CN112540051A - Preparation and application of mesoporous silica-polyvinyl alcohol hydrogel sustained-release patch - Google Patents
Preparation and application of mesoporous silica-polyvinyl alcohol hydrogel sustained-release patch Download PDFInfo
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- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 74
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 72
- 238000013268 sustained release Methods 0.000 title claims abstract description 23
- 239000012730 sustained-release form Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000017 hydrogel Substances 0.000 title claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 78
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000002105 nanoparticle Substances 0.000 claims description 32
- 239000007864 aqueous solution Substances 0.000 claims description 21
- 229940043267 rhodamine b Drugs 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 19
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 239000004088 foaming agent Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 229940079593 drug Drugs 0.000 description 17
- 239000003814 drug Substances 0.000 description 17
- 229910052681 coesite Inorganic materials 0.000 description 8
- 229910052906 cristobalite Inorganic materials 0.000 description 8
- 229910052682 stishovite Inorganic materials 0.000 description 8
- 229910052905 tridymite Inorganic materials 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 230000037323 metabolic rate Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 210000003491 skin Anatomy 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 210000000434 stratum corneum Anatomy 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 230000008685 targeting Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/32—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. carbomers, poly(meth)acrylates, or polyvinyl pyrrolidone
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- A61K47/50—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
- A61K47/69—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit
- A61K47/6949—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes
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- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/70—Web, sheet or filament bases ; Films; Fibres of the matrix type containing drug
- A61K9/7023—Transdermal patches and similar drug-containing composite devices, e.g. cataplasms
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Abstract
The invention belongs to the technical field of material preparation, and particularly relates to preparation and application of a mesoporous silica-polyvinyl alcohol hydrogel sustained-release patch. The invention mainly prepares mesoporous silica-polyvinyl alcohol (SiO) by a chemical method2The PVA) hydrogel slow-release patch realizes the slow release of dye molecules through the mesoporous structure of silicon dioxide and the microporous structure of polyvinyl alcohol. The porous structure of the patch is adjusted by controlling the concentration of the mesoporous silicon dioxide and the polyvinyl alcohol,thereby optimizing the water resistance of the patch and controlling the release rate of dye molecules.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to preparation and application of a mesoporous silica-polyvinyl alcohol hydrogel sustained-release patch.
Background
The patch is a sheet-like preparation which is applied to the skin surface and can release a drug through the stratum corneum to exert an effect on the local or systemic body. Compared with oral medicines, the patch preparation can avoid the metabolism of the medicines in the liver, avoid the biological stimulation to the gastrointestinal tract and reduce or avoid the toxic and side effects of the medicines; the patch can be directly used near the focus position, and has the advantages of high drug targeting property, low dosage, convenient use and the like. The sustained-release patch can realize the slow release of the drug according to the needs of the patient, and can keep the proper drug concentration in the body for a long time by prolonging the release time, thereby avoiding the side effect of large-dose administration concentration on the patient, promoting the drug absorption and improving the drug curative effect while improving the compliance and the medication safety of the patient, reducing the administration frequency and facilitating the medication of the patient.
The mesoporous silica nanoparticles are widely applied to the field of biomedicine due to large specific surface area, high physical and chemical stability and good biocompatibility, and the mesoporous structure on the surface of the mesoporous silica nanoparticles can be used for loading drugs and realizing the slow release of drug molecules. However, the low metabolic rate of silica in vivo limits its use in the clinical setting. Therefore, the mesoporous silica nano particles loaded with the drug are fixed in the microporous framework of the polyvinyl alcohol film to prepare the silica-polyvinyl alcohol (PVA) sustained-release patch, so that the drug molecules are slowly released in vitro. Here we studied the slow release behavior of the patch using the dye molecule rhodamine b (rb) instead of the drug molecule.
Disclosure of Invention
The core content of the invention is that mesoporous silica nano particles are prepared by a sol-gel method, and are fixed inside a microporous PVA film after being loaded with dye, so that the mesoporous silica/PVA sustained-release patch is obtained. The PVA film with water stability is obtained through optimizing by selecting the type of the PVA precursor and the concentration of the solution and adjusting the drying temperature and time of the PVA film. And then the concentration of the silicon dioxide particles is adjusted to obtain the drug sustained-release film with higher flexibility.
The invention is realized by the following technical scheme:
the preparation method of the mesoporous silica-polyvinyl alcohol hydrogel sustained-release patch comprises the following steps:
(1) adding a sodium hydroxide (NaOH) aqueous solution into water, adding a surfactant, namely cetyltrimethylammonium bromide (CTAB), serving as a pore-foaming agent, adding Tetraethoxysilane (TEOS) under a water-bath heating condition, cooling to room temperature after reaction, centrifugally washing, and drying in vacuum to obtain mesoporous silica nanoparticles with the particle size of about 200 nm;
(2) preparing PVA aqueous solution, and drying at constant temperature for a certain time at different temperatures to obtain the PVA microporous film patch with water stability.
(3) Immersing the prepared mesoporous silica nanoparticles in a high-concentration dye solution, stirring at normal temperature, and centrifugally washing to obtain the dye molecule-loaded mesoporous nanoparticles.
(4) Adding mesoporous silica nanoparticles loaded with dye molecules of different masses into PVA aqueous solutions of different mass ratio concentrations, pouring the solutions into a container, and drying for a certain time to obtain the RB-loaded mesoporous silica/PVA sustained-release patch.
As a preferred technical scheme of the invention, the PVA model is selected from PVA-105 and PVA-117; the mass concentration of PVA is selected from 1 to 10%, preferably 3% and 5%.
As a preferred technical scheme of the invention, the drying is carried out for 6 to 72 hours at the constant temperature of 40 to 60 ℃.
In a preferred technical scheme of the invention, the dye molecule is Rhodamine B (RB).
As a preferred technical scheme of the invention, the step (1) is as follows: adding 3.5mL of 1M sodium hydroxide (NaOH) aqueous solution into 500mL of water, adding 100mg of surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) serving as a pore-foaming agent, adding 5mL of Tetraethoxysilane (TEOS) under the water bath heating condition of 80 ℃, reacting for 4 hours, cooling to room temperature, centrifugally washing, and drying in vacuum to obtain the mesoporous silica nanoparticles with the particle size of about 200 nm.
As a preferred technical scheme of the invention, the step (2) is as follows: preparing PVA aqueous solutions with different types (PVA-105 and PVA-117) and different mass ratio concentrations (1-10%), and drying at constant temperature (40-60 ℃) for a certain time (6-72h) at different temperatures to obtain the PVA microporous film patch with water stability.
As a preferred technical scheme of the invention, the step (3) is as follows: immersing the prepared mesoporous silica nanoparticles in a high-concentration dye solution (10mM), stirring at normal temperature for 24h, and centrifugally washing to obtain the mesoporous nanoparticles loaded with dye molecules (rhodamine B, RB).
As a preferred technical scheme of the invention, the step (4) is as follows: adding the RB-loaded mesoporous silica nanoparticles (10-30mg) with different masses into 3mL of PVA aqueous solution with different mass ratio concentrations (5-10%), pouring the PVA aqueous solution into a watch glass, and drying the PVA aqueous solution for a certain time at 50 ℃ to obtain the RB-loaded mesoporous silica/PVA sustained-release patch.
The invention provides a mesoporous silica-polyvinyl alcohol hydrogel sustained-release patch which is prepared by the preparation method.
The beneficial effects of the invention compared with the prior art comprise:
the invention mainly prepares mesoporous silica-polyvinyl alcohol (SiO) by a chemical method2The PVA) hydrogel slow-release patch realizes the slow release of dye molecules through the mesoporous structure of silicon dioxide and the microporous structure of polyvinyl alcohol. The porous structure of the patch is adjusted by controlling the concentration of the mesoporous silica and the polyvinyl alcohol, so that the water resistance of the patch is optimized and the release rate of dye molecules is controlled.
Drawings
FIG. 1, mesoporous SiO2Schematic preparation of PVA sustained release patch.
FIG. 2, SiO-before optimization of the reaction conditions, respectively2Optimized SiO/PVA film (left)2PVA film (middle) and SiO after dye loading2Photograph of PVA film (right).
FIG. 3, SiO2Scanning electron microscope image of PVA film.
FIG. 4, SiO2The slow release effect of the PVA film is shown.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the invention are not limited thereto.
Example 1:
1) adding 3.5mL of 1M sodium hydroxide (NaOH) aqueous solution into 500mL of water, adding 100mg of surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) serving as a pore-foaming agent, adding 5mL of Tetraethoxysilane (TEOS) under the water bath heating condition of 80 ℃, reacting for 4 hours, cooling to room temperature, centrifugally washing, and drying in vacuum to obtain the mesoporous silica nanoparticles with the particle size of about 200 nm.
2) Preparing PVA aqueous solution with the model of PVA-105 and the mass ratio concentration of 3 percent, and drying for 24 hours at the constant temperature of 50 ℃ to obtain the PVA microporous film patch with water stability.
3) Immersing the prepared mesoporous silica nanoparticles in a high-concentration dye solution (10mM), stirring at normal temperature for 24h, and centrifugally washing to obtain the mesoporous nanoparticles loaded with dye molecules (rhodamine B, RB).
4) And adding the RB-loaded mesoporous silica nanoparticles (20mg) into 3mL of PVA aqueous solution with the mass ratio concentration of 3%, pouring the PVA aqueous solution into a watch glass, and drying the PVA aqueous solution at 50 ℃ for a certain time to obtain the RB-loaded mesoporous silica/PVA sustained-release patch. The specific route is shown in fig. 1.
Wherein, FIG. 2 shows SiO before optimizing the reaction conditions2Optimized SiO/PVA film (left)2PVA film (middle) and SiO after dye loading2Photograph of PVA film (right). It can be seen that the film has increased flexibility after optimization.
FIG. 3, SiO2Scanning electron microscope image of PVA film. In the figure, the white particles are mesoporous SiO2And (3) nanoparticles. It can be confirmed that SiO2The nanoparticles were successfully loaded in the PVA film.
Example 2
1) Firstly, adding 3.5mL of 1M sodium hydroxide (NaOH) aqueous solution into 500mL of water, then adding 100mg of surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) as a pore-foaming agent, adding 5mL of Tetraethoxysilane (TEOS) under the water bath heating condition of 80 ℃, reacting for 4h, cooling to room temperature, centrifugally washing and drying in vacuum to obtain the mesoporous silica nanoparticles with the particle size of about 200 nm.
2) Preparing PVA aqueous solution with the model of PVA-105 and the mass ratio concentration of 5%, and drying for 24 hours at the constant temperature of 50 ℃ to obtain the PVA microporous film patch with water stability.
3) Immersing the prepared mesoporous silica nanoparticles in a high-concentration dye solution (10mM), stirring at normal temperature for 24h, and centrifugally washing to obtain the mesoporous nanoparticles loaded with dye molecules (rhodamine B, RB).
4) And adding the RB-loaded mesoporous silica nanoparticles (20mg) into 3mL of PVA water solution with the mass ratio concentration of 5%, pouring the PVA water solution into a watch glass, and drying the PVA water solution at 50 ℃ for a certain time to obtain the RB-loaded mesoporous silica/PVA sustained-release patch.
Comparative example 1
A PVA sustained-release patch having a RB loading of 3% was prepared according to the preparation method of example 1, using the steps 2) and 4).
Comparative example 2
A PVA sustained-release patch having a RB loading of 5% was prepared according to the preparation method of example 2, using steps 2) and 4).
Example 3
The sustained-release patches obtained in examples 1 and 2 and comparative examples 1 and 2 were placed in a predetermined amount of pure water, and the RB content released into the water was measured by an ultraviolet-visible spectrophotometer every time (3 to 24 hours), to investigate the sustained-release behavior of the patches.
Wherein, FIG. 4, SiO2The slow release effect of the PVA film is shown. It can be seen that mesoporous SiO is added2After nanoparticles, the dye release time was extended from 3 hours (PVA) to over 24 hours (PVA + SNP).
Wherein SNP represents SiO2And (3) nanoparticles.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. The preparation method of the mesoporous silica-polyvinyl alcohol hydrogel sustained-release patch is characterized by comprising the following steps:
(1) adding a sodium hydroxide (NaOH) aqueous solution into water, adding a surfactant, namely cetyltrimethylammonium bromide (CTAB), serving as a pore-foaming agent, adding Tetraethoxysilane (TEOS) under a water-bath heating condition, cooling to room temperature after reaction, centrifugally washing, and drying in vacuum to obtain mesoporous silica nanoparticles with the particle size of about 200 nm;
(2) preparing PVA aqueous solution, and drying at constant temperature for a certain time at different temperatures to obtain PVA microporous film patch with water stability;
(3) immersing the prepared mesoporous silica nanoparticles in a high-concentration dye solution, stirring at normal temperature, and centrifugally washing to obtain mesoporous nanoparticles loaded with dye molecules;
(4) adding mesoporous silica nanoparticles loaded with dye molecules with different masses into PVA aqueous solutions with different concentrations, pouring the solutions into a container, and drying for a certain time to obtain the RB-loaded mesoporous silica/PVA sustained-release patch.
2. The method according to claim 1, wherein the PVA type is selected from the group consisting of PVA-105, PVA-117; the mass concentration of PVA is selected from 1 to 10%, preferably 3% and 5%.
3. The method of claim 1, wherein the drying is carried out at a constant temperature of 40-60 ℃ for a period of 6-72 hours.
4. The method according to claim 1, wherein the dye molecule is rhodamine b (rb).
5. The method according to claim 1, wherein the step (1) is: adding 3.5mL of 1M sodium hydroxide (NaOH) aqueous solution into 500mL of water, adding 100mg of surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) as a pore-foaming agent, adding 5mL of Tetraethoxysilane (TEOS) under the water bath heating condition of 80 ℃, reacting for 4 hours, cooling to room temperature, centrifugally washing, and drying in vacuum to obtain the mesoporous silica nanoparticles with the particle size of about 200 nm.
6. The method according to claim 1, wherein the step (2) is: preparing PVA aqueous solutions with different types (PVA-105 and PVA-117) and different concentrations (1-10 percent), and drying at constant temperature of different temperatures (40-60 ℃) for a certain time (6-72 hours) to obtain the PVA microporous film patch with water stability.
7. The preparation method according to claim 1, wherein the prepared mesoporous silica nanoparticles are immersed in a high-concentration dye solution (10mM), stirred at normal temperature for 24h, and centrifugally washed to obtain dye molecule (rhodamine B, RB) -loaded mesoporous nanoparticles.
8. The preparation method of claim 1, wherein the RB loaded mesoporous silica nanoparticles (10-30mg) with different masses are added into 3mL of PVA aqueous solution with different mass ratio concentrations (5-10%), and the mixture is poured into a watch glass and dried at 50 ℃ for a certain time to obtain the RB loaded mesoporous silica/PVA sustained-release patch.
9. A mesoporous silica-polyvinyl alcohol hydrogel sustained-release patch characterized by being prepared by the preparation method of any one of the preceding claims 1 to 8.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114031876A (en) * | 2021-09-18 | 2022-02-11 | 贵州省材料产业技术研究院 | Anti-swelling polyvinyl alcohol composite preservative film and preparation method and application thereof |
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