CN110200937A - The preparation method of porous hybrid microballoon containing sustained release performance - Google Patents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/13—Amines
- A61K31/135—Amines having aromatic rings, e.g. ketamine, nortriptyline
- A61K31/138—Aryloxyalkylamines, e.g. propranolol, tamoxifen, phenoxybenzamine
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- A61K31/155—Amidines (), e.g. guanidine (H2N—C(=NH)—NH2), isourea (N=C(OH)—NH2), isothiourea (—N=C(SH)—NH2)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/34—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having five-membered rings with one oxygen as the only ring hetero atom, e.g. isosorbide
- A61K31/341—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having five-membered rings with one oxygen as the only ring hetero atom, e.g. isosorbide not condensed with another ring, e.g. ranitidine, furosemide, bufetolol, muscarine
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- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/395—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
- A61K31/40—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having five-membered rings with one nitrogen as the only ring hetero atom, e.g. sulpiride, succinimide, tolmetin, buflomedil
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- 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
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- 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
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- 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
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Abstract
The present invention relates to technical field of polymer materials, disclose a kind of preparation method of porous hybrid microballoon containing sustained release performance, by nanometer calcium carbonate, water, organic solvent, polyethylene glycol (400) diacrylate, long chain fatty acids, sustained release agent, first ultrasonic disperse after mixing is subsequently added into after photoinitiator and carries out emulsifying by the uniform velocity stirring, obtains stable w/o type Pickering lotion, then it is polymerize by illumination, obtains the porous hybrid microballoon containing sustained release performance after washing is dry.The present invention not only through solid particle and other components synergistic effect, nano particle is promoted to form larger sized aggregated structure, improve its adsorptivity on interface, there is w/o type Pickering emulsion-stabilizing, and pass through the direct bundled slow-releasing agent of in-situ polymerization of monomer, sustained release agent/porous microsphere composite material is synthesized, the new function of microballoon is imparted, improves microballoon to the targeting of certain organs and tissue and the slow release of drug release.
Description
Technical field
The present invention relates to technical field of polymer materials, in particular to a kind of long chain fatty acids synergic nano carbonic acid calcium stable
Porous hybrid microballoon of the w/o type Pickering emulsion polymerization containing sustained release performance preparation method.
Background technique
The microsphere supported system of porous hybrid can utilize itself biggish specific surface area and porous structure, change adding for active matter
Delivery mode is summed it up, to reach the sustained release purpose for extending effective acting time, reducing toxic side effect.Porous hybrid microballoon conduct
A kind of novel active matter carrier system is widely studied and applied in the control sustained release field of drug or cosmetics.
Newborn effect is a kind of chemical phenomenon altogether for collaboration, and also known as synergistic effect refers to that two or more component is added
Or allotment is together, generated effect is greater than the summation acted on when various components are used alone.In w/o type Pickering cream
In many applications of liquid, many product emulsions need to keep its own characteristic for a long time, therefore lotion must be stable.So
And nano particle does not have surface-active generally, is difficult to be adsorbed on oil/water interface formation stable emulsion.Therefore it is prepared in lotion
In by the synergistic effect of solid particle and other components, promotion nano particle forms larger sized aggregated structure, improves it
, there is emulsion-stabilizing in the adsorptivity on interface, in w/o type Pickering stability of emulsion and nanotechnology using upper equal
There is very big research significance.
Summary of the invention
Goal of the invention: aiming at the problems existing in the prior art, the present invention provides a kind of long chain fatty acids synergic nano carbon
The preparation method of porous hybrid microballoon of the w/o type Pickering emulsion polymerization of sour calcium stable containing sustained release performance, the present invention is not only
By the synergistic effect of solid particle and other components, nano particle is promoted to form larger sized aggregated structure, improve its
There is w/o type Pickering emulsion-stabilizing in the adsorptivity on interface, and directly wrapped up and being delayed by the in-situ polymerization of monomer
Agent is released, sustained release agent/porous microsphere composite material is synthesized, imparts the new function of microballoon, improve microballoon to certain organs and group
The slow release of the targeting and drug release knitted.
Technical solution: the preparation method of the present invention provides a kind of porous hybrid microballoon containing sustained release performance, including it is as follows
Step: the preparation of Pickering lotion: sequentially added in a light resistant container nanometer calcium carbonate, deionized water, organic solvent,
Polyethylene glycol (400) diacrylate, long chain fatty acids and sustained release agent after 5 ~ 10min of ultrasonic disperse, are added photoinitiator, lead to
It crosses at the uniform velocity stirring progress 5 ~ 30min of emulsifying and forms stable w/o type Pickering lotion；It is porous miscellaneous containing sustained release performance
Change the preparation of microballoon: the Pickering lotion being introduced into Photoreactor, seals 5 ~ 10min of illumination, obtains polymerization porous hybrid
Microsphere suspension liquid, up to the porous hybrid microballoon containing sustained release performance after the polymerization porous hybrid microsphere suspension liquid is dried.
Preferably, in the preparation process of the Pickering lotion, the nanometer calcium carbonate, deionized water, You Jirong
Agent, polyethylene glycol (400) diacrylate, long chain fatty acids, the weight ratio of sustained release agent and photoinitiator are 3:10 ~ 20:80:
20:2 ~ 5:1 ~ 10:0.8.
Preferably, the organic solvent is toluene, normal octane, paraxylene, isoamyl acetate, positive certain herbaceous plants with big flowers alcohol or undecyl alcohol.
Preferably, the long chain fatty acids are undecenoic acid, linoleic acid, erucic acid or stearic acid.
Preferably, the sustained release agent is water soluble drug；The preferred ranitidine hydrochloride of the water soluble drug, hydrochloride
Double croaks, Propranolol or enalapril.
Preferably, the photoinitiator is 2- hydroxy-2-methyl -1- phenylacetone, 1- hydroxy-cyciohexyl Benzophenone, 2-
Hydroxy-2-methyl -1- is to ethoxy ether phenylacetone, 4- to toluene sulfydryl benzophenone, 2,4,6- trimethylbenzoyl -
Diphenyl phosphate oxidation, 2- isopropyl thioxanthone.
The utility model has the advantages that the 1, present invention passes through the synergistic effect of inorganic nanoparticles and long chain fatty acids, promote inorganic nano
Particle forms larger sized aggregated structure, improves its adsorptivity on interface, prepares stable w/o type Pickering
Lotion has very big research significance using upper in w/o type Pickering stability of emulsion and nanotechnology；And drawn by light
The more uniform porous hybrid microballoon of size is prepared in hair Pickering emulsion polymerization.
2, by utilizing surface carbon for inside active medicine package to polyethylene glycol acrylate/calcium carbonate hybrid microballoon
The acid dissolution responsiveness of sour calcium layer and the water-wet behavior of polyethylene glycol acrylate improve microballoon to certain organs and tissue
The slow release of targeting and drug release makes microballoon have new research direction in controlled release agent V-neck V domain.
3, the present invention has chosen abundant raw material, and cheap nanometer calcium carbonate can reduce cost as raw material, improve warp
Ji benefit.And the introducing of inorganic nano-particle can effectively stable emulsion, while the mechanical strength of microballoon can be enhanced, mention
High surface roughness etc..
4, present invention uses ultrasonic disperse, emulsifying, after photopolymerization can convection drying obtain finished product, not only operative employee
Sequence is simple and easy, and can't generate liquid and waste slag produced in preparation process, meets environmentally protective theory.
Detailed description of the invention
Fig. 1 is the scanning electron microscope diagram piece of porous hybrid microballoon made from embodiment 1.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing.
Embodiment 1:
The preparation method of present embodiments provide for a kind of porous hybrid microballoon containing sustained release performance, comprising the following steps:
The preparation of Pickering lotion: weighing 0.3g nanometer calcium carbonate and be added and one be protected from light in trial jar, then successively by 1.5g go from
Sub- water, the positive certain herbaceous plants with big flowers alcohol of 8g, 2g polyethylene glycol (400) diacrylate, 0.2g undecenoic acid and 0.2 ranitidine hydrochloride sequentially add
In bottle, 5 ~ 10min of ultrasonic disperse.
Then 0.08g 2,4,6- trimethylbenzoy-dipheny phosphorous oxide is weighed again, and above-mentioned dispersion microemulsion solution is added
In, 5 ~ 30min is emulsified with the even speed stirring to pulp of 10 krpm by high speed disperser and forms stable w/o type
Pickering lotion.
The preparation of porous hybrid microballoon containing sustained release performance: w/o type Pickering lotion obtained is poured into Photoreactor
In, 5 ~ 10min of illumination obtains polymerization porous hybrid microsphere suspension liquid, polymerization porous hybrid microsphere suspension liquid is filtered, washing
Afterwards, after dry 48h is put into 60 DEG C of drying boxes, it is more can to obtain the sustained release that long chain fatty acids synergic nano calcium carbonate is prepared
Hole hybrid microspheres.The electron scanning micrograph of the porous hybrid microballoon is as shown in Figure 1.This is porous miscellaneous as we can see from the figure
The size for changing microballoon is more uniform, and size is in 10 microns.
Embodiment 2:
The preparation method of present embodiments provide for a kind of porous hybrid microballoon containing sustained release performance, comprising the following steps:
The preparation of Pickering lotion: it weighs 0.3g nanometer calcium carbonate choosing addition one and is protected from light in trial jar, then successively remove 1.2g
Ionized water, the positive certain herbaceous plants with big flowers alcohol of 8g, 2g polyethylene glycol (400) diacrylate, 0.2g linoleic acid and 0.3g metformin hydrochloride successively add
Enter in bottle, 5 ~ 10min of ultrasonic disperse.
Then 0.08g 2,4,6- trimethylbenzoy-dipheny phosphorous oxide is weighed again, and above-mentioned dispersion microemulsion solution is added
In, 5 ~ 30min is emulsified with the even speed stirring to pulp of 10 krpm by high speed disperser and forms stable w/o type
Pickering lotion.
The preparation of porous hybrid microballoon containing sustained release performance: w/o type Pickering lotion obtained is poured into Photoreactor
In, 5 ~ 10min of illumination obtains polymerization porous hybrid microsphere suspension liquid, and polymerization porous hybrid microsphere suspension liquid is put into 60 DEG C and is done
In dry case after dry 48h, can obtain long chain fatty acids synergic nano calcium carbonate be prepared it is porous miscellaneous containing sustained release performance
Change microballoon.
Embodiment 3:
The preparation method of present embodiments provide for a kind of porous hybrid microballoon containing sustained release performance, comprising the following steps:
The preparation of Pickering lotion: weighing the choosing of 0.3g nanometer calcium carbonate and be added and one be protected from light in trial jar, then successively by 1g go from
Sub- water, the positive certain herbaceous plants with big flowers alcohol of 8g, 2g polyethylene glycol (400) diacrylate, 0.36g erucic acid and 0.15g Propranolol sequentially add in bottle,
5 ~ 10min of ultrasonic disperse.
Then 0.08g 2,4,6- trimethylbenzoy-dipheny phosphorous oxide is weighed again, and above-mentioned dispersion microemulsion solution is added
In, 5 ~ 30min is emulsified with the even speed stirring to pulp of 10 krpm by high speed disperser and forms stable w/o type
Pickering lotion.
The preparation of porous hybrid microballoon containing sustained release performance: w/o type Pickering lotion obtained is poured into Photoreactor
In, 5 ~ 10min of illumination obtains polymerization porous hybrid microsphere suspension liquid, and polymerization porous hybrid microsphere suspension liquid is put into 60 DEG C and is done
In dry case after dry 48h, can obtain long chain fatty acids synergic nano calcium carbonate be prepared it is porous miscellaneous containing sustained release performance
Change microballoon.
Embodiment 4:
The preparation method of present embodiments provide for a kind of porous hybrid microballoon containing sustained release performance, comprising the following steps:
The preparation of Pickering lotion: it weighs 0.3g nanometer calcium carbonate choosing addition one and is protected from light in trial jar, then successively remove 1.5g
Ionized water, the positive certain herbaceous plants with big flowers alcohol of 8g, 2g polyethylene glycol (400) diacrylate, 0.2g erucic acid and 0.2g enalapril sequentially add in bottle,
5 ~ 10min of ultrasonic disperse.
Then 0.08g 2,4,6- trimethylbenzoy-dipheny phosphorous oxide is weighed again, and above-mentioned dispersion microemulsion solution is added
In, 5 ~ 30min is emulsified with the even speed stirring to pulp of 10 krpm by high speed disperser and forms stable w/o type
Pickering lotion.
The preparation of porous hybrid microballoon containing sustained release performance: w/o type Pickering lotion obtained is poured into Photoreactor
Middle 5 ~ 10min of illumination obtains polymerization porous hybrid microsphere suspension liquid, and polymerization porous hybrid microsphere suspension liquid is put into 60 DEG C of dryings
In case after dry 48h, the porous hybrid containing sustained release performance that long chain fatty acids synergic nano calcium carbonate is prepared can be obtained
Microballoon.
Embodiment 5:
The preparation method of present embodiments provide for a kind of porous hybrid microballoon containing sustained release performance, comprising the following steps:
The preparation of Pickering lotion: weighing the choosing of 0.3g nanometer calcium carbonate and be added and one be protected from light in trial jar, then successively by 2g go from
Sub- water, the positive certain herbaceous plants with big flowers alcohol of 8g, 2g polyethylene glycol (400) diacrylate, 0.3g erucic acid and 0.5g ranitidine hydrochloride sequentially add bottle
It is interior, 5 ~ 10min of ultrasonic disperse.
Then 0.08g 2,4,6- trimethylbenzoy-dipheny phosphorous oxide is weighed again, and above-mentioned dispersion microemulsion solution is added
In, 5 ~ 30min is emulsified with the even speed stirring to pulp of 10 krpm by high speed disperser and forms stable w/o type
Pickering lotion.
The preparation of porous hybrid microballoon containing sustained release performance: w/o type Pickering lotion obtained is poured into Photoreactor
Middle 5 ~ 10min of illumination obtains polymerization porous hybrid microsphere suspension liquid, and polymerization porous hybrid microsphere suspension liquid is put into 60 DEG C of dryings
In case after dry 48h, the porous hybrid containing sustained release performance that long chain fatty acids synergic nano calcium carbonate is prepared can be obtained
Microballoon.
Embodiment 6
The preparation method of present embodiments provide for a kind of porous hybrid microballoon containing sustained release performance, comprising the following steps:
The preparation of Pickering lotion: weighing the choosing of 0.3g nanometer calcium carbonate plus set one and be protected from light trial jar, then successively by 1.2g go from
Sub- water, the positive certain herbaceous plants with big flowers alcohol of 8g, 2g polyethylene glycol (400) diacrylate, 0.5g erucic acid and 0.12g ranitidine hydrochloride sequentially add bottle
It is interior, 5 ~ 10min of ultrasonic disperse.
Then 0.08g 2,4,6- trimethylbenzoy-dipheny phosphorous oxide is weighed again, and above-mentioned dispersion microemulsion solution is added
In, 5 ~ 30min is emulsified with the even speed stirring to pulp of 10 krpm by high speed disperser and forms stable w/o type
Pickering lotion.
The preparation of porous hybrid microballoon containing sustained release performance: w/o type Pickering lotion obtained is poured into Photoreactor
In, 5 ~ 10min of illumination obtains polymerization porous hybrid microsphere suspension liquid, and polymerization porous hybrid microsphere suspension liquid is put into 60 DEG C and is done
In dry case after dry 48h, can obtain long chain fatty acids synergic nano calcium carbonate be prepared it is porous miscellaneous containing sustained release performance
Change microballoon.
The technical concepts and features of above embodiment only to illustrate the invention, its object is to allow be familiar with technique
People cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent transformation or modification that Spirit Essence is done, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of the porous hybrid microballoon containing sustained release performance, which comprises the steps of:
The preparation of Pickering lotion: nanometer calcium carbonate is sequentially added in a light resistant container, deionized water, organic solvent, is gathered
Ethylene glycol (400) diacrylate, long chain fatty acids and sustained release agent after 5 ~ 10min of ultrasonic disperse, are added photoinitiator, pass through
At the uniform velocity stirring carries out 5 ~ 30min of emulsifying and forms stable w/o type Pickering lotion；
The preparation of porous hybrid microballoon containing sustained release performance: the Pickering lotion is introduced into Photoreactor, illumination after sealing
5 ~ 10min obtains polymerization porous hybrid microsphere suspension liquid, will be slow up to containing after polymerization porous hybrid microsphere suspension liquid drying
Release the porous hybrid microballoon of performance.
2. a kind of preparation method of porous hybrid microballoon containing sustained release performance according to claim 1, which is characterized in that
In the preparation process of the Pickering lotion, the nanometer calcium carbonate, deionized water, organic solvent, polyethylene glycol (400)
Diacrylate, long chain fatty acids, the weight ratio of sustained release agent and photoinitiator are 3:10 ~ 20:80:20:2 ~ 5:1 ~ 5:0.8.
3. a kind of preparation method of porous hybrid microballoon containing sustained release performance according to claim 1, which is characterized in that institute
Stating organic solvent is toluene, normal octane, paraxylene, isoamyl acetate, positive certain herbaceous plants with big flowers alcohol or undecyl alcohol.
4. a kind of preparation method of porous hybrid microballoon containing sustained release performance according to claim 1, which is characterized in that institute
Stating long chain fatty acids is undecenoic acid, linoleic acid, erucic acid or stearic acid.
5. a kind of preparation method of porous hybrid microballoon containing sustained release performance according to claim 1, which is characterized in that institute
Stating sustained release agent is water soluble drug.
6. a kind of preparation method of porous hybrid microballoon containing sustained release performance according to claim 5, which is characterized in that institute
Stating water soluble drug is ranitidine hydrochloride, metformin hydrochloride, Propranolol or enalapril.
7. a kind of preparation method of porous hybrid microballoon containing sustained release performance according to any one of claim 1 to 6,
It is characterized in that, the photoinitiator is 2- hydroxy-2-methyl -1- phenylacetone, 1- hydroxy-cyciohexyl Benzophenone, 2- hydroxyl
Base-2- methyl-1-is to ethoxy ether phenylacetone, 4- to toluene sulfydryl benzophenone, 2,4,6- trimethylbenzoyl-two
Phenylphosphine oxide, 2- isopropyl thioxanthone.
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| CN111116975A (en) * | 2019-12-30 | 2020-05-08 | 浙江大学 | Pickering emulsion gel based on mutual attraction of liquid drops and preparation method thereof |
| CN111849327A (en) * | 2020-07-07 | 2020-10-30 | 淮阴工学院 | preparation method of pH stimulation responsiveness intelligent self-warning self-repairing anticorrosion water-based coating |
| CN111992151A (en) * | 2020-07-07 | 2020-11-27 | 淮阴工学院 | preparation method of pH stimulation responsive slow-release hybrid microspheres |
| CN111849327B (en) * | 2020-07-07 | 2021-08-17 | 淮阴工学院 | preparation method of pH stimulation responsiveness intelligent self-warning self-repairing anticorrosion water-based coating |
| CN112979994A (en) * | 2021-04-01 | 2021-06-18 | 常州大学 | preparation method of Pickering miniemulsion with stable pH phase-inversion hybrid calcium carbonate |
| CN112979994B (en) * | 2021-04-01 | 2022-03-01 | 常州大学 | preparation method of Pickering miniemulsion with stable pH phase-inversion hybrid calcium carbonate |
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Application publication date: 20190906 Assignee: Deqian Technology (Jiangsu) Co.,Ltd. Assignor: HUAIYIN INSTITUTE OF TECHNOLOGY Contract record no.: X2021980015041 Denomination of invention: Preparation method of porous hybrid microspheres containing slow-release performance Granted publication date: 20210423 License type: Common License Record date: 20211222 |
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