CN101129340A - Method of producing nano magnetic polylactic acid composite particle for photodynamic medicament carrier - Google Patents
Method of producing nano magnetic polylactic acid composite particle for photodynamic medicament carrier Download PDFInfo
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- CN101129340A CN101129340A CNA2007100443156A CN200710044315A CN101129340A CN 101129340 A CN101129340 A CN 101129340A CN A2007100443156 A CNA2007100443156 A CN A2007100443156A CN 200710044315 A CN200710044315 A CN 200710044315A CN 101129340 A CN101129340 A CN 101129340A
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Abstract
The invention relates to a method for preparing a nanometer magnetic polylactic acid composite granule of a photodynamic medicinal vector, which comprises the following steps: (1) getting the black deposit Fe3O4 by adding over ammonia in the solution with Fe3+ and Fe2+in the nitrogen and the ambient temperature; (2) dispersing the deposit in the alcohol; adding oleic acid; dispersing with hyperacoustic; forming oil-wetted surface nanometer Fe3O4 granule; (3) transferring granule to the dissolvent; adding polylactic acid and photodynamic medicine; proceeding with ultrasonic homogenization; (4) adding di(2-ethyl group hexyl) sodium sulfosuccinate in the aqueous solution; mixing in the ambient temperature; removing the dissolvent in the low temperature and vacuum; getting the nanometer magnetic polylactic acid composite granule of a medicinal vector. The method has the simple operation, the small device, the low energy, the uniform granule, the good dispensability, the good bioavailability, the good magnetic response and the apparent photodynamic effect, which is easy to extend.
Description
Technical field
The invention belongs to nano-magnetic medicinal carrier field, particularly relate to the particulate preparation method of a kind of optical dynamic drug carrier nano magnetic.
Background technology
In nano-magnetic medicinal carrier field, from end of the seventies development so far, existing magnetic albumin microsphere, magnetic fluid, magnetic liposome and organic composite granulated etc.Show that after deliberation the magnetic albumin microsphere: particle diameter is big, magnetic induction is not strong, easily causes blood vessel embolism.Magnetic fluid: owing to there is not parcel, reactivity is strong, instability.Magnetic liposome: particle diameter is big, is difficult for preparation, is easily caught by reticuloendothelial system (RES).But the Biodegradable nano material as pharmaceutical carrier have drug loading height, controllable sustained-release, advantage such as optional material is wide and preparation method is many (J.Photoch.Photob.B.:Bio., 2002,66,89-106).
Photodynamic therapy is a kind of therapy of novelty, is widely used in diseases such as the various cancers of treatment, cardiovascular disease, dermatosis and oculopathy.Ultimate principle is that photosensitizer is under the irradiation of certain wavelength light, generation electron spin exchange, oxygen molecule around making changes singlet oxygen or free radical etc. into, matter between singlet oxygen or free radical energy oxidation various kinds of cell, comprise blood plasma, mitochondrion, lysosome and nuclear membrane or the like, make pathogen death, thereby reach the effect of treatment.
But most of photosensitizer are hydrophobic, and reuniting easily in aqueous solution causes quantum yield to reduce.In addition, photosensitizer is not high in the selection delay efficient of lesions position, thereby the research of photosensitizer drug carrier is imperative, the nanometer optical dynamic drug carrier is studied (J.Mater.Chem.2004 widely, 14,487-493), comprise nano-particle such as pottery, metal and Biodegradable material.With salting out method light power medicine ZnPcF16 is loaded in polylactic acid (PLA) nanoparticle and Polyethylene Glycol (PEG) the modification PLA nanoparticle, average diameter of particles 1000nm, drug loading have only 0.61% (Int.J.Cancer, 1996,66,821.).With polylactic acid-polyglycolic acid copolymer (PLGA) and polylactic acid (PLA) carrier, the granule mean diameter 130nm of preparation, drug loading 8% (Int.J.Pharm. as light power medicine p-THPP, 2002,233,239. and Eur.J.Pharm.Sci., 2003,18,241.).Polyacrylamide (PAA) and amination polyacrylamide (AFPAA) nano-particle find that as the carrier of light power medicine amido modified nano-particle makes the singlet oxygen productive rate reduce by 40% (Sensors Actuators B, 2003,90,82.).But aspects such as these nano particles, dispersibility, biocompatibility, light power medicine action effect, effect is also very desirable frequently.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nano magnetic polylactic acid composite particle for photodynamic medicament carrier, the composite particles that this method is prepared can be satisfied with the requirement of magnetic nano drug field on using more all sidedly.
The preparation method of nano magnetic polylactic acid composite particle for photodynamic medicament carrier of the present invention comprises the following steps:
(1) under the room temperature nitrogen, to containing Fe
3+And Fe
2+Add excess of ammonia water in the aqueous solution of salt and get black precipitate Fe
3O
4
(2) precipitation is dispersed in the alcoholic solution, adds oleic acid, ultra-sonic dispersion forms surperficial lipophilic nano ferriferrous oxide granule;
(3) the granule decant(-ation) adds polylactic acid and light power medicine, ultrasonic emulsification in solvent;
(4) add two (2-ethylhexyl) 2-Sulfosuccinic acid sodium water solution again, stirring at room, vacuum and low temperature is removed solvent, obtains nano magnetic polylactic acid composite particle for photodynamic medicament carrier.
Described Fe
3+Salt is ferric chloride, Fe
2+Salt is a kind of in ferrous chloride or the ferrous sulfate, and molar concentration rate is 2: 1;
Described ammonia concn is 1.5mol/l;
Described oleic acid amount is 10 times of precipitation capacity;
Described solvent is meant a kind of in chloroform or the dichloromethane, with the volume ratio of water be 1: 25;
Described smooth power medicine is a kind of (as: the two alcohol of porphyrin dipropyl ether etc.) in the various hydrophobic photosensitizer;
Described two (2-ethylhexyl) sodium sulfosuccinate concentration of aqueous solution is 0.049 mol/L;
Described stirring at room is meant and stirs 20h.
Beneficial effect of the present invention:
(1) simple to operate, equipment needed thereby quantity is few, and energy consumption is low;
(2) particulate epigranular, good dispersion;
(3) good biocompatibility has good magnetic responsiveness, and light power medicine action effect is obvious.
Description of drawings
Fig. 1 is the flow chart of the nano magnetic polylactic acid composite particle for photodynamic medicament carrier prepared of method provided by the invention;
Fig. 2 is 20,000 times of the transmission electron microscope pictures (1) of the nano magnetic polylactic acid composite particle for photodynamic medicament carrier prepared of method provided by the invention: (a) individual particle, (b) integral body; (2) 10 ten thousand times.
Fig. 3 is the fluorescence spectrum figure of the nano magnetic polylactic acid composite particle for photodynamic medicament carrier prepared of method provided by the invention, excitation wavelength 400nm, (a) the fluorescence spectrum figure of the nano magnetic polylactic acid composite particle that obtains after the magnetic separation, (b) the fluorescence spectrum figure of entire reaction solution.
The nano magnetic polylactic acid composite particle for photodynamic medicament carrier that Fig. 4 method provided by the invention is prepared produces the uv-spectrogram that singlet oxygen detects.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Take by weighing 2.51g (0.0093mol) FeCl
36H
2O and 1.25g (0.0045mol) FeSO
47H
2O is dissolved in the 600ml deionized water, and under the room temperature nitrogen protection, to add 24ml concentration be that the ammonia of 1.5mol/l obtains black precipitate in pointwise in above-mentioned solution.Separate with the washing precipitation 5 times at interval of deionized water and ethanol by magnetic, precipitation is dispersed in the alcoholic solution, separates with the washing precipitation 5 times at interval of deionized water and ethanol, precipitation is dispersed in the alcoholic solution by magnetic, add oleic acid 10.42g again, ultra-sonic dispersion 30min.Separate with the unnecessary oleic acid of ethanol flush away by magnetic, with the lipophilic nano ferriferrous oxide granule 0.003g of surface modified decant(-ation) in 1600 μ l chloroforms or dichloromethane equal solvent, the light power medicine that adds 0.08g polylactic acid and 60 μ l0.015 M, ultrasonic emulsification 30min.Under stirring condition, the chloroform of above-mentioned 1600 μ l or dichloromethane are added the aqueous solution that 40ml contains 0.90gAOT.Behind the stirring at room reaction 20h, vacuum and low temperature is removed organic solvent chloroform or dichloromethane, finally obtains nano magnetic polylactic acid composite particle for photodynamic medicament carrier.
Take by weighing 2.51g (0.0093mol) FeCl
36H
2O and 1.25g (0.0045mol) FeSO
47H
2O is dissolved in the 600ml deionized water, under the room temperature nitrogen protection, dropwise adds the ammonia that 24ml concentration is 1.5mol/l in above-mentioned solution, obtains black precipitate.Separate with the washing precipitation 5 times at interval of deionized water and ethanol by magnetic, precipitation is dispersed in ethanol is molten to be separated with the washing precipitation 5 times at interval of deionized water and ethanol by magnetic, precipitation is dispersed in the alcoholic solution, adds oleic acid 10.42g again, ultra-sonic dispersion emulsifying 30min.Separate with the unnecessary oleic acid of ethanol flush away by magnetic, with the lipophilic nano ferriferrous oxide granule 0.003g of surface modified decant(-ation) in 1600 μ l chloroforms or dichloromethane equal solvent, the light power medicine that adds 0.016g polylactic acid and 20 μ l0.015M, ultrasonic emulsification 30min.Under stirring condition, the chloroform of above-mentioned 1600 μ l or dichloromethane are added the aqueous solution that 40ml contains 0.90gAOT.Behind the stirring at room reaction 20h, vacuum and low temperature is removed organic solvent chloroform or dichloromethane, finally obtains nano magnetic polylactic acid composite particle for photodynamic medicament carrier.
Claims (8)
1. the preparation method of nano magnetic polylactic acid composite particle for photodynamic medicament carrier comprises the following steps:
(1) under the room temperature nitrogen, to containing Fe
3+And Fe
2+Add excess of ammonia water in the aqueous solution of salt and get black precipitate Fe
3O
4
(2) precipitation is dispersed in the alcoholic solution, adds oleic acid, ultra-sonic dispersion forms surperficial lipophilic nano ferriferrous oxide granule;
(3) the granule decant(-ation) adds polylactic acid and light power medicine, ultrasonic emulsification in solvent;
(4) add two (2-ethylhexyl) 2-Sulfosuccinic acid sodium water solution again, stirring at room, vacuum and low temperature is removed solvent, obtains nano magnetic polylactic acid composite particle for photodynamic medicament carrier.
2. the preparation method of nano magnetic polylactic acid composite particle for photodynamic medicament carrier according to claim 1 is characterized in that: described Fe
3+Salt is ferric chloride, Fe
2+Salt is a kind of in ferrous chloride or the ferrous sulfate, and molar concentration rate is 2: 1.
3. the preparation method of nano magnetic polylactic acid composite particle for photodynamic medicament carrier according to claim 1, it is characterized in that: described ammonia concn is 1.5mol/L.
4. the preparation method of nano magnetic polylactic acid composite particle for photodynamic medicament carrier according to claim 1, it is characterized in that: described oleic acid amount is 10 times of precipitation capacity.
5. the preparation method of nano magnetic polylactic acid composite particle for photodynamic medicament carrier according to claim 1 is characterized in that: described solvent is meant a kind of in chloroform or the dichloromethane, with the volume ratio of water be 1: 25.
6. the preparation method of nano magnetic polylactic acid composite particle for photodynamic medicament carrier according to claim 1 is characterized in that: described smooth power medicine is a kind of in the various hydrophobic photosensitizer.
7. the preparation method of nano magnetic polylactic acid composite particle for photodynamic medicament carrier according to claim 1, it is characterized in that: described two (2-ethylhexyl) sodium sulfosuccinate concentration of aqueous solution is 0.049mol/L.
8. the preparation method of nano magnetic polylactic acid composite particle for photodynamic medicament carrier according to claim 1 is characterized in that: described stirring at room is meant and stirs 20h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102688494A (en) * | 2011-03-23 | 2012-09-26 | 卢世璧 | Preparation method of protein drug-carrying magnetic composite nano-material and application thereof |
| CN111622020A (en) * | 2020-04-30 | 2020-09-04 | 福建省闽清双棱纸业有限公司 | Waterproof kraft paper with strong tensile property in length direction and preparation method thereof |
-
2007
- 2007-07-27 CN CN2007100443156A patent/CN101129340B/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102688494A (en) * | 2011-03-23 | 2012-09-26 | 卢世璧 | Preparation method of protein drug-carrying magnetic composite nano-material and application thereof |
| CN111622020A (en) * | 2020-04-30 | 2020-09-04 | 福建省闽清双棱纸业有限公司 | Waterproof kraft paper with strong tensile property in length direction and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN101129340B (en) | 2010-09-08 |
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