CN115869228B - Nanometer slow-release microcapsule and preparation method thereof - Google Patents
Nanometer slow-release microcapsule and preparation method thereof Download PDFInfo
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 229920001661 Chitosan Polymers 0.000 claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000003607 modifier Substances 0.000 claims abstract description 57
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical class [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 47
- 239000011248 coating agent Substances 0.000 claims abstract description 33
- 238000000576 coating method Methods 0.000 claims abstract description 33
- 239000008367 deionised water Substances 0.000 claims abstract description 32
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 32
- 125000005456 glyceride group Chemical group 0.000 claims abstract description 25
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims abstract description 25
- 241000723346 Cinnamomum camphora Species 0.000 claims abstract description 20
- SXYIRMFQILZOAM-HVNFFKDJSA-N dihydroartemisinin methyl ether Chemical compound C1C[C@H]2[C@H](C)CC[C@H]3[C@@H](C)[C@@H](OC)O[C@H]4[C@]32OO[C@@]1(C)O4 SXYIRMFQILZOAM-HVNFFKDJSA-N 0.000 claims abstract description 20
- 238000005516 engineering process Methods 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 235000002789 Panax ginseng Nutrition 0.000 claims abstract description 13
- 239000001506 calcium phosphate Substances 0.000 claims description 39
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 39
- 229940078499 tricalcium phosphate Drugs 0.000 claims description 39
- 229910000391 tricalcium phosphate Inorganic materials 0.000 claims description 39
- 235000019731 tricalcium phosphate Nutrition 0.000 claims description 39
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 34
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 27
- 238000005406 washing Methods 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 239000007822 coupling agent Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 21
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- 239000000654 additive Substances 0.000 claims description 14
- 230000000996 additive effect Effects 0.000 claims description 14
- 239000000839 emulsion Substances 0.000 claims description 14
- 235000010413 sodium alginate Nutrition 0.000 claims description 14
- 239000000661 sodium alginate Substances 0.000 claims description 14
- 229940005550 sodium alginate Drugs 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 10
- 238000010008 shearing Methods 0.000 claims description 10
- 241000208340 Araliaceae Species 0.000 claims description 7
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims description 7
- 235000003140 Panax quinquefolius Nutrition 0.000 claims description 7
- 229920002305 Schizophyllan Polymers 0.000 claims description 7
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 235000008434 ginseng Nutrition 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- WDQLRUYAYXDIFW-RWKIJVEZSA-N (2r,3r,4s,5r,6r)-4-[(2s,3r,4s,5r,6r)-3,5-dihydroxy-4-[(2r,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-6-[[(2r,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxymethyl]oxan-2-yl]oxy-6-(hydroxymethyl)oxane-2,3,5-triol Chemical compound O[C@@H]1[C@@H](CO)O[C@@H](O)[C@H](O)[C@H]1O[C@H]1[C@H](O)[C@@H](O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)[C@H](O)[C@@H](CO[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)O1 WDQLRUYAYXDIFW-RWKIJVEZSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 238000013268 sustained release Methods 0.000 claims 1
- 239000012730 sustained-release form Substances 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 230000000844 anti-bacterial effect Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000002453 shampoo Substances 0.000 description 6
- 239000004519 grease Substances 0.000 description 5
- 229920001282 polysaccharide Polymers 0.000 description 4
- 239000005017 polysaccharide Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 210000004761 scalp Anatomy 0.000 description 4
- -1 schizophyllan polysaccharide Chemical class 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000032798 delamination Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 208000001840 Dandruff Diseases 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 239000003205 fragrance Substances 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 210000002374 sebum Anatomy 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- Cosmetics (AREA)
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Abstract
The invention relates to the technical field of slow-release microcapsules, and in particular discloses a nano slow-release microcapsule which comprises the following raw materials in parts by weight: 10-20 parts of red ginseng extract, 10-15 parts of camphor tree leaf extract, 5-10 parts of narrow She Qinghao leaf/stem extract, 4-8 parts of chitosan coating modifier, 1-3 parts of nano modified hydroxyapatite, 15-25 parts of caprylic/capric glyceride and 20-30 parts of deionized water. The nanometer slow-release microcapsule adopts red ginseng extract, camphor tree leaf extract and angustifolia She Qinghao leaf/stem extract as main raw materials, the three raw materials are mutually matched, and the chitosan coating modifier and the nanometer modified hydroxyapatite are added to mutually coordinate and synergize, so that the microcapsule prepared by a critical preparation technology can slowly release, the sudden release condition of a product is easily changed, the thermal stability of the product is high, and the treatment efficiency is excellent.
Description
Technical Field
The invention relates to the technical field of slow-release microcapsules, in particular to a nano slow-release microcapsule and a preparation method thereof.
Background
The shampoo is one of the commonly used washing and caring products in the life of people, and has the characteristics of moistening, fine foam, lasting fragrance and the like. The original shampoo only meets the requirements of people on hair cleaning, but with the improvement of living standard, people slowly require the hair to be smooth and straight after washing, remove dandruff and the like, and in order to improve the use effect of the shampoo, components are added into the shampoo to improve the functionality of the shampoo; and the scalp treatment capability can be enhanced by combining shampoo with a slow release technology.
The existing slow-release microcapsule has poor effects on scalp grease cleaning and bacteriostasis treatment, is easy to cause sudden release, has poor thermal stability and low treatment efficiency, and is further improved based on the invention.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a nanometer slow-release microcapsule and a preparation method thereof, so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a nanometer slow-release microcapsule which comprises the following raw materials in parts by weight:
10-20 parts of red ginseng extract, 10-15 parts of camphor tree leaf extract, 5-10 parts of narrow She Qinghao leaf/stem extract, 4-8 parts of chitosan coating modifier, 1-3 parts of nano modified hydroxyapatite, 15-25 parts of caprylic/capric glyceride and 20-30 parts of deionized water.
Preferably, the nanometer slow-release microcapsule comprises the following raw materials in parts by weight:
15 parts of red ginseng extract, 12.5 parts of camphor tree leaf extract, 7.5 parts of narrow She Qinghao leaf/stem extract, 6 parts of chitosan coating modifier, 2 parts of nano modified hydroxyapatite, 20 parts of caprylic/capric glyceride and 25 parts of deionized water.
Preferably, the preparation method of the chitosan coating modifier comprises the following steps:
s01: adding nano tricalcium phosphate into deionized water with the weight being 2-5 times that of the nano tricalcium phosphate, then adding hydrochloric acid, then adding sodium dodecyl sulfate accounting for 5-10% of the total weight of the nano tricalcium phosphate, stirring fully, washing with water, and drying to obtain a nano tricalcium phosphate modifier;
s02: adding chitosan into 4-6 times of sodium alginate solution, adding nano tricalcium phosphate modifier accounting for 5-10% of the total chitosan and citric acid accounting for 1-5% of the total chitosan, and continuously stirring uniformly to obtain the chitosan coating modifier.
Preferably, the mass fraction of the sodium alginate solution is 10-20%.
Preferably, the hydrochloric acid adjusts the pH to 5.0.
Preferably, the preparation method of the nano modified hydroxyapatite comprises the following steps:
firstly, delivering nano-hydroxyapatite into deionized water with the volume being 3-5 times that of the nano-hydroxyapatite, then adding a coupling agent with the volume being 5-10% of that of the nano-hydroxyapatite and sodium hydroxide with the volume being 1-5% of that of the nano-hydroxyapatite, uniformly stirring, finally adding schizophyllan with the volume being 1-2% of that of the nano-hydroxyapatite, continuously stirring and fully mixing, and finally washing and drying to obtain the nano-modified hydroxyapatite.
Preferably, the coupling agent is coupling agent KH560.
Preferably, the particle size of the nano hydroxyapatite is 10-20nm.
The invention also provides a preparation method of the nanometer slow-release microcapsule, which comprises the following steps:
firstly, stirring and mixing a chitosan coated modifier and nano modified hydroxyapatite to obtain an additive;
step two: adding Ginseng radix Rubri extract, camphor tree leaf extract and She Qinghao leaf/stem extract into deionized water to form water phase;
step three: heating the oil phase of the caprylic/capric glyceride to 50-70 ℃, then adding the caprylic/capric glyceride into the water phase in the third step, then adding the additive, shearing and homogenizing at a rotating speed of 1000-1500r/min, and shearing and homogenizing for 25-35min to obtain a premix;
step four: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
Preferably, the critical preparation technology is that the premixed emulsion is injected into a carbon dioxide fluid reaction kettle, and is treated for 30-60min under the conditions of the temperature of 310-330K, the pressure of 10-12MPa and the CO flow rate to obtain a suspension; the flow rate of CO is 0.4-0.7L/min, and finally the water washing and drying are carried out.
Compared with the prior art, the invention has the following beneficial effects:
the nanometer slow-release microcapsule adopts red ginseng extract, camphor tree leaf extract and angustifolia She Qinghao leaf/stem extract as main raw materials, the three raw materials are mutually matched, and the chitosan coating modifier and the nanometer modified hydroxyapatite are added to mutually coordinate and synergize, so that the microcapsule prepared by a critical preparation technology can slowly release, the sudden release condition of a product is easily changed, the thermal stability of the product is high, and the treatment efficiency is excellent.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The nano slow-release microcapsule comprises the following raw materials in parts by weight:
10-20 parts of red ginseng extract, 10-15 parts of camphor tree leaf extract, 5-10 parts of narrow She Qinghao leaf/stem extract, 4-8 parts of chitosan coating modifier, 1-3 parts of nano modified hydroxyapatite, 15-25 parts of caprylic/capric glyceride and 20-30 parts of deionized water.
The nano slow-release microcapsule of the embodiment comprises the following raw materials in parts by weight:
15 parts of red ginseng extract, 12.5 parts of camphor tree leaf extract, 7.5 parts of narrow She Qinghao leaf/stem extract, 6 parts of chitosan coating modifier, 2 parts of nano modified hydroxyapatite, 20 parts of caprylic/capric glyceride and 25 parts of deionized water.
The preparation method of the chitosan coating modifier comprises the following steps:
s01: adding nano tricalcium phosphate into deionized water with the weight being 2-5 times that of the nano tricalcium phosphate, then adding hydrochloric acid, then adding sodium dodecyl sulfate accounting for 5-10% of the total weight of the nano tricalcium phosphate, stirring fully, washing with water, and drying to obtain a nano tricalcium phosphate modifier;
s02: adding chitosan into 4-6 times of sodium alginate solution, adding nano tricalcium phosphate modifier accounting for 5-10% of the total chitosan and citric acid accounting for 1-5% of the total chitosan, and continuously stirring uniformly to obtain the chitosan coating modifier.
The mass fraction of the sodium alginate solution in the embodiment is 10-20%.
The hydrochloric acid of this example adjusts the pH to 5.0.
The preparation method of the nano modified hydroxyapatite of the embodiment comprises the following steps:
firstly, delivering nano-hydroxyapatite into deionized water with the volume being 3-5 times that of the nano-hydroxyapatite, then adding a coupling agent with the volume being 5-10% of that of the nano-hydroxyapatite and sodium hydroxide with the volume being 1-5% of that of the nano-hydroxyapatite, uniformly stirring, finally adding schizophyllan with the volume being 1-2% of that of the nano-hydroxyapatite, continuously stirring and fully mixing, and finally washing and drying to obtain the nano-modified hydroxyapatite.
The coupling agent of this example is coupling agent KH560.
The particle size of the nano hydroxyapatite of the embodiment is 10-20nm.
The preparation method of the nanometer slow-release microcapsule comprises the following steps:
firstly, stirring and mixing a chitosan coated modifier and nano modified hydroxyapatite to obtain an additive;
step two: adding Ginseng radix Rubri extract, camphor tree leaf extract and She Qinghao leaf/stem extract into deionized water to form water phase;
step three: heating the oil phase of the caprylic/capric glyceride to 50-70 ℃, then adding the caprylic/capric glyceride into the water phase in the third step, then adding the additive, shearing and homogenizing at a rotating speed of 1000-1500r/min, and shearing and homogenizing for 25-35min to obtain a premix;
step four: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
The critical preparation technology of the embodiment is that the premixed emulsion is injected into a carbon dioxide fluid reaction kettle, and is treated for 30-60min under the conditions of the temperature of 310-330K, the pressure of 10-12MPa and the CO flow rate, so as to obtain a suspension; the flow rate of CO is 0.4-0.7L/min, and finally the water washing and drying are carried out.
Example 1.
The nano slow-release microcapsule comprises the following raw materials in parts by weight:
10 parts of red ginseng extract, 10 parts of camphor tree leaf extract, 5 parts of narrow She Qinghao leaf/stem extract, 4 parts of chitosan coating modifier, 1 part of nano modified hydroxyapatite, 15 parts of caprylic/capric glyceride and 20 parts of deionized water.
The preparation method of the chitosan coating modifier comprises the following steps:
s01: adding nano tricalcium phosphate into deionized water with the weight being 2 times that of the nano tricalcium phosphate, then adding hydrochloric acid, then adding sodium dodecyl sulfate accounting for 5% of the total weight of the nano tricalcium phosphate, stirring fully, washing with water, and drying to obtain a nano tricalcium phosphate modifier;
s02: adding chitosan into 4 times of sodium alginate solution, adding nano tricalcium phosphate modifier accounting for 5% of the total chitosan and citric acid accounting for 1% of the total chitosan, and continuously stirring uniformly to obtain the chitosan coating modifier.
The mass fraction of the sodium alginate solution of this example was 10%.
The hydrochloric acid of this example adjusts the pH to 5.0.
The preparation method of the nano modified hydroxyapatite of the embodiment comprises the following steps:
the nano-hydroxyapatite is firstly sent into deionized water with the volume being 3 times that of the nano-hydroxyapatite, then the coupling agent with the volume being 5 percent of the total volume of the nano-hydroxyapatite and the sodium hydroxide with the volume being 1 percent are added, the mixture is stirred uniformly, finally the schizophyllan polysaccharide with the volume being 1 percent is added, the mixture is stirred continuously and fully, and finally the nano-modified hydroxyapatite is obtained after washing and drying.
The coupling agent of this example is coupling agent KH560.
The particle size of the nano hydroxyapatite of this example was 10nm.
The preparation method of the nanometer slow-release microcapsule comprises the following steps:
firstly, stirring and mixing a chitosan coated modifier and nano modified hydroxyapatite to obtain an additive;
step two: adding Ginseng radix Rubri extract, camphor tree leaf extract and She Qinghao leaf/stem extract into deionized water to form water phase;
step three: heating the oil phase of the caprylic/capric glyceride to 50 ℃, then adding the caprylic/capric glyceride into the water phase in the third step, then adding an additive, shearing and homogenizing for 25-35min at a rotating speed of 1000r/min, so as to obtain a premix;
step four: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
The critical preparation technology of the embodiment is that the premixed emulsion is injected into a carbon dioxide fluid reaction kettle, and is treated for 30min under the conditions of the temperature of 310K, the pressure of 10MPa and the CO flow rate to obtain a suspension; the CO flow rate is 0.4L/min, and finally the water washing and drying are carried out.
Example 2.
The nano slow-release microcapsule comprises the following raw materials in parts by weight:
20 parts of red ginseng extract, 15 parts of camphor tree leaf extract, 10 parts of narrow She Qinghao leaf/stem extract, 8 parts of chitosan coating modifier, 3 parts of nano modified hydroxyapatite, 25 parts of caprylic/capric glyceride and 30 parts of deionized water.
The preparation method of the chitosan coating modifier comprises the following steps:
s01: adding nano tricalcium phosphate into deionized water with the weight being 5 times that of the nano tricalcium phosphate, then adding hydrochloric acid, then adding sodium dodecyl sulfate accounting for 10% of the total weight of the nano tricalcium phosphate, stirring fully, washing with water, and drying to obtain a nano tricalcium phosphate modifier;
s02: adding chitosan into 6 times of sodium alginate solution, adding 10% of nano tricalcium phosphate modifier and 5% of citric acid into the total chitosan, and continuously stirring uniformly to obtain the chitosan coating modifier.
The mass fraction of the sodium alginate solution of this example was 20%.
The hydrochloric acid of this example adjusts the pH to 5.0.
The preparation method of the nano modified hydroxyapatite of the embodiment comprises the following steps:
firstly, the nano-hydroxyapatite is sent into deionized water with the weight being 5 times that of the nano-hydroxyapatite, then, a coupling agent with the weight being 10 percent of that of the nano-hydroxyapatite and sodium hydroxide with the weight being 5 percent are added, the mixture is stirred uniformly, finally, 2 percent of schizophyllan polysaccharide is added, the mixture is stirred continuously and fully, and finally, the nano-modified hydroxyapatite is obtained after washing and drying.
The coupling agent of this example is coupling agent KH560.
The particle size of the nano hydroxyapatite of the embodiment is 20nm.
The preparation method of the nanometer slow-release microcapsule comprises the following steps:
firstly, stirring and mixing a chitosan coated modifier and nano modified hydroxyapatite to obtain an additive;
step two: adding Ginseng radix Rubri extract, camphor tree leaf extract and She Qinghao leaf/stem extract into deionized water to form water phase;
step three: heating the oil phase of the caprylic/capric glyceride to 70 ℃, then adding the caprylic/capric glyceride into the water phase in the third step, then adding an additive, shearing and homogenizing for 25-35min at a rotating speed of 1500r/min, so as to obtain a premix;
step four: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
The critical preparation technology of the embodiment is that the premixed emulsion is injected into a carbon dioxide fluid reaction kettle, and is treated for 60min under the conditions of the temperature of 330K, the pressure of 12MPa and the CO flow rate to obtain a suspension; the CO flow rate is 0.7L/min, and finally the water washing and drying are carried out.
Example 3.
The nano slow-release microcapsule comprises the following raw materials in parts by weight:
15 parts of red ginseng extract, 12.5 parts of camphor tree leaf extract, 7.5 parts of narrow She Qinghao leaf/stem extract, 6 parts of chitosan coating modifier, 2 parts of nano modified hydroxyapatite, 20 parts of caprylic/capric glyceride and 25 parts of deionized water.
The preparation method of the chitosan coating modifier comprises the following steps:
s01: adding nano tricalcium phosphate into deionized water with the volume being 3.5 times that of the nano tricalcium phosphate, then adding hydrochloric acid, then adding sodium dodecyl sulfate with the volume being 7.5 percent of the total volume of the nano tricalcium phosphate, stirring fully, washing with water, and drying to obtain a nano tricalcium phosphate modifier;
s02: adding chitosan into 5 times of sodium alginate solution, adding nano tricalcium phosphate modifier accounting for 7.5 percent of the total chitosan and citric acid accounting for 3 percent of the total chitosan, and continuously and uniformly stirring to obtain the chitosan coating modifier.
The mass fraction of the sodium alginate solution of this example was 15%.
The hydrochloric acid of this example adjusts the pH to 5.0.
The preparation method of the nano modified hydroxyapatite of the embodiment comprises the following steps:
the nano-hydroxyapatite is firstly sent into deionized water with the weight being 4 times that of the nano-hydroxyapatite, then the coupling agent with the weight being 7.5 percent of the total weight of the nano-hydroxyapatite and the sodium hydroxide with the weight being 3 percent are added, the mixture is stirred uniformly, finally the schizophyllan polysaccharide with the weight being 1.5 percent is added, the mixture is stirred continuously and fully, and finally the nano-modified hydroxyapatite is obtained after washing and drying.
The coupling agent of this example is coupling agent KH560.
The particle size of the nano hydroxyapatite of the embodiment is 15nm.
The preparation method of the nanometer slow-release microcapsule comprises the following steps:
firstly, stirring and mixing a chitosan coated modifier and nano modified hydroxyapatite to obtain an additive;
step two: adding Ginseng radix Rubri extract, camphor tree leaf extract and She Qinghao leaf/stem extract into deionized water to form water phase;
step three: heating the oil phase of the caprylic/capric glyceride to 60 ℃, then adding the caprylic/capric glyceride into the water phase in the third step, then adding an additive, shearing and homogenizing for 30min at a rotating speed of 1250r/min, so as to obtain a premix;
step four: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
The critical preparation technology of the embodiment is that the premixed emulsion is injected into a carbon dioxide fluid reaction kettle, and is treated for 45min under the conditions of the temperature of 320K, the pressure of 11MPa and the CO flow rate to obtain a suspension; the CO flow rate is 0.55L/min, and finally the water washing and drying are carried out.
Example 4.
The nano slow-release microcapsule comprises the following raw materials in parts by weight:
12 parts of red ginseng extract, 12 parts of camphor tree leaf extract, 6 parts of narrow She Qinghao leaf/stem extract, 5 parts of chitosan coating modifier, 2 parts of nano modified hydroxyapatite, 18 parts of caprylic/capric glyceride and 22 parts of deionized water.
The preparation method of the chitosan coating modifier comprises the following steps:
s01: adding nano tricalcium phosphate into deionized water with the volume being 3 times that of the nano tricalcium phosphate, then adding hydrochloric acid, then adding sodium dodecyl sulfate accounting for 6% of the total volume of the nano tricalcium phosphate, stirring fully, washing with water, and drying to obtain a nano tricalcium phosphate modifier;
s02: adding chitosan into 5 times of sodium alginate solution, adding nano tricalcium phosphate modifier accounting for 6% of the total chitosan and 2% of citric acid, and continuously stirring uniformly to obtain the chitosan coating modifier.
The mass fraction of the sodium alginate solution in this example was 12%.
The hydrochloric acid of this example adjusts the pH to 5.0.
The preparation method of the nano modified hydroxyapatite of the embodiment comprises the following steps:
the nano-hydroxyapatite is firstly sent into deionized water with the weight being 4 times that of the nano-hydroxyapatite, then the coupling agent with the weight being 6 percent and the sodium hydroxide with the weight being 2 percent are added, the mixture is stirred uniformly, finally the schizophyllan polysaccharide with the weight being 1.2 percent is added, the mixture is stirred continuously and fully, and finally the nano-modified hydroxyapatite is obtained after washing and drying.
The coupling agent of this example is coupling agent KH560.
The particle size of the nano hydroxyapatite of the embodiment is 12nm.
The preparation method of the nanometer slow-release microcapsule is characterized by comprising the following steps of:
firstly, stirring and mixing a chitosan coated modifier and nano modified hydroxyapatite to obtain an additive;
step two: adding Ginseng radix Rubri extract, camphor tree leaf extract and She Qinghao leaf/stem extract into deionized water to form water phase;
step three: heating the oil phase of the caprylic/capric glyceride to 55 ℃, then adding the caprylic/capric glyceride into the water phase in the third step, then adding an additive, shearing and homogenizing for 27min at a rotating speed of 1200r/min, and obtaining a premix;
step four: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
The critical preparation technology of the embodiment is that the premixed emulsion is injected into a carbon dioxide fluid reaction kettle, and is treated for 40min under the conditions of temperature 315K, pressure 11MPa and CO flow rate to obtain suspension; the CO flow rate is 0.5L/min, and finally the water washing and drying are carried out.
Comparative example 1.
The difference from example 3 is that no chitosan coating modifier was added.
Comparative example 2.
The difference from example 3 is that the chitosan coating modifier is replaced with chitosan.
Comparative example 3.
The difference from example 3 is that no nano tricalcium phosphate modifier is added in the preparation of the chitosan coating modifier.
Comparative example 4.
The difference from example 3 is that the nano tricalcium phosphate modifier is replaced by nano tricalcium phosphate.
Comparative example 5.
The difference from example 3 is that no nano-modified hydroxyapatite was added.
Comparative example 6.
The difference from example 3 is that nano-modified hydroxyapatite is replaced with hydroxyapatite.
The results of the performance measurements of examples 1-4 and comparative examples 1-6 are as follows
From examples 1 to 4 and comparative examples 1 to 6, the product of example 3 has excellent antibacterial property and antibacterial stability effect;
as can be seen from comparative examples 1 to 4, the antibacterial effect of the product is obviously reduced after 28 days in 14 days in which the chitosan coating modifier is not added, the antibacterial performance is obviously reduced, the nano tricalcium phosphate modifier is not added, the antibacterial performance is prone to be poor, the nano modified hydroxyapatite is not added, the antibacterial burst phenomenon of the product is obvious, and only the chitosan coating modifier prepared by the method provided by the invention is matched with the nano modified hydroxyapatite, the performance coordination effect of the product is enhanced, and the product is slow-release and excellent in antibacterial efficiency.
The tester uses a grease tester Sebumeter SM815 to test the grease content of the scalp respectively, records data as D0, washes hair once a day by adopting the product for 60 days, tests the grease content of the skin on 14 th day, 28 th day and 60 th day respectively, and records the data;
rate of change in oil content = { (oil content after use of product-oil content before use of product)/oil content before use of product } ×100%
The product performance tests of examples 1-4 are as follows:
the raw materials of the product can complement and strengthen the product to treat scalp grease, and the raw materials are synergistic together to remarkably inhibit sebum.
Stability evaluation:
high temperature stability (45+ -1) deg.C, treatment time of three months; the low temperature stability is-5 to-10 ℃, the treatment time is one week, the high temperature and the low temperature are alternated, and the treatment time is one month; after the test is finished, the temperature is restored to room temperature to observe smell, color, existence of precipitation and delamination and the like.
Judgment standard:
stable-smell, no change in color, no precipitation, and uniform semipermeable effect.
Unstable-smell, color change, precipitation or precipitation, delamination of the solution, and any appearance.
Centrifugal stability: 3000rpm,30min, and the presence or absence of delamination was examined.
The results are shown in the following Table
From the above results, it can be seen that examples 1, 2, 3 and 4 have good stability without any abnormality in the centrifugation test at high temperature and low temperature.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. If other components are adopted for replacement, the chitosan coating modifier and the nano modified hydroxyapatite have quite even poor effects, and are within the protection scope of the invention.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (8)
1. The nanometer slow-release microcapsule is characterized by comprising the following raw materials in parts by weight:
10-20 parts of red ginseng extract, 10-15 parts of camphor tree leaf extract, 5-10 parts of narrow She Qinghao leaf/stem extract, 4-8 parts of chitosan coating modifier, 1-3 parts of nano modified hydroxyapatite, 15-25 parts of caprylic/capric glyceride and 20-30 parts of deionized water;
the preparation method of the chitosan coating modifier comprises the following steps:
s01: adding nano tricalcium phosphate into deionized water with the weight being 2-5 times that of the nano tricalcium phosphate, then adding hydrochloric acid, then adding sodium dodecyl sulfate accounting for 5-10% of the total weight of the nano tricalcium phosphate, stirring fully, washing with water, and drying to obtain a nano tricalcium phosphate modifier;
s02: adding chitosan into a sodium alginate solution with the weight being 4-6 times that of the chitosan, then adding a nano tricalcium phosphate modifier with the weight being 5-10% of the total weight of the chitosan and citric acid with the weight being 1-5% of the total weight of the chitosan, and continuously and uniformly stirring to obtain a chitosan coating modifier; the preparation method of the nano modified hydroxyapatite comprises the following steps:
firstly, delivering nano-hydroxyapatite into deionized water with the volume being 3-5 times that of the nano-hydroxyapatite, then adding a coupling agent with the volume being 5-10% of that of the nano-hydroxyapatite and sodium hydroxide with the volume being 1-5% of that of the nano-hydroxyapatite, uniformly stirring, finally adding schizophyllan with the volume being 1-2% of that of the nano-hydroxyapatite, continuously stirring and fully mixing, and finally washing and drying to obtain the nano-modified hydroxyapatite.
2. The nano slow release microcapsule according to claim 1, wherein the nano slow release microcapsule comprises the following raw materials in parts by weight:
15 parts of red ginseng extract, 12.5 parts of camphor tree leaf extract, 7.5 parts of narrow She Qinghao leaf/stem extract, 6 parts of chitosan coating modifier, 2 parts of nano modified hydroxyapatite, 20 parts of caprylic/capric glyceride and 25 parts of deionized water.
3. The nano slow release microcapsule according to claim 1, wherein the mass fraction of the sodium alginate solution is 10-20%.
4. The nano-sustained release microcapsule according to claim 1, wherein the pH is adjusted to 5.0 with hydrochloric acid.
5. The nano slow release microcapsule according to claim 1, wherein the coupling agent is a coupling agent KH560.
6. The nano slow release microcapsule according to claim 1, wherein the particle size of the nano hydroxyapatite is 10-20nm.
7. A method for preparing the nano slow release microcapsule according to any one of claims 1-6, comprising the steps of:
firstly, stirring and mixing a chitosan coated modifier and nano modified hydroxyapatite to obtain an additive;
step two: adding Ginseng radix Rubri extract, camphor tree leaf extract and She Qinghao leaf/stem extract into deionized water to form water phase;
step three: heating the oil phase of the caprylic/capric glyceride to 50-70 ℃, then adding the caprylic/capric glyceride into the water phase in the third step, then adding the additive, shearing and homogenizing at a rotating speed of 1000-1500r/min, and shearing and homogenizing for 25-35min to obtain a premix;
step four: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
8. The method for preparing the nanometer slow-release microcapsule according to claim 7, wherein the critical preparation technology is that the premixed emulsion is injected into a carbon dioxide fluid reaction kettle, and the temperature is 310-330K, the pressure is 10-12MPa, and the CO is 2 Treating for 30-60min under the condition of flow velocity to obtain suspension; CO 2 The flow rate is 0.4-0.7L/min, and finally washing and drying are carried out.
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