according to the following formula:
Figure DEST_PATH_IMAGE001
x-total flavone content in milligrams per 100 milliliters (mg/100 mL) of sample;
A-Total Flavonoids content in mg in the test solution calculated from the standard curve;
v-volume of sample measured in milliliters (mL);
v1 — volume of sample to volume in milliliters (mL);
v2 — volume of sample solution for the amount of test fluid prepared in milliliters (mL).
The anti-aging compositions prepared in examples 1 to 3 and comparative examples 1 to 4 were measured for the total flavone content, and the results are shown in table 1.
TABLE 1 Total Flavonoids content
Figure 890392DEST_PATH_IMAGE002
As can be seen from Table 1, the total flavone content of the antiaging compositions obtained in examples 1 to 3 was comparatively high. As can be seen from the comparison of example 2 with comparative examples 1-4, the process provided by the invention has higher total flavone content than that obtained by extraction in the conventional process.
Experiment 2 DPPH radical scavenging test
Antioxidant is any substance that is present at low concentrations to effectively inhibit the oxidation of free radicals, either by acting directly on the free radicals or by indirectly consuming substances that readily form free radicals, preventing further reactions from occurring. The current research methods for free radical scavengers mainly belong to 2 types, one type is an in vitro model, and the other type is an in vivo model, wherein the DPPH method is the most common method in the in vitro model.
DPPH is also called 1, 1-diphenyl-2-trinitrophenylhydrazine, is a very stable free radical with a nitrogen center, and the stability of DPPH mainly comes from the steric hindrance of 3 benzene rings with resonance stabilization effect, so that unpaired electrons on the nitrogen atom in the middle cannot play the role of electron pairing. Its absolute ethyl alcohol solution is purple, and has maximum absorption at wavelength of 517nm, and its absorbance and concentration are in linear relation. When a radical scavenger is added thereto, DPPH may be combined with or substituted for the radical scavenger, whereby the radical scavenging ability can be evaluated by decreasing the number of radicals, decreasing the absorbance, and decreasing the color of the solution. Namely, the antioxidant capacity was calculated by measuring the DPPH-removing effect of the sample at a wavelength of 517 nm.
According to the method described in the reference (Rong laughing nitrile, evaluation of antioxidant activity of turmeric extract based on DPPH free radical scavenging capacity [ J ]. drug evaluation research, 2011,34(05): 360-. Then, transferring 10mL of the composition to be detected into a centrifugal tube, centrifuging for 10 minutes at 9000 rpm/separation, discarding the supernatant, obtaining a precipitate, adding 10mL of acetone, and performing shake extraction for 30 minutes under a dark condition to obtain a sample to be detected; and respectively taking the samples to be detected after gradient dilution, and determining the DPPH free radical scavenging capacity of the composition to be detected by taking the IC50 value as an evaluation index of the DPPH radical scavenging capacity of the composition to be detected.
Diluting ascorbic acid standard substance with water to 0.03, 0.04, 0.05, 0.06, 0.08 mg/mL concentration gradient solutions, detecting their DPPH radical scavenging effect, calculating the DPPH radical scavenging rate (Y) of ascorbic acid, and performing linear fitting to obtain a standard curve equation Y =0.5257X +0.4659, R2=0.9956, yielding an IC50 value for ascorbic acid of 6.5mg/100 mL.
The anti-aging compositions obtained in examples 1 to 4 and comparative examples 1 to 4 were subjected to DPPH radical scavenging test, and the test results are shown in Table 2.
TABLE 2 IC50 values for each test group
Figure DEST_PATH_IMAGE003
As can be seen from Table 2, the anti-aging compositions prepared in examples 1 to 4 of the present invention have significantly higher antioxidant capacity than those prepared in comparative examples 1 to 4, and the antioxidant capacity of the anti-aging compositions prepared in example 4 is further improved by adding Ganoderma atrum, Aloe Vera, and Glycyrrhiza uralensis.
Experiment 3 human body patch test
The anti-aging compositions prepared in examples 1 to 4 of the present invention were subjected to a skin-closed patch test to evaluate potential adverse reactions of the products on human skin. The specific method is performed by referring to the method described in section 2 of the chapter seventh human body safety inspection method in technical Specification for cosmetic safety (2015 edition). The judgment criteria are shown in Table 3, and the test results are shown in Table 4.
Figure 558265DEST_PATH_IMAGE004
TABLE 4 test results of human skin occlusion patch
Figure DEST_PATH_IMAGE005
As can be seen from Table 4, the anti-aging composition prepared by the embodiment of the invention has no potential adverse reaction to human skin, and can be used as a raw material to be applied in cosmetics.
Example 5
The anti-aging toner comprises the following components in percentage by mass: 1% of dipropylene glycol, 2% of methyl propylene glycol, 1% of glycerol, 260.5% of glyceryl polyether, 0.5% of p-hydroxyacetophenone, 0.05% of allantoin, 0.1% of trehalose, 0.03% of hydroxyethyl cellulose, 0.02% of dipotassium glycyrrhizinate, 0.05% of xanthan gum, 0.5% of hexylene glycol, 160.3% of octyl dodecanol polyether, 0.1% of carbomer, 0.03% of tromethamine, 0.02% of sodium hyaluronate, 0.02% of SCLEROTIUM rolfsii (scleroticum rolfsii) glue, 1% of the anti-aging composition prepared in example 1 and the balance of water.
Example 6
An anti-aging emulsion comprises the following components in percentage by mass: 1% of phenyl trimethicone, 1% of polydimethylsiloxane, 3% of isononyl isononanoate, 0.5% of dimethiconol, 2% of cyclopentadimethylsiloxane, 0.5% of polydimethylsiloxane cross-linked polymer, 2% of dipropylene glycol, 5% of glycerol, 0.05% of sodium hyaluronate, 0.2% of panthenol, 0.05% of allantoin, 0.3% of acrylic acid/C10-30 alkanol acrylate cross-linked polymer, 0.5% of C20-22 alcohol phosphate, 0.5% of C20-22 alcohol, 0.15% of aminomethyl propanol, 0.03% of disodium EDTA, 0.1% of propyl hydroxybenzoate, 0.5% of phenoxyethanol, 0.05% of ethylhexyl glycerol, 0.2% of methyl hydroxybenzoate, 5% of the anti-aging composition prepared in example 2, and the balance of water.
Test 4 volunteer test
The anti-aging product obtained in example 6 was subjected to an anti-aging test for 8 weeks according to a method described in a reference (juliepin, grand crystal, plum a. ginseng anti-aging mask clinical efficacy test and analysis [ J ]. chinese cosmetic medicine, 2016,25(02): 33-36.).
30 healthy volunteers were selected. Inclusion criteria were: firstly, the male and the female are not limited, and the age is 30-65 years; certain facial/eye skin is loose or fine wrinkles are on the face/eyes; secondly, the body is healthy, the attitude is serious, the expression capability is realized, and the feeling after use can be truly reflected; voluntarily participates in the study, and signs and reads the informed consent, can strictly comply with the requirements of the study scheme, uses the product according to the requirements of the study scheme and completes follow-up visits. Exclusion criteria: women in gestation or lactation; ② sensitive skin; the skin of the face is damaged or the skin disease affecting the observation of the face state is suffered; the face has received skin treatment, beauty and other tests that may affect the outcome; sun burn or use of hormone drugs and immunosuppressant within about 1 month; sixthly, the patients who have participated in other facial clinical studies or received dermatologist treatment within the current or near 3 months. Termination and rejection criteria: firstly, a test subject requires to stop the test; the compliance of the testee is not good; thirdly, the test cannot be continued due to adverse reaction or special physiological and pathological changes and the like; and fourthly, in the test, other skin care products which have influence on the experiment are used, and the skin care products are excessively irradiated by ultraviolet rays.
And (3) long-acting test: after the volunteers clean the face every night, the anti-aging emulsion prepared in the example 6 is applied, and the face is not required to be cleaned and any other cosmetics are not required to be smeared after the face is massaged and absorbed for 8 weeks continuously; the follow-up visits were 1 each at 0, 2, 4, 6, 8 weeks before use, for a total of 5 times, with the subjects being asked to follow-up at the same time of day for each follow-up.
The instrument measurement method comprises the following steps: the test was carried out using a moisture tester Corneometer, a skin moisture loss tester, Tewameter, a skin elasticity tester MPA580 from CK, Germany, and a VISIA facial image analysis system from Canfield, USA. Specifically, the method comprises the following steps: measuring the water content of the stratum corneum of the skin (the water content of the skin): measuring the water content of the horny layer of the left cheek part and the right cheek part by using a water content tester, measuring for 4 times, and taking an average value; measurement of the percutaneous water loss (TEWL value) of facial skin: measuring the percutaneous water loss of the left face and the right face by using a skin water loss analyzer, and taking an average value after 2 times of measurement; measuring the elasticity of the facial skin: measuring the skin elasticity of the left eye tail, the right eye tail and the under eye by using a skin elasticity tester, and calculating the average value of R2, wherein R2= Ua/Uf; ua is the recovery value of the skin when negative pressure is added on the skin surface from the elimination of the negative pressure to the next continuous test; uf is the maximum skin stretch in the presence of negative pressure. Imaging the face: subjects' faces were photographed using the VISIA facial image analysis system (front, left and right 45 ° orientation). And extracting the wrinkle value and the texture value, and taking an average value.
Test results of water content of skin stratum corneum: as can be seen from figure 1, compared with week 0, the water content of the stratum corneum of the skin is gradually increased from week 2 of the product, and the anti-aging emulsion prepared by the invention shows good moisturizing effect.
TEWL value (in g/hm)2) The measurement results of (a): as can be seen from FIG. 2, the water loss through skin gradually decreases from week 2 of the product application, and the anti-aging emulsion prepared by the invention shows good water locking effect.
Test results of skin elasticity: as can be seen from FIG. 3, compared with week 0, the skin elasticity is significantly improved from week 4 of the product, and the anti-aging emulsion prepared by the invention shows good effect of improving the skin elasticity.
The result of the skin wrinkle score test shows that the facial wrinkle score of the volunteers is obviously and gradually reduced from the 4 th week of the product compared with the 0 week, which shows that the anti-aging emulsion prepared by the invention has strong efficacy of improving facial wrinkles and fine lines, and does not cause skin tolerance due to long-term use. In addition, as can be seen from fig. 5, the small fine lines in the crow's feet area of the volunteers were significantly improved after 8 weeks of using the product.
Therefore, the anti-aging emulsion prepared by the embodiment of the invention can improve the water content of the skin, reduce the water loss of the skin, improve the elasticity of the skin, effectively remove the facial wrinkles and fine lines and show good anti-aging effect after being used by a subject for a long time.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. An anti-aging composition is characterized by being mainly prepared by extracting the following Chinese medicinal materials in parts by weight: 30-50 parts of abelmoschus manihot, 10-20 parts of rhodiola rosea and 1-10 parts of lemon.
2. The anti-aging composition according to claim 1, wherein the anti-aging composition is mainly prepared by extracting the following Chinese medicinal materials in parts by weight: 40 parts of abelmoschus manihot, 15 parts of rhodiola rosea and 5 parts of lemon.
3. The anti-aging composition according to claim 1, further comprising the following extracts of Chinese herbs by weight: 15 parts of ganoderma atrum, 7 parts of aloe and 5 parts of liquorice.
4. Anti-ageing composition according to claim 1 or 2, characterized in that it is prepared by a process comprising the following steps:
(1) cutting lemon peel, transferring into a chromatographic column, packing the column, compacting, and eluting with ethanol water solution to obtain an eluent;
(2) adding water into the eluent to obtain a mixed solution;
(3) drying Abelmoschus manihot and radix Rhodiolae, pulverizing, adding appropriate amount of mixed solution, soaking, transferring into chromatography column, packing, compacting, and eluting with the mixed solution obtained in step (3) to obtain extractive solution;
(4) centrifuging the extractive solution, collecting supernatant, adding dipropylene glycol, mixing, and rotary evaporating to remove ethanol.
5. The method for preparing the antiaging composition according to claim 4, wherein the volume fraction of the ethanol aqueous solution in the step (1) is 90-95%; the flow rate of elution is 1-2BV/h, and the collection amount of the eluent is 1-2 BV.
6. The method for preparing the antiaging composition according to claim 4, wherein the volume fraction of ethanol in the mixed solution in the step (2) is 60-80%.
7. The method for preparing the antiaging composition according to claim 4, wherein the soaking time in the step (3) is 6 to 12 hours; the flow rate of elution is 1-2BV/h, and the collection amount of the eluent is 2-3 BV.
8. The method for preparing the antiaging composition according to claim 4, wherein the dipropylene glycol is added in the step (4) in an amount of 40 to 60% by weight based on the supernatant.
9. The method for preparing the antiaging composition according to claim 4, wherein Ganoderma atrum, Aloe vera, and Glycyrrhiza uralensis are further added in the step (3).
10. The anti-aging composition according to any one of claims 1 to 9, which is applied as an additive to cosmetics in the form of cream, milky lotion, essence, pack, toner.
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