CN113398032A - Snow chrysanthemum hydrogel with whitening and freckle removing effects - Google Patents

Snow chrysanthemum hydrogel with whitening and freckle removing effects Download PDF

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CN113398032A
CN113398032A CN202110791242.7A CN202110791242A CN113398032A CN 113398032 A CN113398032 A CN 113398032A CN 202110791242 A CN202110791242 A CN 202110791242A CN 113398032 A CN113398032 A CN 113398032A
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hydrogel
coreopsis tinctoria
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CN113398032B (en
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陈新梅
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Shandong University of Traditional Chinese Medicine
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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
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    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
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Abstract

The invention belongs to the technical field of coreopsis tinctoria application, and provides coreopsis tinctoria hydrogel with whitening and freckle removing effects. Comprises the following components in parts by weight: 5-20 parts of coreopsis tinctoria extract, 9400.5-1.5 parts of carbomer, 0.1-0.5 part of sodium benzoate, 5-15 parts of peppermint oil, 5-15 parts of humectant and 2-10 parts of pH regulator. The cedarwood hydrogel with whitening and freckle removing effects provided by the invention has the advantages of smooth surface, no sediment and foam, fine and uniform gel, moderate viscosity, easiness in coating, high spreading speed, easiness in cleaning, stable quality and obvious whitening and freckle removing effects.

Description

Snow chrysanthemum hydrogel with whitening and freckle removing effects
Technical Field
The invention relates to the technical field of coreopsis tinctoria application, and particularly relates to coreopsis tinctoria hydrogel with whitening and freckle removing effects.
Background
Coreopsis tinctoria Nutt, which is named as coreopsis tinctoria Nutt, the medicine application part is a capitate inflorescence, is mainly distributed in Xinjiang areas in China, and is rich in various components such as flavonoids, coumarin, organic acids, amino acids, saponins, volatile oils, tannin, saccharides and phenols, wherein the content of the flavonoids is highest, the coreopsis tinctoria flower tea has the effects of resisting oxidation, resisting inflammation, inhibiting bacteria, reducing blood pressure, reducing blood sugar, enhancing immunity and the like, has high medicinal value, and is often used as scented tea in Xinjiang. In particular, the antioxidant effect of the coreopsis tinctoria is more than 10 times of that of vitamin E, and the coreopsis tinctoria can prevent cell aging and canceration. The flavonoid compound can be used as natural antioxidant, has effects of scavenging active oxygen, antagonizing oxidative stress injury, and regulating cell signal transduction pathway, and can be used for preventing and treating pigmented dermatosis and other related dermatosis caused by oxidative injury.
Earlier researches show that the crude extract of the snow chrysanthemum flavone can clear DPPH free radicals, inhibit spontaneous lipid peroxidation, has a certain reducing capacity, can improve the SOD activity of brain tissues, reduce the MDA content and inhibit oxidative stress, has good antioxidation effect, and can be used for whitening, spot fading and acne removal. However, the development of coreopsis tinctoria products is less at present, and the existing products have the problems of unstable quality and unsatisfactory whitening and freckle removing effects.
Disclosure of Invention
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a coreopsis tinctoria hydrogel with whitening and freckle removing effects, which comprises the following components in parts by weight: 5-20 parts of coreopsis tinctoria extract, 9400.5-1.5 parts of carbomer, 0.1-0.5 part of sodium benzoate, 5-15 parts of peppermint oil, 5-15 parts of humectant and 2-10 parts of pH regulator.
Preferably, the humectant is one or more of glycerol, polyethylene glycol and sorbitol.
Preferably, the pH regulator is one or more of sodium hydroxide, triethanolamine and ethylenediamine.
Preferably, the preparation method of the coreopsis tinctoria extract comprises the following steps: extracting coreopsis tinctoria flower in water for 1-2 times by refluxing for 10-20 min each time, extracting in 70-80% ethanol solution for 2-3 times by refluxing for 25-35 min each time, combining the extracting solutions, and performing suction filtration and rotary evaporation to obtain a concentrated solution.
Preferably, the mass volume ratio of the coreopsis tinctoria to water is 1g: 40-60 ml, and the mass volume ratio of the coreopsis tinctoria to a 70-80% ethanol solution is 1g: 30-40 ml.
Preferably, the reflux extraction temperature of the coreopsis tinctoria in water is 70-80 ℃, and the reflux extraction temperature of the coreopsis tinctoria in a 70-80% ethanol solution is 40-50 ℃.
Preferably, the ratio of the concentrated solution to the coreopsis tinctoria raw material is 1mL: 1.0-1.2 g.
The cedarwood hydrogel with whitening and freckle removing effects provided by the invention has the advantages of smooth surface, no sediment and foam, fine and uniform gel, moderate viscosity, easiness in coating, high spreading speed, easiness in cleaning, stable quality and obvious whitening and freckle removing effects.
Detailed Description
The invention provides a coreopsis tinctoria hydrogel with whitening and freckle removing effects, which comprises the following components in parts by weight: 5-20 parts of coreopsis tinctoria extract, 9400.5-1.5 parts of carbomer, 0.1-0.5 part of sodium benzoate, 5-15 parts of peppermint oil, 5-15 parts of humectant and 2-10 parts of pH regulator.
In the present invention, the following components are preferably included in parts by weight: the coreopsis tinctoria extract is preferably 5-20 parts, more preferably 8-15 parts, and even more preferably 10 parts; the preferable part of the carbomer 940 is 0.5-1.5 parts, the further preferable part is 0.8-1.2 parts, and the further preferable part is 1 part; the preferable part of the sodium benzoate is 0.1-0.5 part, the more preferable part is 0.2-0.4 part, and the more preferable part is 0.3 part; the mint oil is preferably 5-15 parts, more preferably 7-12 parts, and even more preferably 10 parts; the humectant is preferably 5-15 parts, more preferably 7-12 parts, and even more preferably 10 parts; the pH regulator is preferably 2 to 10 parts, more preferably 3 to 8 parts, and still more preferably 5 parts.
In the present invention, the humectant is preferably one or more of glycerin, polyethylene glycol and sorbitol, and is more preferably sorbitol.
In the present invention, the pH adjuster is preferably one or more of sodium hydroxide, triethanolamine, and ethylenediamine, and is more preferably sodium hydroxide.
In the invention, the preparation method of the coreopsis tinctoria extract comprises the following steps: extracting coreopsis tinctoria flower in water for 1-2 times by refluxing for 10-20 min each time, extracting in 70-80% ethanol solution for 2-3 times by refluxing for 25-35 min each time, combining the extracting solutions, and performing suction filtration and rotary evaporation to obtain a concentrated solution.
In the invention, the mass-to-volume ratio of the coreopsis tinctoria to water is preferably 1g: 40-60 ml, more preferably 1g: 45-55 ml, and still more preferably 1g:50 ml.
In the invention, the reflux extraction temperature of the coreopsis tinctoria in water is preferably 70-80 ℃, and further preferably 80 ℃; the extraction time is preferably 10-20 min, and more preferably 15 min; the number of extraction is preferably 1 to 2, and more preferably 2.
In the invention, the mass-to-volume ratio of the coreopsis tinctoria to the 70-80% ethanol solution is preferably 1g: 30-40 ml, and more preferably 1g:35 ml.
In the invention, the reflux extraction temperature of the coreopsis tinctoria in a 70-80% ethanol solution is preferably 40-50 ℃, and further preferably 45 ℃; the time for extraction is preferably 25 to 35min, more preferably 30min, and the number of extraction is preferably 2 to 3, more preferably 3.
In the present invention, the concentration of the ethanol solution is preferably 70 to 80%, and more preferably 75%.
In the invention, the ratio of the concentrated solution to the coreopsis tinctoria raw material is preferably 1mL: 1.0-1.2 g, and more preferably 1mL:1.2 g.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a coreopsis tinctoria hydrogel with whitening and freckle removing effects, which comprises the following components, by weight, 10 parts of coreopsis tinctoria extract, 9401 parts of carbomer, 0.3 part of sodium benzoate, 10 parts of peppermint oil, 10 parts of sorbitol and 5 parts of sodium hydroxide, and all the raw materials are mixed according to the parts by weight to obtain the coreopsis tinctoria hydrogel.
The coreopsis tinctoria extract of this example was prepared as follows: reflux extraction was carried out using 1g: adding 50ml of coreopsis tinctoria into water, heating to 80 ℃, extracting under reflux at 80 ℃ for 15min for 2 times, filtering, and collecting water extract and filter residue; then, according to the weight ratio of 1g of coreopsis tinctoria and 75% ethanol solution: adding 75% ethanol solution into filter residue, heating to 45 ℃, performing reflux extraction at 45 ℃ for 30min for 3 times, collecting ethanol extract, combining with water extract, performing suction filtration and rotary evaporation, and removing water and ethanol to obtain concentrated solution, wherein the ratio of the concentrated solution to the coreopsis tinctoria is 1ml:1.2 g.
Example 2
The embodiment provides a snow chrysanthemum hydrogel with whitening and freckle removing effects, which comprises the following components, by weight, 20 parts of a snow chrysanthemum extract, 9401.5 parts of carbomer, 0.1 part of sodium benzoate, 5 parts of peppermint oil, 15 parts of glycerol and 10 parts of ethylenediamine, and all the raw materials are mixed according to the parts by weight to obtain the snow chrysanthemum hydrogel.
The coreopsis tinctoria extract of this example was prepared as follows: reflux extraction was carried out using 1g: adding coreopsis tinctoria into water at a mass volume ratio of 40ml, heating to 70 ℃, extracting under reflux at 70 ℃ for 20min for 2 times, filtering, and collecting water extract and filter residue; then, according to the weight ratio of 1g of coreopsis tinctoria and 70% ethanol solution: adding 70% ethanol solution into filter residue, heating to 40 ℃, performing reflux extraction at 40 ℃ for 25min for 2 times, collecting ethanol extract, combining with water extract, performing suction filtration and rotary evaporation, and removing water and ethanol to obtain concentrated solution, wherein the ratio of the concentrated solution to the coreopsis tinctoria is 1ml:1.0 g.
Example 3
The embodiment provides a snow chrysanthemum hydrogel with whitening and freckle removing effects, which comprises the following components in parts by weight, 5 parts of a snow chrysanthemum extract, 9400.5 parts of carbomer, 0.5 part of sodium benzoate, 15 parts of peppermint oil, 5 parts of polyethylene glycol and 2 parts of triethanolamine, and all the raw materials are mixed according to the parts by weight to obtain the snow chrysanthemum hydrogel.
The coreopsis tinctoria extract of this example was prepared as follows: reflux extraction was carried out using 1g: adding coreopsis tinctoria into water at a mass volume ratio of 60ml, heating to 75 ℃, extracting under reflux at 75 ℃ for 10min for 1 time, filtering, and collecting water extract and filter residue; then, according to the weight ratio of 1g of coreopsis tinctoria and 80% ethanol solution: adding 80% ethanol solution into filter residue according to the mass ratio of 40ml, heating to 50 ℃, performing reflux extraction at 50 ℃ for 35min, extracting for 3 times, collecting ethanol extract, combining with water extract, performing suction filtration and rotary evaporation, and removing water and ethanol to obtain concentrated solution, wherein the ratio of the obtained concentrated solution to the coreopsis tinctoria flower is 1ml: 1.1 g.
Comparative example 1
This comparative example provides a sherry hydrogel, which is different from example 1 in that 15 parts by weight of Hydroxypropylmethylcellulose (HPMC) was used instead of 1 part by weight of carbomer 940 in example 1.
Comparative example 2
This comparative example provides a coreopsis tinctoria hydrogel, which differs from example 1 in that 5 parts by weight of sodium carboxymethylcellulose (CMC-Na) is used in place of 1 part by weight of carbomer 940 of example 1.
Comparative example 3
This comparative example provides a coreopsis tinctoria hydrogel, which is different from example 1 in that the peppermint oil in example 1 is replaced with a mixed absorption enhancer of propylene glycol and azone, wherein the mixing mass ratio of propylene glycol and azone is 1: 1.
Comparative example 4
The comparative example provides a coreopsis tinctoria hydrogel, which is different from example 1 in that the extraction method of the coreopsis tinctoria extract is different, and the extraction method of the coreopsis tinctoria extract in the comparative example is as follows: reflux extraction was carried out, according to 1g: adding coreopsis tinctoria into 60% ethanol at a mass-volume ratio of 67ml, heating to 80 ℃, performing reflux extraction at 80 ℃ for 21min, extracting for 3 times, combining filtrates, performing suction filtration, and performing rotary evaporation to obtain a concentrated solution, wherein the ratio of the concentrated solution to the coreopsis tinctoria is 1ml: 1.3 g.
(1) Sensory evaluation and stability test were performed on the snow chrysanthemum hydrogels prepared in examples 1 to 2 and comparative examples 1 to 2 by the following methods:
TABLE 1 sensory evaluation index and score
Figure BDA0003161026590000051
TABLE 2 sensory evaluation results
Figure BDA0003161026590000052
Figure BDA0003161026590000061
From the sensory evaluation results (table 2), the coreopsis tinctoria hydrogel prepared by the method has the advantages of smooth surface, no precipitation and foam, fine and uniform gel, moderate viscosity, easiness in coating, high spreading speed, easiness in cleaning, higher sensory score and better quality.
And (4) checking the stability: (1) heat resistance test: placing the prepared gel in a 55 ℃ water bath kettle at constant temperature for 2h, taking out, and observing whether the gel is layered or not and color change after the room temperature is recovered; (2) cold resistance test: placing the gel in a refrigerator at-20 deg.C for 72h, and observing whether the gel has delamination phenomenon and color change after recovering room temperature; (3) and (3) centrifugal test: placing the gel in a centrifuge, centrifuging at 3000r/min for 30min, taking out, and observing whether the gel has delamination phenomenon and color change. The above test results were evaluated according to the stability rating table of table 3.
TABLE 3 stability scoring Table
Figure BDA0003161026590000062
Table 4 stability test results
Figure BDA0003161026590000063
From the stability inspection results (table 4), it can be seen that the coreopsis tinctoria hydrogel prepared by the invention has good heat resistance, cold resistance, and centrifugal resistance, and good stability.
(2) Particle size inspection method: a suitable amount of the sample was placed on a slide glass and coated with a thin layer having an area equivalent to that of the cover glass, and 3 sheets were coated in total and measured by a particle size and particle size distribution measurement method (first method of general rule 0982). As a result: neither example 1 nor example 2 detected particles larger than 180 um.
(3) And (3) detecting microorganisms: reference to non-sterile product microbial limit check: microorganism count method (general rule 1105), control bacteria inspection method (general rule 1106) and non-sterile drug microorganism limit standard (general rule 1107). As a result: the microbiological indicators of example 1 and example 2 meet the regulations.
(4) Determination of the influence of the snow Chrysanthemum hydrogel on tyrosinase activity and melanin synthesis in mouse B16 melanocytes
1. Material
Mouse B16 melanoma cell line; DMEM medium; (ii) trypsin; L-DOPA.
Arbutin (98%), purchased externally, and diluted to 2mg/mL with deionized water, labeled as arbutin group;
the coreopsis tinctoria hydrogel of example 1;
the coreopsis tinctoria hydrogel of example 2;
the coreopsis tinctoria hydrogel of comparative example 3;
the coreopsis tinctoria hydrogel of comparative example 4;
microplate reader, BIO-RAD USA.
2. Method of producing a composite material
2.1 mouse B16 melanocyte cultures: under aseptic conditions, 1 × 105Mouse B16 melanocytes per mL were inoculated in a DMEM medium flask containing 10% (volume parts) calf serum at 37 deg.C with 5% CO2The cells were cultured in an incubator and were digested with 0.25% trypsin every 3 days for subculture.
2.2 intracellular tyrosinase Activity determination
After the cells had grown to log phase, they were digested with 0.25% pancreatin and adjusted to 2X 10 cells4one/mL, seeded in 96-well plates at 100. mu.L per well. After culturing in an incubator for 24h, the supernatant was discarded, the samples to be tested were added, 8 replicates of each sample to be tested were added, and the control group replaced the samples to be tested with the same amount of maintenance solution. Incubate for 3 days. After 3 days, the supernatant was discarded and washed twice with PBS pH6.8, and 90. mu.L of PBS containing 1% Triton X-100 was added to each well. Sonicate in ice bath, add 10. mu.L of 10mM L-DOPA to each well, incubate at 37 ℃ for 60min, measure absorbance values at 490nm for each well.
Inhibition rate (1-average absorbance value of sample group to be measured/average absorbance value of control group) × 100%.
2.3 determination of the intracellular Melanin content
B16 melanocytes at 1 × 105one/mL of the density was seeded in 6-well plates. 3mL of the cells in each well are incubated for 24h, the supernatant is discarded, the sample to be tested is added, after the reaction for 3d, the supernatant is discarded, the cells are washed by PBS, 0.5mL of pancreatin digestive cells are added into each well for 3min, 2mL of maintenance solution is added to stop the digestion, and each group of cells is counted respectively. Centrifuging the cell suspension, removing the supernatant, adding 1mol/L NaOH solution into the precipitate, and heating at 80 deg.C for 30 min. The absorbance at 475nm was measured by a spectrophotometer.
Melanin synthesis inhibition rate ═ 1- (sample well absorbance value/sample well cell number)/(control well absorbance value/control well cell number) ] × 100%
3. Results
TABLE 5 Effect on tyrosinase activity and melanin synthesis in mouse B16 melanocytes
Set of samples to be tested Tyrosinase inhibitor (%) Melanin synthesis inhibition (%)
Example 1 87.5 80.1
Example 2 85.6 81.5
Comparative example 3 75.2 74.5
Comparative example 4 72.5 70.9
Arbutin group 80.5 79.8
As can be seen from table 5. The snow chrysanthemum hydrogels of examples 1 and 2 have significant inhibitory effects on both cell tyrosinase activity and melanin synthesis and exceed the effects of arbutin, while comparative examples 3 and 4 have less inhibitory effects on cell tyrosinase activity and melanin synthesis than examples 1 and 2. The results show that the coreopsis tinctoria hydrogel provided by the invention has good whitening and freckle removing effects.
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 (7)

1. A coreopsis tinctoria hydrogel with whitening and freckle removing effects is characterized by comprising the following components in parts by weight: 5-20 parts of coreopsis tinctoria extract, 9400.5-1.5 parts of carbomer, 0.1-0.5 part of sodium benzoate, 5-15 parts of peppermint oil, 5-15 parts of humectant and 2-10 parts of pH regulator.
2. The snow chrysanthemum hydrogel with whitening and freckle removing effects according to claim 1, wherein the humectant is one or more of glycerol, polyethylene glycol and sorbitol.
3. The snow chrysanthemum hydrogel with whitening and freckle removing effects as claimed in claim 1 or 2, wherein the pH regulator is one or more of sodium hydroxide, triethanolamine and ethylenediamine.
4. The coreopsis tinctoria hydrogel with whitening and freckle removing effects of claim 1, wherein the preparation method of the coreopsis tinctoria extract comprises the following steps: extracting coreopsis tinctoria flower in water for 1-2 times by refluxing for 10-20 min each time, extracting in 70-80% ethanol solution for 2-3 times by refluxing for 25-35 min each time, combining the extracting solutions, and performing suction filtration and rotary evaporation to obtain a concentrated solution.
5. The snow chrysanthemum hydrogel with whitening and freckle removing effects according to claim 4, wherein the mass volume ratio of the snow chrysanthemum to water is 1g: 40-60 ml, and the mass volume ratio of the snow chrysanthemum to a 70-80% ethanol solution is 1g: 30-40 ml.
6. The snow chrysanthemum hydrogel with whitening and freckle removing effects as claimed in claim 4 or 5, wherein the temperature for reflux extraction of snow chrysanthemum in water is 70-80 ℃, and the temperature for reflux extraction of snow chrysanthemum in 70-80% ethanol solution is 40-50 ℃.
7. The coreopsis tinctoria hydrogel with whitening and freckle removing effects of claim 4, wherein the ratio of the concentrated solution to the coreopsis tinctoria raw material is 1mL: 1.0-1.2 g.
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