CN116553563B - Purification method of siliceous sponge spicules and application of siliceous sponge spicules in transdermal repairing of acne skin - Google Patents
Purification method of siliceous sponge spicules and application of siliceous sponge spicules in transdermal repairing of acne skin Download PDFInfo
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- CN116553563B CN116553563B CN202310560808.4A CN202310560808A CN116553563B CN 116553563 B CN116553563 B CN 116553563B CN 202310560808 A CN202310560808 A CN 202310560808A CN 116553563 B CN116553563 B CN 116553563B
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000000746 purification Methods 0.000 title claims abstract description 14
- 208000002874 Acne Vulgaris Diseases 0.000 title abstract description 16
- 206010000496 acne Diseases 0.000 title abstract description 16
- 230000005484 gravity Effects 0.000 claims abstract description 66
- 238000001914 filtration Methods 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 24
- 239000006185 dispersion Substances 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000004381 surface treatment Methods 0.000 claims description 42
- 239000007788 liquid Substances 0.000 claims description 32
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 238000002791 soaking Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 10
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical compound O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 235000018936 Vitellaria paradoxa Nutrition 0.000 claims description 6
- 241001135917 Vitellaria paradoxa Species 0.000 claims description 6
- 229940059958 centella asiatica extract Drugs 0.000 claims description 6
- 229940057910 shea butter Drugs 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 19
- 238000004519 manufacturing process Methods 0.000 abstract description 5
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- 150000002632 lipids Chemical class 0.000 description 2
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- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 description 1
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- 206010067484 Adverse reaction Diseases 0.000 description 1
- 229930105110 Cyclosporin A Natural products 0.000 description 1
- PMATZTZNYRCHOR-CGLBZJNRSA-N Cyclosporin A Chemical compound CC[C@@H]1NC(=O)[C@H]([C@H](O)[C@H](C)C\C=C\C)N(C)C(=O)[C@H](C(C)C)N(C)C(=O)[C@H](CC(C)C)N(C)C(=O)[C@H](CC(C)C)N(C)C(=O)[C@@H](C)NC(=O)[C@H](C)NC(=O)[C@H](CC(C)C)N(C)C(=O)[C@H](C(C)C)NC(=O)[C@H](CC(C)C)N(C)C(=O)CN(C)C1=O PMATZTZNYRCHOR-CGLBZJNRSA-N 0.000 description 1
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- 229920002674 hyaluronan Polymers 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; Compounds thereof
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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
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
- A61P17/10—Anti-acne agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract
The invention belongs to the technical field of spongy spicule preparation, and particularly relates to a purification method of a siliceous spongy spicule and application of the siliceous spongy spicule in transdermal repairing of acne skin. Compared with the prior art, the method of the invention is that the siliceous sponge spicule is sequentially subjected to specific gravity filtration, dispersion filtration, polarity removal, drying and dehydration treatment to obtain the purified siliceous sponge spicule. The invention also provides application of the siliceous sponge spicule prepared by the purification method in transdermal treatment of acne. The method is simple and convenient to operate, the siliceous sponge spicule purified by the method has high purity, and can not adsorb new impurities in the production, transportation and use processes, thereby effectively improving the safety. Having a higher throughput efficiency and a more stable product quality.
Description
Technical Field
The invention belongs to the technical field of spongy spicule preparation, and particularly relates to a purification method of a siliceous spongy spicule and application of the siliceous spongy spicule in transdermal repairing of acne skin.
Background
In the field of medical cosmetology, skin has been the subject of human protection and beautification. The manufacturing process of microneedles is mature, but the choice of microneedle material is always a problem. The traditional roller metal microneedle has complex process, high cost, complex operation and slow repair, and is easy to cause skin to break and bleed in the using process.
Transdermal absorption in daily cosmetics means that functional ingredients in cosmetics act on the surface of the skin or enter the epidermis or dermis according to the effectiveness of the product. Unlike pharmaceuticals, transdermal absorption of cosmetic functional ingredients is a process that aims at accumulating in the affected skin layer and accumulates and acts at that site.
In the description of the transdermal delivery of hyaluronic acid and cyclosporin A, which is promoted by the synergistic effect of the spongy spicule and the liposome system, 850+/-125 micro-channels with the depth of 48.6+/-13.5 microns can be formed on the surface of skin per square millimeter after the spongy spicule is used for massaging the skin, and the micro-channels can exist for more than 72 hours continuously, can form a large number of channels on the surface of the skin and can not penetrate through macromolecular substances of normal skin, can enter the skin through the micro-channels, can be used in a large area, and can be very potential as a novel micro-needle for physical permeation promotion of skin administration.
However, in the existing sponge spicule production process, equipment investment is large, energy consumption is high, production operation is complex, potential safety hazards exist, and the prepared sponge spicule is incomplete and has low purity. Functional use is limited by percutaneous absorption and penetration promotion, no application scheme for effectively treating acne through skin is available, and the main stream of skin care products for treating acne in the market is to add components with oil control or antibacterial effects into the skin care products to achieve the aim of removing acnes. However, most components with oil control or antibacterial effects are easy to stimulate skin or destroy normal flora on the surface layer of skin, so that skin barrier is easy to damage, the moisturizing ability of skin is reduced, and the water-oil balance of skin is disturbed, so that acne is easy to repeat, and the absorption rate of effective active substances in the external skin care product is generally less than 10%.
Disclosure of Invention
The invention aims to provide a high-efficiency purification method and surface treatment of siliceous spongy spicules, and the spongy spicules prepared by the method are complete and high in purity.
A method for purifying siliceous sponge spicules comprises the following steps: and (3) specific gravity filtration, dispersion filtration, ultrasonic separation, cleaning and drying treatment to obtain the purified siliceous sponge spicule.
In particular, the specific gravity filtration is:
soaking original siliceous sponge spicules in specific gravity filtrate, dividing the soaked original siliceous sponge spicules into upper, middle and lower layers, and taking siliceous sponge spicules in the middle layer;
the concentration of the specific gravity filtrate is 10-40wt% of hydrogen peroxide water solution, and the soaking time is 0.5-12h.
In particular, the dispersion filtration is:
placing the siliceous sponge spicules after specific gravity filtration into a dispersion liquid, and dispersing the siliceous sponge spicules by stirring; the siliceous sponge spicules are divided into an upper layer, a middle layer and a lower layer, and the siliceous sponge spicules in the middle layer are taken;
the concentration of the dispersion liquid is 10-40wt% of hydrogen peroxide water solution, and the soaking time is 30-180min;
the stirring speed is more than or equal to 100rpm.
In particular, the ultrasonic separation is: drying the dispersed and filtered siliceous sponge spicules, placing the siliceous sponge spicules in a polar cleaning solution, performing ultrasonic treatment, drying again, and vibrating and sieving to obtain high-purity siliceous sponge spicules;
the polar cleaning liquid is acetone;
the number of the screen meshes of the vibration screen is 100-300 meshes.
In particular, the washing and drying are: and (3) washing with distilled water to remove residual polar washing liquid, and drying until the water content is lower than 0.01%.
The invention also discloses application of the siliceous sponge spicule in skin care products, and the specific skin care products are resident skin care products with the effect of treating acne.
The invention also provides a preparation method of the surface-treated siliceous sponge spicule, which comprises the following steps:
(1) Taking the siliceous sponge spicules prepared by the purification method;
(2) Mixing the shea butter with water, alcohol, acetone, centella asiatica extract to form a uniform surface treatment solution;
(3) The surface treatment solution is kept at a constant temperature of more than or equal to 35 ℃, and is put into siliceous sponge spicules and heated to an azeotropic point in a low-pressure environment;
(4) When the surface treatment solution is evaporated until the residual solution is less than or equal to 5%, vacuumizing, and removing the residual solution until the weight is constant; and fishing out the solid matters in the surface-treated siliceous sponge bone needles.
The surface treatment solvent is divided into a solvent and a solute;
the solute accounts for 10-15wt%; the ratio of the shea butter to the centella asiatica extract in the solute is 2-3:1;
in the solute, the volume ratio of water, alcohol and acetone is 10:40-70:20-50;
the addition amount of the siliceous sponge spicule is 0.1-10wt% of the surface treatment solvent;
the low-pressure environment in the step (3) is less than or equal to 0.05Mpa;
the air pressure of the vacuum in the step (4) is less than or equal to 100pa.
The invention also discloses application of the surface-treated siliceous sponge spicule in skin care products, wherein the specific skin care products are resident skin care products with the effect of treating acne.
Compared with the prior art, the method of the invention is that the siliceous sponge spicule is sequentially subjected to specific gravity filtration, dispersion filtration, polarity removal, drying and dehydration treatment to obtain the purified siliceous sponge spicule. The invention also provides application of the siliceous sponge spicule prepared by the purification method in transdermal treatment of acne. The method is simple and convenient to operate, the siliceous sponge spicule purified by the method has high purity, and can not adsorb new impurities in the production, transportation and use processes, thereby effectively improving the safety. Having a higher throughput efficiency and a more stable product quality.
Meanwhile, the invention also provides the siliceous sponge spicule after surface treatment, the shea butter and the centella asiatica extract are wrapped on the surface of the siliceous sponge spicule, and on the premise of excessively increasing the diameter of the siliceous sponge spicule, the microenvironment at the relevant position can be kept balanced on the basis of forming a micro-channel, and the shea butter can keep skin oil to prevent desiccation due to water loss; the centella asiatica extract can relieve skin adverse reaction caused by high active substance absorptivity; the application range and the effect of the siliceous sponge spicule are further improved.
Drawings
The invention will be further described with reference to the drawings and examples.
FIGS. 1-3 are experimental comparisons of various persons of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the present invention, but are merely illustrative of the present invention. The experimental methods used in the following examples are not specifically described, but the experimental methods in which specific conditions are not specified in the examples are generally carried out under conventional conditions, and the materials, reagents, etc. used in the following examples are commercially available unless otherwise specified.
In specific embodiments, steps, material selections, numerical parameters that are not described in detail are all routine selections in the art, or any prior art that is presently disclosed.
The original siliceous sponge spicules of the invention are from moss sponge or bee sponge.
EXAMPLE 1 purification of siliceous sponge spicules
The purification method of the siliceous sponge spicule with the serial number 1 comprises the following steps:
(1) Specific gravity filtration: placing original siliceous sponge spicules between a first specific gravity filter screen and a second specific gravity filter screen of a specific gravity filter device;
soaking with specific gravity filtrate to soften the original siliceous sponge spicule, separating out impurities therein, and positioning the impurities with larger specific gravity below the second specific gravity filter screen according to different specific gravity; the impurities with smaller specific gravity float upwards and are positioned above the first specific gravity filter screen, and after soaking, siliceous sponge spicules which are positioned between the first specific gravity filter screen and the second specific gravity filter screen and are used for softening specific gravity filtration are taken;
the specific gravity filtrate was a 10wt% aqueous hydrogen peroxide solution, and the soaking time was 12 hours.
(2) Dispersion filtration: adding dispersion liquid into the dispersion filter tank body;
placing siliceous sponge spicules after specific gravity filtration between a first dispersing filter screen and a second dispersing filter screen, and starting a stirrer;
the softened siliceous sponge spicules are crushed and dispersed, and impurities with larger specific gravity are downwards positioned below the second dispersing filter screen according to different specific gravities; the impurities with smaller specific gravity float upwards and are positioned above the first dispersing filter screen, the stirring and dispersing time is 3 hours, and after the dispersing is finished, siliceous sponge spicules positioned in the middle layer between the first dispersing filter screen and the second dispersing filter screen are taken;
the concentration of the dispersion is 10wt% of hydrogen peroxide water solution, and the soaking time is 180min;
the stirring speed was 100rpm.
(3) Ultrasonic separation: placing the dispersed and filtered siliceous sponge spicules in a vacuum oven at 40 ℃ for drying for 24 hours;
placing in an ultrasonic material stripper with acetone and a magnetic stirring rotor, starting the ultrasonic material stripper, washing with acetone to remove polar groups of siliceous sponge spicules, drying in a vacuum oven at 120deg.C for 4 hr, and sieving with a 100-300 mesh sieve to obtain high-purity siliceous sponge spicules.
(4) And (5) cleaning and drying: and (3) washing with distilled water to remove residual polar washing liquid, and drying until the water content is lower than 0.01%.
The purification method of the serial number 2 siliceous sponge spicule comprises the following steps:
(1) Specific gravity filtration: placing original siliceous sponge spicules between a first specific gravity filter screen and a second specific gravity filter screen of a specific gravity filter device;
soaking with specific gravity filtrate to soften the original siliceous sponge spicule, separating out impurities therein, and positioning the impurities with larger specific gravity below the second specific gravity filter screen according to different specific gravity; the impurities with smaller specific gravity float upwards and are positioned above the first specific gravity filter screen, and after soaking, siliceous sponge spicules which are positioned between the first specific gravity filter screen and the second specific gravity filter screen and are used for softening specific gravity filtration are taken;
the specific gravity filtrate was 40wt% aqueous hydrogen peroxide solution, and the soaking time was 0.5h.
(2) Dispersion filtration: adding dispersion liquid into the dispersion filter tank body;
placing siliceous sponge spicules after specific gravity filtration between a first dispersing filter screen and a second dispersing filter screen, and starting a stirrer;
the softened siliceous sponge spicules are crushed and dispersed, and impurities with larger specific gravity are downwards positioned below the second dispersing filter screen according to different specific gravities; the impurities with smaller specific gravity float upwards and are positioned above the first dispersing filter screen, the stirring and dispersing time is 3 hours, and after the dispersing is finished, siliceous sponge spicules positioned in the middle layer between the first dispersing filter screen and the second dispersing filter screen are taken;
the concentration of the dispersion is 40wt% of hydrogen peroxide water solution, and the soaking time is 30min;
the stirring speed was 100rpm.
(3) Ultrasonic separation: placing the dispersed and filtered siliceous sponge spicules in a vacuum oven at 40 ℃ for drying for 24 hours;
placing in an ultrasonic material stripper with acetone and a magnetic stirring rotor, starting the ultrasonic material stripper, washing with acetone to remove polar groups of siliceous sponge spicules, drying in a vacuum oven at 120deg.C for 4 hr, and sieving with a 100-300 mesh sieve to obtain high-purity siliceous sponge spicules.
(4) And (5) cleaning and drying: and (3) washing with distilled water to remove residual polar washing liquid, and drying until the water content is lower than 0.01%.
The purification method of the serial number 3 siliceous sponge spicule comprises the following steps:
(1) Specific gravity filtration: placing original siliceous sponge spicules between a first specific gravity filter screen and a second specific gravity filter screen of a specific gravity filter device;
soaking with specific gravity filtrate to soften the original siliceous sponge spicule, separating out impurities therein, and positioning the impurities with larger specific gravity below the second specific gravity filter screen according to different specific gravity; the impurities with smaller specific gravity float upwards and are positioned above the first specific gravity filter screen, and after soaking, siliceous sponge spicules which are positioned between the first specific gravity filter screen and the second specific gravity filter screen and are used for softening specific gravity filtration are taken;
the specific gravity filtrate was a 20wt% aqueous hydrogen peroxide solution, and the soaking time was 6 hours.
(2) Dispersion filtration: adding dispersion liquid into the dispersion filter tank body;
placing siliceous sponge spicules after specific gravity filtration between a first dispersing filter screen and a second dispersing filter screen, and starting a stirrer;
the softened siliceous sponge spicules are crushed and dispersed, and impurities with larger specific gravity are downwards positioned below the second dispersing filter screen according to different specific gravities; the impurities with smaller specific gravity float upwards and are positioned above the first dispersing filter screen, the stirring and dispersing time is 3 hours, and after the dispersing is finished, siliceous sponge spicules positioned in the middle layer between the first dispersing filter screen and the second dispersing filter screen are taken;
the concentration of the dispersion is 20wt% of hydrogen peroxide water solution, and the soaking time is 60min;
the stirring speed was 100rpm.
(3) Ultrasonic separation: placing the dispersed and filtered siliceous sponge spicules in a vacuum oven at 40 ℃ for drying for 24 hours;
placing in an ultrasonic material stripper with acetone and a magnetic stirring rotor, starting the ultrasonic material stripper, washing with acetone to remove polar groups of siliceous sponge spicules, drying in a vacuum oven at 120deg.C for 4 hr, and sieving with a 100-300 mesh sieve to obtain high-purity siliceous sponge spicules.
(4) And (5) cleaning and drying: and (3) washing with distilled water to remove residual polar washing liquid, and drying until the water content is lower than 0.01%.
EXAMPLE 2 surface treatment method of purified siliceous sponge spicules
The preparation method of the siliceous sponge spicule with the surface treatment of the serial number 4 comprises the following steps:
(1) Taking the siliceous sponge bone needle obtained in the sequence number 1 of the example 1;
(2) Preparing a surface treatment liquid, wherein the surface treatment liquid comprises the following components in percentage by mass
(3) Placing the surface treatment liquid in pressure reducing equipment, keeping the temperature to 35 ℃, and putting siliceous sponge spicules; starting the pressure reducing device and heating the surface treatment liquid to the azeotropic point; maintaining the temperature;
the adding amount of the siliceous sponge spicule is 0.1 weight percent of the surface treatment liquid;
at this time, the pressure was less than or equal to 0.05mpa.
(4) Stopping heating and vacuumizing until the air pressure is less than or equal to 100pa when the surface treatment liquid is evaporated to 5wt% of the rest; until the weight is constant; and fishing out the solid matters in the surface-treated siliceous sponge bone needles.
The preparation method of the siliceous sponge spicule with the surface treatment of the serial number 5 comprises the following steps:
(1) Taking the siliceous sponge bone needle obtained in the sequence number 2 of the example 1;
(2) Preparing a surface treatment liquid, wherein the surface treatment liquid comprises the following components in percentage by mass
(3) Placing the surface treatment liquid in pressure reducing equipment, keeping the temperature to 35 ℃, and putting siliceous sponge spicules; starting the pressure reducing device and heating the surface treatment liquid to the azeotropic point; maintaining the temperature;
the adding amount of the siliceous sponge spicule is 10wt% of the surface treatment liquid;
at this time, the pressure was less than or equal to 0.05mpa.
(4) Stopping heating and vacuumizing until the air pressure is less than or equal to 100pa when the surface treatment liquid is evaporated to 5wt% of the rest; until the weight is constant; and fishing out the solid matters in the surface-treated siliceous sponge bone needles.
The preparation method of the siliceous sponge spicule with the surface treatment of the serial number 6 comprises the following steps:
(1) Taking the siliceous sponge bone needle obtained in the sequence number 3 of the example 1;
(2) Preparing a surface treatment liquid, wherein the surface treatment liquid comprises the following components in percentage by mass
(3) Placing the surface treatment liquid in pressure reducing equipment, keeping the temperature to 35 ℃, and putting siliceous sponge spicules; starting the pressure reducing device and heating the surface treatment liquid to the azeotropic point; maintaining the temperature;
the adding amount of the siliceous sponge spicule is 8wt% of the surface treatment liquid;
at this time, the pressure was less than or equal to 0.05mpa.
(4) Stopping heating and vacuumizing until the air pressure is less than or equal to 100pa when the surface treatment liquid is evaporated to 5wt% of the rest; until the weight is constant; and fishing out the solid matters in the surface-treated siliceous sponge bone needles.
Example 3 Performance test
(1) Physical property test
Taking a smear of each group of siliceous sponge spicule samples, placing the smear under SEM for observation, selecting 3 areas for each group, counting the integrity, the length and the diameter of at least 100 siliceous sponge spicules in each area, and calculating an average value; simultaneously calculating the purity of the product; the results are shown in Table 1;
because the siliceous sponge spicule is similar to the middle expansion shape of the tips of the two ends of the sweater needle; a shape is considered incomplete if it is not under the microscope.
The purity is calculated by the number ratio of spongy spicules to debris in the counting area (including intact spongy spicules and broken spongy spicules)
TABLE 1 physical Property test of siliceous sponge spicules
In table 1, since the amount of the impurity chips is too small and the shape of a part of the impurity chips is too similar to that of the broken spongy bone needles to be distinguished, the precise purity cannot be determined. The surface-treated siliceous sponge spicules were not suitable for the standard of purity and no corresponding test was performed.
As can be seen from Table 1, the diameter of the siliceous sponge spicule increased by about 4 μm before and after the surface treatment; the length increases by about 8 μm; the increase of the diameter and the length of the siliceous sponge bone needle after surface treatment indicates that other substances are attached to the surface of the siliceous sponge bone needle. The integrity before and after the surface treatment was not significantly different, indicating that the surface treatment did not negatively affect the morphology of the siliceous sponge spicule.
(2) Human body test
Preparation of cream for use as shown in Table 2 below
TABLE 2 cream ingredients
The preparation method of the cream comprises the following steps:
1. weighing the phase A raw material into a main beaker, heating to 80-85 ℃, homogenizing and dissolving completely, stirring uniformly, and preserving heat for 20 minutes.
2. Weighing the phase B raw material into another beaker, heating to 80-85 ℃ and completely dissolving;
3. adding the B phase raw material into the A phase raw material, homogenizing and dissolving completely, stirring uniformly, and then starting to cool;
4. cooling to 40-45deg.C, adding C phase and D phase (pre-dissolved) materials, and stirring to dissolve.
Human body skin patch test
The prepared cream is referred to the human skin patch experiment in 2022 cosmetic safety technical Specification.
Skin reactions were observed as standard at 30min (after the indentation had disappeared), 24h and 48h, respectively, and observations were recorded.
The results show that the measurement results of 30 persons are 0 level in 30min, 24h and 48h, and no adverse reaction exists.
Oil control effect test
Test instrument: sebumeter SM815
Test conditions: constant temperature and humidity environment, temperature 23+ -1deg.C, humidity 50% + -5%, and subject was allowed to sit still for at least 30 minutes under the environment before testing.
80 subjects with oily skin, 40 men, 40 women were enrolled. The animals were randomly divided into 4 groups of 20 persons each.
Skin lipid content (μg/cm) on both sides of the nose of the subject was measured with a lipid tester Sebumeter SM815, respectively 2 ) Recorded as T0. After each subject cleaned the face, the samples were applied to the face (with emphasis on applying on both sides of the nose wings) once a day for 4 weeks, and the fourth week oil content was noted as T4. The test results are shown in table 3 below.
Wherein the blank group sample is deionized water;
the samples of comparative group 1 were the cream of table 2 without phase D;
table 2 cream with the sample of comparative group 2 being siliceous sponge microneedle with the D phase being sponge microneedle number 3;
the samples of the experimental group were the creams of table 2.
TABLE 3 comparison of grease conditions
As can be seen from the comparison of the group 1 and the blank group in the table 3, the cream has a certain oil control effect; meanwhile, the oil control effect can be greatly improved by adding the siliceous sponge microneedle, and the oil control effect is further improved by adding the siliceous sponge microneedle with surface treatment than by not carrying out surface treatment. Meaning that the siliceous sponge microneedle has good penetration promoting effect, and the surface treatment can further strengthen the penetration promoting effect.
Independent human body test results
3 acne muscle patients were selected for independent testing.
Test instrument: visa facial skin detector
Test period: the cream of Table 2 was used for a period of 2 weeks
The testing method comprises the following steps: after each subject cleans the face, the sample is smeared on the face (the two sides of the nose wing are smeared on the focus) once a day; and other cleaning products and skin care products are stopped.
User 1: the results of the potential (mild) acne muscle tester are shown in figure 1.
User 2: the results for the (moderate) acne muscle tester are shown in figure 2.
User 3: (severe) acne muscle tester, the results are shown in fig. 3.
It can be seen from figures 1-3 that the present invention provides a significant improvement over the acne muscles, whether they are light, medium, or heavy.
The foregoing detailed description is directed to one of the possible embodiments of the present invention, which is not intended to limit the scope of the invention, but is to be accorded the full scope of all such equivalents and modifications so as not to depart from the scope of the invention.
Claims (2)
1. The preparation method of the surface-treated siliceous sponge spicule is characterized by comprising the following steps:
(1) Taking siliceous sponge spicules for purification;
(2) Mixing the shea butter with water, alcohol, acetone, centella asiatica extract to form a uniform surface treatment solution;
(3) The surface treatment solution is kept at a constant temperature of more than or equal to 35 ℃, and is put into siliceous sponge spicules and heated to an azeotropic point in a low-pressure environment;
(4) When the surface treatment solution is evaporated until the residual solution is less than or equal to 5%, vacuumizing, and removing the residual solution until the weight is constant; taking out the solid matters to obtain the siliceous sponge spicules with surface treatment;
the surface treatment solvent is divided into a solvent and a solute;
the solute accounts for 10-15wt%; the ratio of the shea butter to the centella asiatica extract in the solute is 2-3:1;
in the solute, the volume ratio of water, alcohol and acetone is 10:40-70:20-50;
the addition amount of the siliceous sponge spicule is 0.1-10wt% of the surface treatment solvent;
the purification method of the siliceous sponge spicule in the step (1) comprises the following steps: specific gravity filtration, dispersion filtration, ultrasonic separation, cleaning and drying treatment to obtain purified siliceous sponge spicules;
the specific gravity filtration is as follows:
soaking original siliceous sponge spicules in specific gravity filtrate, dividing the soaked original siliceous sponge spicules into upper, middle and lower layers, and taking siliceous sponge spicules in the middle layer; the concentration of the specific gravity filtrate is 10-40wt% of hydrogen peroxide water solution, and the soaking time is 0.5-12h;
the dispersion filtration is as follows: placing the siliceous sponge spicules after specific gravity filtration into a dispersion liquid, and dispersing the siliceous sponge spicules by stirring; the siliceous sponge spicules are divided into an upper layer, a middle layer and a lower layer, and the siliceous sponge spicules in the middle layer are taken; the concentration of the dispersion liquid is 10-40wt% of hydrogen peroxide water solution, and the soaking time is 30-180min; the stirring rotating speed is more than or equal to 100rpm;
the ultrasonic separation is as follows: drying the dispersed and filtered siliceous sponge spicules, placing the siliceous sponge spicules in a polar cleaning solution, performing ultrasonic treatment, drying again, and vibrating and sieving to obtain high-purity siliceous sponge spicules; the polar cleaning liquid is acetone; the number of the screen meshes of the vibration screen is 100-300 meshes;
the cleaning and drying steps are as follows: washing with distilled water to remove residual polar cleaning liquid, and drying until the water content is lower than 0.01%;
in the step (3):
the low-pressure environment is less than or equal to 0.05Mpa;
in the step (4):
the air pressure of the vacuum is less than or equal to 100pa.
2. Use of the surface-treated siliceous sponge spicules prepared according to claim 1 in skin care products.
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| CN105999535A (en) * | 2016-04-27 | 2016-10-12 | 厦门大学 | Application of sponge spicule as skin physical penetration enhancer |
| CN107213095A (en) * | 2017-06-29 | 2017-09-29 | 芜湖凌梦电子商务有限公司 | A kind of net acne maintenance breast of oil-control |
| CN108163861A (en) * | 2018-02-09 | 2018-06-15 | 四川理工学院 | The purification process and purification system of a kind of Silica Sponge Spicule and application |
| CN109820812A (en) * | 2019-03-06 | 2019-05-31 | 成都柯思茉科技有限公司 | The preparation method of high-purity sponge spicule and its application as enhancer of cutaneous penetration |
| CN113908108A (en) * | 2021-10-10 | 2022-01-11 | 广州吉腾生物科技有限公司 | Sponge spicule for quickly repairing skin and preparation method and application thereof |
| CN115557508A (en) * | 2022-09-23 | 2023-01-03 | 杭州释光检测技术有限公司 | Method for purifying siliceous spongy spicules in marine sediments |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105999535A (en) * | 2016-04-27 | 2016-10-12 | 厦门大学 | Application of sponge spicule as skin physical penetration enhancer |
| CN107213095A (en) * | 2017-06-29 | 2017-09-29 | 芜湖凌梦电子商务有限公司 | A kind of net acne maintenance breast of oil-control |
| CN108163861A (en) * | 2018-02-09 | 2018-06-15 | 四川理工学院 | The purification process and purification system of a kind of Silica Sponge Spicule and application |
| CN109820812A (en) * | 2019-03-06 | 2019-05-31 | 成都柯思茉科技有限公司 | The preparation method of high-purity sponge spicule and its application as enhancer of cutaneous penetration |
| CN113908108A (en) * | 2021-10-10 | 2022-01-11 | 广州吉腾生物科技有限公司 | Sponge spicule for quickly repairing skin and preparation method and application thereof |
| CN115557508A (en) * | 2022-09-23 | 2023-01-03 | 杭州释光检测技术有限公司 | Method for purifying siliceous spongy spicules in marine sediments |
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