CN114849604A - Preparation method of single-hole microspheres - Google Patents
Preparation method of single-hole microspheres Download PDFInfo
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- CN114849604A CN114849604A CN202210378025.XA CN202210378025A CN114849604A CN 114849604 A CN114849604 A CN 114849604A CN 202210378025 A CN202210378025 A CN 202210378025A CN 114849604 A CN114849604 A CN 114849604A
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- polyvinyl alcohol
- aqueous solution
- stirring
- alcohol aqueous
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5026—Organic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyvinyl pyrrolidone, poly(meth)acrylates
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5031—Organic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyethylene glycol, poly(lactide-co-glycolide)
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
Abstract
The invention discloses a preparation method of a polymer microsphere with a single-hole hollow structure. Mixing polycaprolactone and polylactic acid according to a certain proportion, dissolving in dichloromethane, slowly adding a certain volume of the polymer solution into a stirred polyvinyl alcohol aqueous solution with a certain concentration, stirring for a certain time at a certain temperature, standing and precipitating polymer microspheres in the polyvinyl alcohol aqueous solution, washing for several times, and drying for 12 hours at 50 ℃ to obtain a final product. Compared with the prior art, the invention has the advantages that: the surface of the obtained polymer microsphere is provided with a hole; the obtained polymer microsphere has a spherical cavity inside, can be used for loading medicines, and has the advantages of simple manufacturing steps, low manufacturing cost and contribution to popularization and use.
Description
Technical Field
The invention relates to the technical field of polymer microspheres, in particular to a preparation method of a single-hole microsphere.
Background
Compared with solid microspheres, the single-hole microspheres can wrap the medicine after preparation, so that the possible damage of harsh physical or chemical conditions to the medicine in the preparation process of the microspheres can be avoided, the controlled release effect of the single-hole microspheres is better compared with porous microspheres, and due to the reduction of the number of holes, the number of medicine molecules diffused out of cavities of the microspheres in unit time is less, so that the diffusion time is longer, and the slow release effect is realized.
At present, the single-pore microspheres are mostly prepared by a template method, the steps are complicated, the cost is high, the popularization is not facilitated, the solvent volatilization method is a simple and effective preparation method of the high-molecular microspheres, and the single-pore microspheres are prepared by improving the solvent volatilization method.
Disclosure of Invention
The invention aims to provide a polymer microsphere with a single open pore and an internal cavity structure, which is used for local drug controlled release in vivo.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a preparation method of a single-hole microsphere is characterized by comprising the following steps: the preparation method comprises the steps of mixing polycaprolactone and polylactic acid according to a ratio, dissolving in dichloromethane, slowly adding the mixed polymer solution into the stirring polyvinyl alcohol aqueous solution, heating and stirring, standing and precipitating polymer microspheres in the polyvinyl alcohol aqueous solution, washing for multiple times, and drying at 50 ℃ for 12 hours to obtain a final product.
Preferably, the mass ratio of the polycaprolactone to the polylactic acid is 7: 3-3: 7.
Preferably, the mass fraction of the macromolecular mixture of polycaprolactone and polylactic acid in dichloromethane is 10-30%.
Preferably, the total volume of the polycaprolactone and the polylactic acid polymer solution is 500-1000 ml.
Preferably, the concentration of the polyvinyl alcohol aqueous solution is 1-3%.
Preferably, the volume of the polyvinyl alcohol aqueous solution is 2500-4000 ml.
Preferably, the stirring mode of the polyvinyl alcohol aqueous solution is mechanical stirring, and the rotating speed is 100-400 rpm.
Preferably, the stirring temperature is 30-50 ℃, and the stirring time is 12-24 hours.
After adopting the structure, the invention has the following advantages: the surface of the obtained polymer microsphere is provided with a hole; the obtained polymer microsphere has a spherical cavity inside, can be used for loading medicines, and has the advantages of simple manufacturing steps, low manufacturing cost and contribution to popularization and use.
Drawings
FIG. 1 is a scanning electron microscope image of a polymer microsphere with a single-hole hollow structure according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
With the attached figure 1, the preparation method of the single-hole microsphere is characterized in that: the preparation method comprises the steps of mixing polycaprolactone and polylactic acid according to a ratio, dissolving in dichloromethane, slowly adding the mixed polymer solution into the stirring polyvinyl alcohol aqueous solution, heating and stirring, standing and precipitating polymer microspheres in the polyvinyl alcohol aqueous solution, washing for multiple times, and drying at 50 ℃ for 12 hours to obtain a final product.
The mass ratio of the polycaprolactone to the polylactic acid is 7: 3-3: 7, the optimal mass ratio of the polycaprolactone to the polylactic acid is 3:2, the mass fraction of a high polymer mixture of the polycaprolactone and the polylactic acid in dichloromethane is 10% -30%, the total volume of the polycaprolactone and the polylactic acid high polymer solution is 500-1000 ml, the concentration of the polyvinyl alcohol aqueous solution is 1-3%, the volume of the polyvinyl alcohol aqueous solution is 2500-4000 ml, the stirring mode of the polyvinyl alcohol aqueous solution is mechanical stirring, the rotating speed is 100-400 rpm, the stirring temperature is 30-50 ℃, and the stirring time is 12-24 hours.
In the specific implementation of the invention, the preparation of the (first) polycaprolactone and polylactic acid macromolecule solution is that 120g of polycaprolactone and 80g of polylactic acid are dissolved in 800ml of dichloromethane and stirred for 2h at 37 ℃ to ensure complete dissolution.
And (II) preparing a polyvinyl alcohol aqueous solution, namely dissolving 52.5g of polyvinyl alcohol powder in 3500ml of distilled water, and stirring for 2 hours at 50 ℃ to ensure that the polyvinyl alcohol powder is completely dissolved.
And (III) volatilizing the solvent and forming microspheres, after the polyvinyl alcohol aqueous solution is completely dissolved and is cooled to room temperature, slowly adding the polycaprolactone and polylactic acid high molecular solution into the polyvinyl alcohol aqueous solution which is mechanically stirred at the rotating speed of 350rpm, setting the temperature of a stirring system to be 35 ℃, and stirring for 24 hours.
And (IV) washing and drying the microspheres, standing the stirring system to settle the microspheres, removing supernatant after the microspheres are completely settled, adding distilled water or tap water again to clean, repeatedly cleaning for 5-8 times, and drying the microspheres in a drying oven at 50 ℃ for 12 hours to obtain the final polymer microspheres with single holes and hollow structures.
The present invention and its embodiments have been described above, but the description is not limitative, and the actual structure is not limited thereto. In summary, those skilled in the art should, without departing from the spirit of the present invention, devise similar structural modes and embodiments without inventively designing them, and shall fall within the scope of the present invention.
Claims (8)
1. A preparation method of a single-hole microsphere is characterized by comprising the following steps: the preparation method comprises the steps of mixing polycaprolactone and polylactic acid according to a ratio, dissolving in dichloromethane, slowly adding the mixed polymer solution into the stirring polyvinyl alcohol aqueous solution, heating and stirring, standing and precipitating polymer microspheres in the polyvinyl alcohol aqueous solution, washing for multiple times, and drying at 50 ℃ for 12 hours to obtain a final product.
2. The method for preparing a single-pore microsphere according to claim 1, wherein the method comprises the following steps: the mass ratio of the polycaprolactone to the polylactic acid is 7: 3-3: 7.
3. The method for preparing a single-pore microsphere according to claim 1, wherein: the mass fraction of the high molecular mixture of polycaprolactone and polylactic acid in dichloromethane is 10-30%.
4. The method for preparing a single-pore microsphere according to claim 1, wherein: the total volume of the polycaprolactone and the polylactic acid polymer solution is 500-1000 ml.
5. The method for preparing a single-pore microsphere according to claim 1, wherein: the concentration of the polyvinyl alcohol aqueous solution is 1-3%.
6. The method for preparing a single-pore microsphere according to claim 1, wherein: the volume of the polyvinyl alcohol aqueous solution is 2500-4000 ml.
7. The method for preparing a single-pore microsphere according to claim 1, wherein: the stirring mode of the polyvinyl alcohol aqueous solution is mechanical stirring, and the rotating speed is 100-400 rpm.
8. The method for preparing a single-pore microsphere according to claim 1, wherein: the stirring temperature is 30-50 ℃, and the stirring time is 12-24 hours.
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| CN202210378025.XA CN114849604B (en) | 2022-04-12 | 2022-04-12 | Preparation method of single-hole microsphere |
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| CN202210378025.XA CN114849604B (en) | 2022-04-12 | 2022-04-12 | Preparation method of single-hole microsphere |
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| CN114849604A true CN114849604A (en) | 2022-08-05 |
| CN114849604B CN114849604B (en) | 2023-08-18 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB178809A (en) * | 1921-04-20 | 1923-06-04 | Ste Chim Usines Rhone | Process for the production of solutions of volatile oils |
| CN1586704A (en) * | 2004-07-15 | 2005-03-02 | 浙江大学 | Method for preparing polylactic porous microball |
| CN101108168A (en) * | 2007-08-03 | 2008-01-23 | 西安力邦医药科技有限责任公司 | Method of manufacturing fulvestrant sustained-release microspheres |
| CN102249245A (en) * | 2011-04-28 | 2011-11-23 | 华南理工大学 | Single-hole silicon dioxide hollow microsphere and preparation method thereof |
| CN102417552A (en) * | 2011-09-22 | 2012-04-18 | 中国科学院过程工程研究所 | Polymer nanomicrosphere product with uniform and controllable size and preparation method thereof |
| CN104119554A (en) * | 2014-07-15 | 2014-10-29 | 天津工业大学 | Method for preparing organic porous film by adopting freezing method |
| CN104940942A (en) * | 2014-03-31 | 2015-09-30 | 东北林业大学 | Preparation method of single-hole hollow arabinogalactan-chitosan composite microspheres |
| DE102018222807A1 (en) * | 2017-12-22 | 2019-06-27 | Shandong Rientech Medical Technology Co., Ltd. | Degradable embolic microspheres with high drug loading capacity and process for their preparation |
-
2022
- 2022-04-12 CN CN202210378025.XA patent/CN114849604B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB178809A (en) * | 1921-04-20 | 1923-06-04 | Ste Chim Usines Rhone | Process for the production of solutions of volatile oils |
| CN1586704A (en) * | 2004-07-15 | 2005-03-02 | 浙江大学 | Method for preparing polylactic porous microball |
| CN101108168A (en) * | 2007-08-03 | 2008-01-23 | 西安力邦医药科技有限责任公司 | Method of manufacturing fulvestrant sustained-release microspheres |
| CN102249245A (en) * | 2011-04-28 | 2011-11-23 | 华南理工大学 | Single-hole silicon dioxide hollow microsphere and preparation method thereof |
| CN102417552A (en) * | 2011-09-22 | 2012-04-18 | 中国科学院过程工程研究所 | Polymer nanomicrosphere product with uniform and controllable size and preparation method thereof |
| CN104940942A (en) * | 2014-03-31 | 2015-09-30 | 东北林业大学 | Preparation method of single-hole hollow arabinogalactan-chitosan composite microspheres |
| CN104119554A (en) * | 2014-07-15 | 2014-10-29 | 天津工业大学 | Method for preparing organic porous film by adopting freezing method |
| DE102018222807A1 (en) * | 2017-12-22 | 2019-06-27 | Shandong Rientech Medical Technology Co., Ltd. | Degradable embolic microspheres with high drug loading capacity and process for their preparation |
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| CN114849604B (en) | 2023-08-18 |
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