CN106619570B - A kind of synthetic method of hollow mesoporous silicon dioxide nano medicament capsule - Google Patents
A kind of synthetic method of hollow mesoporous silicon dioxide nano medicament capsule Download PDFInfo
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- 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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- 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
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
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Abstract
The invention belongs to Nano medication fields, more particularly to a kind of synthetic method of hollow mesoporous silicon dioxide nano medicament capsule, this method first carries out propyl acrylate base group modification to hollow mesoporous silicon oxide, is dispersed in the buffer containing drug, then polyethyleneglycol diacrylate and initiator ammonium persulfate is added, accelerator N is added dropwise thereto again, N, N', N'- tetramethylethylenediamine, make polyethyleneglycol diacrylate that polymerization reaction occur in hollow meso-porous titanium dioxide silicon face and propyl acrylate group, forms polymer wrapper.The encapsulation that the loading, Nano capsule of drug are completed in the buffer containing drug, can be to avoid the leakage of the drug in encapsulation process, and synthesis process is simple, and the thickness and compactness extent of package are adjustable.
Description
Technical field
The invention belongs to Nano medication fields, and in particular to a kind of synthesis of hollow mesoporous silicon dioxide nano medicament capsule
Method.
Background technique
Nanotechnology has expedited the emergence of Nano medication in the development of biomedical aspect, i.e., drug and auxiliary material is prepared into partial size and existed
The Drug-loaded Nanoparticles within the scope of 1~100 nm simultaneously construct Nano medication delivery system.The appearance of Nano medication is so that medicine
The many conventional difficulties in field are addressed.Compared to conventional medicament, Nano medication conveying can improve the stability of drug, metabolism
Dynamics, and drug effect is increased substantially by the targeting conveying to lesion tissue and reduces side effect.More receive is studied at present
Rice pharmaceutical carrier has liposome, polymer micelle, haemocyanin, gold nano grain and mesoporous silicon oxide etc..Its intermediary hole two
Silica has orderly adjustable meso-hole structure, high specific pore volume product, is easy to the characteristics such as surface modification and good biological safety,
Research hotspot as Nano medication.Hollow mesoporous silica nano-particle is a kind of using mesoporous silicon oxide as the hollow of shell
Nano material, possessed cavity can account for 50% of particle overall volume or more, greatly improve load capacity, be very suitable for making
For nano-medicament carrier.
Although hollow mesoporous silica nano-particle is well suited as nano-medicament carrier, how using hollow mesoporous
Nano SiO 2 particle realizes loading and encapsulation to drug, is still a challenge, and a kind of current mode is to utilize model
De Huali directly carries out drug loading, without take surface encapsulation (Small, 2010,6,471-478; ACS Nano,
2008,2,889-896) hollow mesoporous silica nano-particle surface is without envelope when, being loaded and encapsulated using which
Dress will cause drug leakage, and cause the holding time of Nano medication to shorten reduces with drug effect；Another side of process of synthesizing nano-drugs
Formula be hollow mesoporous silica nano-particle is packaged by surface modification (J. Am. Chem. Soc., 2011,
133, 8778- 8781;Angew. Chem. Int. Ed. Engl., 2013,52,5580-5584), the packaging method
Multistep reaction is needed, process is cumbersome, and first that the mesoporous silicon oxide after loading drug is molten from drug due to needing before encapsulation
It is separated in liquid, this process equally will cause drug leakage, it is therefore desirable to further to the prior art to be improved.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide it is a kind of it is simple and effective, can be directly in drug solution
In the synthetic method of nano medicinal capsule that is loaded and encapsulates, it is intended to improve drug effect, avoid revealing, extend the shelf life.
Based on above-mentioned purpose, the present invention is adopted the following technical scheme that:
A kind of synthetic method of hollow mesoporous silicon dioxide nano medicament capsule, is made of following steps:
(1) hollow mesoporous silica nano-particle ultrasonic disperse is added into ammonium hydroxide and 3- (front three in dehydrated alcohol
Oxygroup first silicon substrate) propyl methacrylate, under 30-35 °C, with the mixing speed of 500 rpm, after stirring 3-8 h, from
Heart separation, gained precipitates ultrasonic disperse in 1 × PBS buffer solution, then is centrifugated, and to remove remaining ethyl alcohol, obtains table
The hollow mesoporous silica nano-particle precipitating of propyl acrylate group is modified in face；
Wherein, the dehydrated alcohol, hollow mesoporous silica nano-particle, ammonium hydroxide, 3- (trimethoxy first silicon substrate)
The ratio of propyl methacrylate is (10 ~ 100) mL: (5 ~ 50) mg: (0.2 ~ 5) mL: (50 ~ 500) mg, described
Ammonium hydroxide mass percentage concentration be 28-30 %；
(2) drug is sufficiently dissolved in 1 × PBS buffer solution, adds the surface modification propyl acrylate of step (1)
The hollow mesoporous silica nano-particle of group precipitates, and ultrasonic disperse is uniform；
Wherein, 1 × PBS buffer solution of the drug containing, surface modification propyl acrylate group hollow mesoporous two
The ratio of silica nano particle precipitating is (10 ~ 50) mL: (5 ~ 50) mg；
(3) polyethyleneglycol diacrylate and initiator ammonium persulfate are added in the solution in step (2), at 40 °C
Under, N containing accelerator, N, N', 1 × PBS buffer solution of N'- tetramethylethylenediamine, reaction 4-6 is added dropwise thereto while stirring
h；It is then centrifuged for separating, the nano particle of surface package polymer is separated with drug solution, obtains hollow mesoporous dioxy
SiClx nano medicinal capsule；
Wherein, the monomer polyethyleneglycol diacrylate, ammonium persulfate, N, N, N', N'- tetramethylethylenediamine ratio are
(20 ~ 200) mg: (1 ~ 10) mg: (1 ~ 10) mg.
Further, the hollow mesoporous silica nano-particle partial size is 300-500 nm.
Further, the polyethyleneglycol diacrylate molecular size range can be selected from 250-2000.
Further, the frequency of the ultrasonic disperse is 40 kHz, 15-20 min of time.
Further, 12000 rpm of speed, 15 min of time of the centrifuge separation.
Further, mixing speed is 500 rpm in the step (3).
Compared with prior art, technical effect of the invention are as follows:
1. synthetic method of the invention is to complete the encapsulation of the loading, Nano capsule of drug directly in drug solution, keep away
Exempt from the drug leakage loss in encapsulation process, synthesis process is simple, and thickness, the compactness extent of surface polyethylene glycol package can
Regulated and controled according to the additional amount of polyethyleneglycol diacrylate, polyethyleneglycol diacrylate molecular weight reduces, wrapping layer
Compactness extent improves, and increasing polyethyleneglycol diacrylate dosage can be improved thickness.
2. the drug solution of synthetic method of the invention can be used for next group nanometer after separating with synthetic Nano capsule
The synthesis of capsule, reuse is good in economic efficiency, is easy to amplify production.
3. hollow mesoporous silicon dioxide nano medicament capsule surface of the present invention is polyethylene glycol package, there is biology
The good feature of compatibility, because may be directly applied to field of biomedicine without further being modified.
Detailed description of the invention
Fig. 1 is the high-resolution and low resolved transmittance electricity of the hollow mesoporous silicon dioxide nano medicament capsule of the embodiment of the present invention 2
Mirror figure；
Fig. 2 is the high-resolution and low resolved transmittance electricity of the hollow mesoporous silicon dioxide nano medicament capsule of the embodiment of the present invention 3
Mirror figure.
Specific embodiment
Embodiment 1:
A kind of synthetic method for the hollow mesoporous silicon dioxide nano medicament capsule loading gemcitabine hydrochloride, including it is following
Step:
(1) by 50 mg partial sizes be 500 nm hollow mesoporous silica nano-particle with the frequency ultrasound 20 of 40 kHz
Min is dispersed in 50 mL dehydrated alcohols, adds 5 mL ammonium hydroxide and 3- (trimethoxy first silicon substrate) methacrylic acid of 500mg
Propyl ester is stirred to react 8 h under 35 °C with the speed of 500 rpm；15 min are centrifuged with 12000 rpm revolving speeds later, it will be from
Precipitating after the heart is dispersed in 20 1 × PBS buffer solution of mL with 40 kHz frequency ultrasound, 20 min, then with 12000 rpm's
Speed is centrifuged 15 min, to remove remaining ethyl alcohol, obtains the hollow mesoporous silicon oxide of surface modification propyl acrylate group
Nanoparticle precipitate.
(2) 300 mg gemcitabine hydrochlorides are sufficiently dissolved in 1 × PBS buffer solution of 50 mL, adds step
(1) the hollow mesoporous silica nano-particle precipitating of resulting surface modification propyl acrylate group, under 40 kHz frequencies
20 min of ultrasonic disperse.
(3) it is 1000 polyethyleneglycol diacrylates and 10 mg that 100 mg molecular weight are added in the solution in step (2)
Initiator ammonium persulfate is stirred, while 5 mL accelerator solution (institutes being added dropwise thereto under 40 °C with the speed of 500 rpm
The accelerator solution stated is 1 × PBS buffer solution containing 10 mg N, N, N', N'- tetramethylethylenediamines), dropwise addition process is held
Continuous 1 h, the reaction was continued 4 h, are centrifuged 15 min later with 12000 rpm revolving speeds, by the nano particle of surface package polymer with
Drug solution is separated, and hollow mesoporous silicon dioxide nano medicament capsule is obtained.
Embodiment 2:
A kind of synthetic method for the hollow mesoporous silicon dioxide nano medicament capsule loading doxorubicin hydrochloride, including following step
It is rapid:
(1) hollow mesoporous silica nano-particle that 10 mg partial sizes are 300 nm is divided with 40 kHz, 20 min of ultrasound
It is dispersed in 10 mL dehydrated alcohols, adds 0.4 mL ammonium hydroxide and 100 mg 3- (trimethoxy first silicon substrate) methacrylic acid third
Ester is stirred to react 8 h under 30 °C with the speed of 500 rpm；15 min are centrifuged with 12000 rpm revolving speeds later, will be centrifuged
Precipitating afterwards is dispersed in 20 1 × PBS buffer solution of mL with 40 kHz frequency ultrasound, 20 min, then with 12000 rpm revolving speeds
15 min are centrifuged, to remove remaining ethyl alcohol.Obtain the hollow mesoporous silicon dioxide nano of surface modification propyl acrylate group
Particle precipitating.
(2) 100 mg doxorubicin hydrochlorides are dissolved in 1 × PBS buffer solution of 10 mL, are added obtained by step (1)
Surface modification propyl acrylate group hollow mesoporous silica nano-particle precipitating, the ultrasonic disperse under 40 kHz frequencies
20 min。
(3) it is that 2000 polyethyleneglycol diacrylates and 2 mg draw that 80 mg molecular weight are added into step (2) acquired solution
Agent ammonium persulfate is sent out, under 40 °C, is stirred with the speed of 500 rpm, while it is (described that 5 mL accelerator solutions are added dropwise thereto
Accelerator solution be 1 × PBS buffer solution containing 2 mg N, N, N', N'- tetramethylethylenediamines), dropwise addition process continues 1
H, the reaction was continued later 5 h；12000 rpm are centrifuged 15 min later, and the nano particle of surface package polymer and drug is molten
Liquid is separated, and hollow mesoporous silicon dioxide nano medicament capsule is obtained.
As shown in Figure 1, the hollow mesoporous silicon dioxide nano medicament capsule for loading adriamycin in embodiment 2 is amplifying respectively
60000 times and 10000 times of lower transmission electron microscope photos, hollow mesoporous silicon oxide cavity is interior to load drug, and one is wrapped in outside shell
The loose polymeric layer of layer, thickness is about 10 nm.
Embodiment 3
A kind of synthetic method for the hollow mesoporous silicon dioxide nano medicament capsule loading cis-platinum, comprising the following steps:
(1) hollow mesoporous silica nano-particle that 20 mg partial sizes are 300 nm is divided with 40 kHz, 20 min of ultrasound
It is dispersed in 20 mL dehydrated alcohols, adds 0.4 mL ammonium hydroxide and 200 mg 3- (trimethoxy first silicon substrate) methacrylic acid third
Ester is stirred to react 4 h under 30 °C with the speed of 500 rpm；15 min are centrifuged with 12000 rpm revolving speeds later, will be centrifuged
Precipitating afterwards is dispersed in 20 1 × PBS buffer solution of mL with 40 kHz frequency ultrasound, 20 min, then with 12000 rpm revolving speeds
15 min are centrifuged, to remove remaining ethyl alcohol.Obtain the hollow mesoporous silicon dioxide nano of surface modification propyl acrylate group
Particle precipitating.
(2) 40 mg cis-platinums are dissolved in 1 × PBS buffer solution of 20 mL, add step (1) resulting surface and repairs
Adorn the hollow mesoporous silica nano-particle precipitating of propyl acrylate group, 20 min of ultrasonic disperse under 40 kHz frequencies.
(3) it is 250 polyethyleneglycol diacrylates and 3 mg that 50 mg molecular weight are added into step (2) acquired solution
Initiator ammonium persulfate is stirred, while 5 mL accelerator solution (institutes being added dropwise thereto under 40 °C with the speed of 500 rpm
The accelerator solution stated is 1 × PBS buffer solution containing 3 mg N, N, N', N'- tetramethylethylenediamines), process is added dropwise and continues
1 h, the reaction was continued later 3 h；15 min are centrifuged with 12000 rpm revolving speeds later, surface will be wrapped up to the nanometer of polymer
Grain is separated with drug solution, obtains hollow mesoporous silicon dioxide nano medicament capsule.
As shown in Fig. 2, the hollow mesoporous silicon dioxide nano medicament capsule for loading cis-platinum in embodiment 3 is amplifying respectively
40000 times and 10000 times of lower transmission electron microscope photos, hollow mesoporous silicon oxide internal layer packaging medicine, hollow mesoporous silicon oxide
Shell is wrapped in one layer of fine and close polymeric layer, and thickness is about 4 nm.
By Fig. 1-2 it is found that the thickness and compactness extent of the polymer wrapper of hollow mesoporous silicon oxide medicament capsule
With the molecular weight of polyethyleneglycol diacrylate and relative amounts in relation to: the molecular weight of polyethyleneglycol diacrylate reduces
When, polymer wrapper compactness extent increases；When the relative amounts of polyethyleneglycol diacrylate improve, polymer wrapper
Thickness increases.
Claims (6)
1. a kind of synthetic method of hollow mesoporous silicon dioxide nano medicament capsule, which is characterized in that be made of following steps:
(1) hollow mesoporous silica nano-particle ultrasonic disperse is added into ammonium hydroxide and 3- (trimethoxy in dehydrated alcohol
First silicon substrate) propyl methacrylate, under 30-35 °C, after being stirred to react 3-8 h, centrifuge separation, gained precipitating ultrasound
It is dispersed in 1 × PBS buffer solution, then is centrifugated, to remove remaining ethyl alcohol, obtain surface modification propyl acrylate group
Hollow mesoporous silica nano-particle precipitating；
Wherein, the dehydrated alcohol, hollow mesoporous silica nano-particle, ammonium hydroxide, 3- (trimethoxy first silicon substrate) methyl
The ratio of propyl acrylate is (10 ~ 100) mL: (5 ~ 50) mg: (0.2 ~ 5) mL: (50 ~ 500) mg, the ammonium hydroxide
Mass percentage concentration be 28-30 %；
(2) drug is sufficiently dissolved in 1 × PBS buffer solution, adds the surface modification propyl acrylate group of step (1)
Hollow mesoporous silica nano-particle precipitating, ultrasonic disperse is uniform；
Wherein, 1 × PBS buffer solution of the drug containing, surface modification propyl acrylate group hollow meso-porous titanium dioxide
The ratio of nano silicon particles precipitating is (10 ~ 50) mL: (5 ~ 50) mg；
(3) polyethyleneglycol diacrylate and initiator ammonium persulfate, under 40 °C, side are added in the solution in step (2)
N containing accelerator, N, N' is added dropwise in stirring side thereto, and 1 × PBS buffer solution of N'- tetramethylethylenediamine reacts 4-6 h；So
After be centrifugated, by surface package polymer nano particle separated with drug solution, obtain hollow mesoporous silicon oxide
Nano medicinal capsule；
Wherein, the monomer polyethyleneglycol diacrylate, ammonium persulfate, N, N, N', N'- tetramethylethylenediamine ratio are (20
~ 200) mg: (1 ~ 10) mg: (1 ~ 10) mg.
2. a kind of synthetic method of hollow mesoporous silicon dioxide nano medicament capsule according to claim 1, feature exist
In the hollow mesoporous silica nano-particle partial size is 300-500 nm.
3. a kind of synthetic method of hollow mesoporous silicon dioxide nano medicament capsule according to claim 1, feature exist
In the polyethyleneglycol diacrylate molecular size range is selected from 250-2000.
4. a kind of synthetic method of hollow mesoporous silicon dioxide nano medicament capsule according to claim 1, feature exist
In the frequency of the ultrasonic disperse is 40 kHz, 15-20 min of time.
5. a kind of synthetic method of hollow mesoporous silicon dioxide nano medicament capsule according to claim 1, feature exist
In 12000 rpm of speed, 15 min of time of the centrifuge separation.
6. a kind of synthetic method of hollow mesoporous silicon dioxide nano medicament capsule according to claim 1, feature exist
In mixing speed is 500 rpm in the step (3).
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| CN103013016A (en) * | 2011-09-28 | 2013-04-03 | 国家纳米科学中心 | Medical carrier and medical composition and preparation method thereof |
| CN104193982A (en) * | 2014-08-07 | 2014-12-10 | 湖北工业大学 | Methoxypolyethylene-glycol-modified mesoporous silicon dioxide nanoparticle as well as preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013016A (en) * | 2011-09-28 | 2013-04-03 | 国家纳米科学中心 | Medical carrier and medical composition and preparation method thereof |
| CN104193982A (en) * | 2014-08-07 | 2014-12-10 | 湖北工业大学 | Methoxypolyethylene-glycol-modified mesoporous silicon dioxide nanoparticle as well as preparation method and application thereof |
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| PEGylated hollow mesoporous silica nanoparticles as potential drug delivery vehicles;Yufang Zhu et al;《Microporous and Mesoporous Materials》;20101117;第141卷;第199-206页 |
| Preparation and characterization of crosslinked poly(ethylene glycol) diacrylate hydrogels as fouling-resistant membrane coating materials;Hao Ju et al;《Journal of Membrane Science》;20090104;第330卷;第180-188页 |
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