CN106491562A - A kind of preparation method of amido modified mesoporous silicon dioxide nano particle - Google Patents
A kind of preparation method of amido modified mesoporous silicon dioxide nano particle Download PDFInfo
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- CN106491562A CN106491562A CN201611125380.7A CN201611125380A CN106491562A CN 106491562 A CN106491562 A CN 106491562A CN 201611125380 A CN201611125380 A CN 201611125380A CN 106491562 A CN106491562 A CN 106491562A
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- silicon dioxide
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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
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/5115—Inorganic compounds
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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
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5192—Processes
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Abstract
The present invention relates to a kind of preparation method of amido modified mesoporous silicon dioxide nano particle, it is characterised in that comprise the following steps：Weigh 0.08 g of CTAB to be dissolved in 13m1 dehydrated alcohol in the mixed liquor with 27.5 m1 ultra-pure waters, 25 50 min are stirred at room temperature；There is amido modified mesoporous silicon dioxide nano particle prepared by the method for the invention higher drug loading and envelop rate to have preferable load efficiency, efficiently solve the problems, such as that nano-carrier drug loading is relatively low.
Description
Technical field
The present invention relates to a kind of preparation method of amido modified mesoporous silicon dioxide nano particle.
Background technology
Andrographolide also known as andrographolide, are from acanthaceous plant Herba Andrographis Andrographis
The labdane type diterpenoids lactone compound for obtaining is extracted in paniculataNees, is the principle active component in Herba Andrographis
One of, with pharmacological actions such as antiinflammatory, infection, immunomodulating, the infection such as its antibacterium, antifungal, antiviral, protozoacide
Effect is significantly.Meanwhile, kinds of tumors (breast carcinoma, colon cancer and hepatocarcinoma etc.) cell can be suppressed to breed, its extensive antitumor is made
With increasingly causing concern.But it is insoluble in poor water, stability, bitter in the mouth, oral administration biaavailability is relatively low, patient compliance is poor etc. asks
Topic limits clinical practice.Mesoporous silicon dioxide nano particle (mesoporous silica nanoparticles, MSN) is one
Kind have homogeneous adjustable mesoporous (2～50 12m) duct, be easy to modify surfaces externally and internally, have certain wall thickness stable skeleton new
Type inorganic nano material.In addition to good biocompatibility and insignificant cytotoxicity, also specific surface area is big, carry
The advantages of property of medicine can be strong.But the single functional group in MSN surfaces limits its application in Drug absorbability and release, therefore adopts silicon
Alkane coupling agent carries out amido modified to MSN surfaces, can strengthen the interaction of mesoporous material carrier surface and medicine, so as to improve
The drug loading and sustained release performance of medicine.
Content of the invention
The present invention proposes a kind of preparation method of amido modified mesoporous silicon dioxide nano particle.
A kind of preparation method of amido modified mesoporous silicon dioxide nano particle, it is characterised in that comprise the following steps：
（1）Weigh 0.08 g of CTAB to be dissolved in 13m1 dehydrated alcohol in the mixed liquor with 27.5 m1 ultra-pure waters, 25- is stirred at room temperature
50 min；
（2）25%～28% ammonia, 0.5 ml is added when solution clear, 80 DEG C is warming up to, after stirring evenly, is added dropwise over TEOS
0.5m1, is slowly added to APTES 0.5ml after quick stirring 30min, insulation continues reaction 2h；
（3）Reaction stands ripening 8-15h after terminating, and is centrifuged 15 min with 380 × g of 1l；
（4）Extracting waste is precipitated, and successively with ultra-pure water and absolute ethanol washing 3 times, 10 ml, whitely dry then at 100 DEG C every time
Pressed powder O.5 g；
（5）Pressed powder will be obtained to be scattered in 100 ml of ethanol solution of 10 mg/ml ammonium nitrates, 80 DEG C of 10 h of backflow are removing
Template CTAB is gone, (11 380xg) 15 min are centrifuged, extracting waste is deposited in 60 DEG C of 12 h of drying under reduced pressure and obtains pressed powder 0.45
G, obtains final product.
Preferably, the step（1）Mixing time is 30min.
Preferably, the step（2）The addition of ammonia is 26%.
Preferably, the step（3）Curing time is 10h
There is amido modified mesoporous silicon dioxide nano particle prepared by the method for the invention higher drug loading and envelop rate to have
Preferably load efficiency, efficiently solves the problems, such as that nano-carrier drug loading is relatively low.
Specific embodiment
Embodiment 1.
A kind of preparation method of amido modified mesoporous silicon dioxide nano particle, comprises the following steps：
（1）Weigh 0.08 g of CTAB to be dissolved in 13m1 dehydrated alcohol in the mixed liquor with 27.5 m1 ultra-pure waters, 25- is stirred at room temperature
50 min；
（2）25%～28% ammonia, 0.5 ml is added when solution clear, 80 DEG C is warming up to, after stirring evenly, is added dropwise over TEOS
0.5m1, is slowly added to APTES 0.5ml after quick stirring 30min, insulation continues reaction 2h；
（3）Reaction stands ripening 8-15h after terminating, and is centrifuged 15 min with 380 × g of 1l；
（4）Extracting waste is precipitated, and successively with ultra-pure water and absolute ethanol washing 3 times, 10 ml, whitely dry then at 100 DEG C every time
Pressed powder O.5 g；
（5）Pressed powder will be obtained to be scattered in 100 ml of ethanol solution of 10 mg/ml ammonium nitrates, 80 DEG C of 10 h of backflow are removing
Template CTAB is gone, (11 380xg) 15 min are centrifuged, extracting waste is deposited in 60 DEG C of 12 h of drying under reduced pressure and obtains pressed powder 0.45
G, obtains final product.
The step（1）Mixing time is 30min.
Embodiment 2.
A kind of preparation method of amido modified mesoporous silicon dioxide nano particle, comprises the following steps：
（1）Weigh 0.08 g of CTAB to be dissolved in 13m1 dehydrated alcohol in the mixed liquor with 27.5 m1 ultra-pure waters, 25- is stirred at room temperature
50 min；
（2）25%～28% ammonia, 0.5 ml is added when solution clear, 80 DEG C is warming up to, after stirring evenly, is added dropwise over TEOS
0.5m1, is slowly added to APTES 0.5ml after quick stirring 30min, insulation continues reaction 2h；
（3）Reaction stands ripening 8-15h after terminating, and is centrifuged 15 min with 380 × g of 1l；
（4）Extracting waste is precipitated, and successively with ultra-pure water and absolute ethanol washing 3 times, 10 ml, whitely dry then at 100 DEG C every time
Pressed powder O.5 g；
（5）Pressed powder will be obtained to be scattered in 100 ml of ethanol solution of 10 mg/ml ammonium nitrates, 80 DEG C of 10 h of backflow are removing
Template CTAB is gone, (11 380xg) 15 min are centrifuged, extracting waste is deposited in 60 DEG C of 12 h of drying under reduced pressure and obtains pressed powder 0.45
G, obtains final product.
The step（1）Mixing time is 30min, the step（2）The addition of ammonia is 26%.
Embodiment 3.
A kind of preparation method of amido modified mesoporous silicon dioxide nano particle, comprises the following steps：
（1）Weigh 0.08 g of CTAB to be dissolved in 13m1 dehydrated alcohol in the mixed liquor with 27.5 m1 ultra-pure waters, 25- is stirred at room temperature
50 min；
（2）25%～28% ammonia, 0.5 ml is added when solution clear, 80 DEG C is warming up to, after stirring evenly, is added dropwise over TEOS
0.5m1, is slowly added to APTES 0.5ml after quick stirring 30min, insulation continues reaction 2h；
（3）Reaction stands ripening 8-15h after terminating, and is centrifuged 15 min with 380 × g of 1l；
（4）Extracting waste is precipitated, and successively with ultra-pure water and absolute ethanol washing 3 times, 10 ml, whitely dry then at 100 DEG C every time
Pressed powder O.5 g；
（5）Pressed powder will be obtained to be scattered in 100 ml of ethanol solution of 10 mg/ml ammonium nitrates, 80 DEG C of 10 h of backflow are removing
Template CTAB is gone, (11 380xg) 15 min are centrifuged, extracting waste is deposited in 60 DEG C of 12 h of drying under reduced pressure and obtains pressed powder 0.45
G, obtains final product；
The step（1）Mixing time is 30min；The step（2）The addition of ammonia is 26%；The step（3）Ripening
Time is 10h.
Claims (4)
1. a kind of preparation method of amido modified mesoporous silicon dioxide nano particle, it is characterised in that comprise the following steps：
（1）Weigh 0.08 g of CTAB to be dissolved in 13m1 dehydrated alcohol in the mixed liquor with 27.5 m1 ultra-pure waters, 25- is stirred at room temperature
50 min；
（2）25%～28% ammonia, 0.5 ml is added when solution clear, 80 DEG C is warming up to, after stirring evenly, is added dropwise over TEOS
0.5m1, is slowly added to APTES 0.5ml after quick stirring 30min, insulation continues reaction 2h；
（3）Reaction stands ripening 8-15h after terminating, and is centrifuged 15 min with 380 × g of 1l；
（4）Extracting waste is precipitated, and successively with ultra-pure water and absolute ethanol washing 3 times, 10 ml, whitely dry then at 100 DEG C every time
Pressed powder O.5 g；
（5）Pressed powder will be obtained to be scattered in 100 ml of ethanol solution of 10 mg/ml ammonium nitrates, 80 DEG C of 10 h of backflow are removing
Template CTAB is gone, (11 380xg) 15 min are centrifuged, extracting waste is deposited in 60 DEG C of 12 h of drying under reduced pressure and obtains pressed powder 0.45
G, obtains final product.
2. a kind of preparation method of amido modified mesoporous silicon dioxide nano particle as claimed in claim 1, it is characterised in that described
Step（1）Mixing time is 30min.
3. a kind of preparation method of amido modified mesoporous silicon dioxide nano particle as claimed in claim 1, it is characterised in that described
Step（2）The addition of ammonia is 26%.
4. a kind of preparation method of amido modified mesoporous silicon dioxide nano particle as claimed in claim 1, it is characterised in that described
Step（3）Curing time is 10h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611125380.7A CN106491562A (en) | 2016-12-09 | 2016-12-09 | A kind of preparation method of amido modified mesoporous silicon dioxide nano particle |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112107694A (en) * | 2020-10-30 | 2020-12-22 | 黄山中皇制药有限公司 | Xiyanping dry suspension |
| CN112263564A (en) * | 2020-10-30 | 2021-01-26 | 黄山中皇制药有限公司 | Preparation method of Xiyanping dry suspension |
-
2016
- 2016-12-09 CN CN201611125380.7A patent/CN106491562A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112107694A (en) * | 2020-10-30 | 2020-12-22 | 黄山中皇制药有限公司 | Xiyanping dry suspension |
| CN112263564A (en) * | 2020-10-30 | 2021-01-26 | 黄山中皇制药有限公司 | Preparation method of Xiyanping dry suspension |
| CN112263564B (en) * | 2020-10-30 | 2022-07-19 | 黄山中皇制药有限公司 | Preparation method of Xiyanping dry suspension |
| CN112107694B (en) * | 2020-10-30 | 2022-07-22 | 黄山中皇制药有限公司 | Xiyanping dry suspension |
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