CN104528636B - A kind of functional method of magnetic-particle finishing gold nano grain - Google Patents
A kind of functional method of magnetic-particle finishing gold nano grain Download PDFInfo
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- CN104528636B CN104528636B CN201410786298.3A CN201410786298A CN104528636B CN 104528636 B CN104528636 B CN 104528636B CN 201410786298 A CN201410786298 A CN 201410786298A CN 104528636 B CN104528636 B CN 104528636B
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Abstract
The invention provides a kind of functional method of simple magnetic-particle finishing gold nano grain, namely for the method for the magnetic particle surface functional modification gold nano grain of surface carboxyl groups.First utilize polymine (PEI) by the carboxyl functional group amination on magnetic nanometer or micron particles surface; By one end sulfydryl (SH) group, other one end is that polyethylene glycol (PEG) macromolecule of N-hydroxy-succinamide is coupled on amidized magnetic particle subsequently; Last and react with gold nano grain, thus by gold nano particle modification in magnetic nanometer or micron particles.The method step is simple, and easy and simple to handle, price is relatively cheap, can set up a kind of multi-functional research platform of nanometer level.
Description
Technical field
The present invention relates to the preparation method of multifunctional nanoparticles, be specifically related to a kind of for biomolecular labeling, separation and purification, clinical molecular diagnosis, the functional method of the magnetic-particle finishing gold nano grain of the functions such as magnetic target.
Background technology
Gold nano grain is due to the optical property of its uniqueness and good chemical stability, and in nanoelectronics, the aspects such as nanophotonics, sensor, biomolecular labeling, photo-thermal therapy have broad application prospects.
Magnetic micrometer and nano particle may be used for bio-molecular separation, magnetic target medicine, medical science diagnosis and detection etc. due to its magnetic induction characteristic in magnetic field.
Magnetic-particle and gold nano grain are coupled together, a kind of multi-functional research platform of nanometer level can be set up, thus be expected to for bio-imaging and diagnosis etc.Such as, there is research team (Small2010,6:2520-2525) to be connected antigen or antibody at magnetic-particle respectively with gold nano grain, by the specific recognition of antigen-antibody, magnetic-particle and gold nano grain are linked together, thus realize multi-functional.But antigen-antibody is comparatively responsive to environment, easy sex change and cause magnetic-particle to be separated with gold nano grain, and antigen-antibody is expensive.
Therefore, be necessary to find a kind of simple chemical modification method, there is high reactivity, and stable after reaction, finally be necessary giving gold nano grain certain free degree, thus guarantee magnetic-particle does not affect the connection etc. of subsequent bio molecule after being connected with gold nano grain.Polymine
Summary of the invention
Obtaining not enough for overcoming prior art, the invention provides a kind of magnetic-particle surface gold nano grain functional modification method, namely for the method for the magnetic particle surface functional modification gold nano grain of surface carboxyl groups.
A functional method for magnetic-particle finishing gold nano grain, is characterized in that, first utilizes polymine (PEI) by the carboxyl functional group amination on magnetic nanometer or micron particles surface; By one end sulfydryl (SH) group, other one end is that polyethylene glycol (PEG) macromolecule of N-hydroxy-succinamide is coupled on amidized magnetic particle subsequently; Last and react with gold nano grain, thus by gold nano particle modification in magnetic nanometer or micron particles.
Comprise the following steps:
(1) magnetic particle surface amination: get surface carboxyl groups magnetic particle solution, by attraction on the reactor wall, liquid-transfering gun takes liquid away, add carbonate buffer solution, ultrasonic vibration dispersion magnetic particle, repeats above-mentioned cleaning process twice, the carbonate buffer solution of polymine (PEI) subsequently, reaction a period of time, utilize carbonate buffer solution, cleaning magnetic particle;
(2) magnetic particle surface Pegylation: the magnetic particle that step (1) is obtained, add sulfydryl-polyethylene glycol, molecular weight is 3000,-N-hydroxy-succinamide (HS-PEG-3000-NHS) and methoxypolyethylene glycol, molecular weight is 2000, in-N-hydroxy-succinamide (mPEG-2000-NHS) mixed carbonic acid salt buffer, reaction a period of time, chloroform is utilized to clean magnetic particle; Thus by magnetic particle surface Pegylation, long-chain difunctionalization PEG(HS-PEG-3000-NHS) with short chain list functionalization PEG(mPEG-2000-NHS) used in combinationly can ensure, utilizing long-chain difunctionalization PEG to while being connected gold nano grain, also to utilize the difference of length chain PEG molecule to ensure to the spatial degrees of freedom certain be connected gold nano grain;
(3) magnetic particle surface functional modification gold nano grain: magnetic particle step (2) obtained, adds gold nano grain chloroformic solution, reaction a period of time, utilizes ultra-pure water, and cleaning magnetic particle, normal temperature saves backup.
In step (1) carbonate buffer solution used to be pH condition be 8.2 0.05mol/L aqueous sodium carbonate, the carbonate buffer solution concentration of polymine used is 2-20%, and the reaction time is 1-3 hour.
In polyethylene glycol mixed liquor used in step (2), HS-PEG-3000-NHS Mole percent ratio is 1%-40%, and total PEG concentration is 1-40mM, and the reaction time is 1-3 hour.
In step (3), gold nano grain is solid gold nano particle, gold nanorods, and gold nanometer cage, gold nanoshell spheroid, particle diameter is 1-1000nm, and concentration is 0.01-2nmoL, and the lucifuge reaction time is 2-24 hour.
The invention provides the method for the above-mentioned magnetic particle surface functional modification gold nano grain for surface carboxyl groups, the method step is simple, easy and simple to handle, price is relatively cheap, set up a kind of multi-functional research platform of nanometer level, the biomolecular labeling of biomolecule, separation and purification can be realized, clinical molecular diagnosis, the synchronous realization of multiple function such as magnetic target.
Accompanying drawing explanation
Accompanying drawing 1 is the schematic diagram of the surface-functionalized modification gold nano grain of magnetic-particle in the present invention.
Accompanying drawing 2 is Fig. 1 partial enlarged drawings.
Accompanying drawing 3 is Fig. 1 partial enlarged drawings.
Detailed description of the invention
Below embodiments of the invention are elaborated by reference to the accompanying drawings, implement premised on the present embodiment one technical solution of the present invention, give detailed embodiment and concrete operating process, but protection of the present invention is not limited to following embodiment.
embodiment 1:
1) magnetic particle surface amination: the magnetic particle solution of getting 1mL surface carboxyl groups, by attraction on the centrifugal tube wall of 1.5mL, liquid-transfering gun takes liquid away, add 0.05mol/L carbonate buffer solution (pH8.2), ultrasonic vibration dispersion magnetic particle, repeat above-mentioned cleaning process twice, add the carbonate buffer solution of 5% polymine subsequently, reaction 2h.Utilize carbonate buffer solution to clean magnetic particle three times, remove excessive polymine.
2) magnetic particle surface Pegylation: the magnetic particle that step 1) is obtained, (total PEG concentration is 40mM to add sulfydryl-polyethylene glycol (molecular weight is 3000)-N-hydroxy-succinamide (HS-PEG-3000-NHS) of 1mL and methoxypolyethylene glycol (molecular weight is 2000)-N-hydroxy-succinamide (mPEG-2000-NHS) mixed carbonic acid salt buffer, HS-PEG-3000-NHS and mPEG-2000-NHS mol ratio is 1:4) in, reaction 2h.Utilize chloroform to clean magnetic particle three times, remove excessive peg molecule.
3) magnetic particle surface functional modification gold nano grain: by step 2) the magnetic particle that obtains, add in the gold nano grain of 1mL0.1nmoL, lucifuge reaction 18h.Utilize ultra-pure water to clean magnetic particle three times, finally add 1mL ultra-pure water, normal temperature saves backup.
embodiment 2:
1) magnetic particle surface amination: the magnetic particle solution of getting 1mL surface carboxyl groups, by attraction on the centrifugal tube wall of 1.5mL, liquid-transfering gun takes liquid away, add 0.05mol/L carbonate buffer solution (pH8.2), ultrasonic vibration dispersion magnetic particle, repeat above-mentioned cleaning process twice, add the carbonate buffer solution of 5% polymine subsequently, reaction 1h.Utilize carbonate buffer solution to clean magnetic particle three times, remove excessive polymine.
2) magnetic particle surface Pegylation: the magnetic particle that step 1) is obtained, (total PEG concentration is 20mM to add sulfydryl-polyethylene glycol (molecular weight is 3000)-N-hydroxy-succinamide (HS-PEG-3000-NHS) of 1mL and methoxypolyethylene glycol (molecular weight is 2000)-N-hydroxy-succinamide (mPEG-2000-NHS) mixed carbonic acid salt buffer, HS-PEG-3000-NHS and mPEG-2000-NHS mol ratio is 1:9) in, reaction 2h.Utilize chloroform to clean magnetic particle three times, remove excessive peg molecule.
3) magnetic particle surface functional modification gold nano grain: by step 2) the magnetic particle that obtains, add in the gold nano grain of 1mL0.2nmoL, lucifuge reaction 12h.Utilize ultra-pure water to clean magnetic particle three times, finally add 1mL ultra-pure water, normal temperature saves backup.
embodiment 3:
1) magnetic particle surface amination: the magnetic particle solution of getting 1mL surface carboxyl groups, by attraction on the centrifugal tube wall of 1.5mL, liquid-transfering gun takes liquid away, add 0.05mol/L carbonate buffer solution (pH8.2), ultrasonic vibration dispersion magnetic particle, repeat above-mentioned cleaning process twice, add the carbonate buffer solution of 5% polymine subsequently, reaction 2h.Utilize carbonate buffer solution to clean magnetic particle three times, remove excessive polymine.
2) magnetic particle surface Pegylation: the magnetic particle that step 1) is obtained, (total PEG concentration is 10mM to add sulfydryl-polyethylene glycol (molecular weight is 3000)-N-hydroxy-succinamide (HS-PEG-3000-NHS) of 1mL and methoxypolyethylene glycol (molecular weight is 2000)-N-hydroxy-succinamide (mPEG-2000-NHS) mixed carbonic acid salt buffer, HS-PEG-3000-NHS and mPEG-2000-NHS mol ratio is 1:4) in, reaction 2h.Utilize chloroform to clean magnetic particle three times, remove excessive peg molecule.
3) magnetic particle surface functional modification gold nano grain: by step 2) the magnetic particle that obtains, add in the gold nano grain of 1mL0.5nmoL, lucifuge reaction 18h.Utilize ultra-pure water to clean magnetic particle three times, finally add 1mL ultra-pure water, normal temperature saves backup.
embodiment 4:
1) magnetic particle surface amination: the magnetic particle solution of getting 1mL surface carboxyl groups, by attraction on the centrifugal tube wall of 1.5mL, liquid-transfering gun takes liquid away, add the 0.05mol/L carbonate buffer solution (pH8.2) of suitable volumes, ultrasonic vibration dispersion magnetic particle, repeat above-mentioned cleaning process twice, add the carbonate buffer solution of 5% polymine subsequently, reaction 2h.Utilize carbonate buffer solution to clean magnetic particle three times, remove excessive polymine.
2) magnetic particle surface Pegylation: the magnetic particle that step 1) obtains, (total PEG concentration is 30mM to add sulfydryl-polyethylene glycol (molecular weight is 3000)-N-hydroxy-succinamide (HS-PEG-3000-NHS) of 1mL and methoxypolyethylene glycol (molecular weight is 2000)-N-hydroxy-succinamide (mPEG-2000-NHS) mixed carbonic acid salt buffer, HS-PEG-3000-NHS and mPEG-2000-NHS mol ratio is 1:9) in, reaction 1h.Utilize chloroform to clean magnetic particle three times, remove excessive peg molecule.
3) magnetic particle surface functional modification gold nano grain: by step 2) the magnetic particle that obtains, add in the gold nano grain of 1mL0.8nmoL, lucifuge reaction 24h.Utilize ultra-pure water to clean magnetic particle three times, finally add 1mL ultra-pure water, normal temperature saves backup.
embodiment 5:
1) magnetic particle surface amination: the magnetic particle solution of getting 1mL surface carboxyl groups, by attraction on the centrifugal tube wall of 1.5mL, liquid-transfering gun takes liquid away, add the 0.05mol/L carbonate buffer solution (pH8.2) of suitable volumes, ultrasonic vibration dispersion magnetic particle, repeat above-mentioned cleaning process twice, add the carbonate buffer solution of 5% polymine subsequently, reaction 1.5h.Utilize carbonate buffer solution to clean magnetic particle three times, remove excessive polymine.
2) magnetic particle surface Pegylation: the magnetic particle that step 1) is obtained, (total PEG concentration is 25mM to add sulfydryl-polyethylene glycol (molecular weight is 3000)-N-hydroxy-succinamide (HS-PEG-3000-NHS) of 1mL and methoxypolyethylene glycol (molecular weight is 2000)-N-hydroxy-succinamide (mPEG-2000-NHS) mixed carbonic acid salt buffer, HS-PEG-3000-NHS and mPEG-2000-NHS mol ratio is 1:7) in, reaction 1h.Utilize chloroform to clean magnetic particle three times, remove excessive peg molecule.
3) magnetic particle surface functional modification gold nano grain: by step 2) the magnetic particle that obtains, add in the gold nano grain of 1mL1nmoL, lucifuge reaction 20h.Utilize ultra-pure water to clean magnetic particle three times, finally add 1mL ultra-pure water, normal temperature saves backup.
Although content of the present invention has done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple amendment of the present invention and substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (4)
1. a functional method for magnetic-particle finishing gold nano grain, is characterized in that, first utilizes polymine (PEI) by the carboxyl functional group amination on magnetic nanometer or micron particles surface; By one end sulfydryl (SH) group, other one end is that polyethylene glycol (PEG) macromolecule of N-hydroxy-succinamide is coupled on amidized magnetic particle subsequently; Last and react with gold nano grain, thus by gold nano particle modification in magnetic nanometer or micron particles, comprise the following steps:
(1) magnetic particle surface amination: get surface carboxyl groups magnetic particle solution, by attraction on the reactor wall, liquid-transfering gun takes liquid away, add carbonate buffer solution, ultrasonic vibration dispersion magnetic particle, repeats above-mentioned cleaning process twice, the carbonate buffer solution of polymine (PEI) subsequently, reaction a period of time, utilize carbonate buffer solution, cleaning magnetic particle;
(2) magnetic particle surface Pegylation: the magnetic particle that step (1) is obtained, add sulfydryl-polyethylene glycol, molecular weight is 3000,-N-hydroxy-succinamide (HS-PEG-3000-NHS) and methoxypolyethylene glycol, molecular weight is 2000, in-N-hydroxy-succinamide (mPEG-2000-NHS) mixed carbonic acid salt buffer, reaction a period of time, chloroform is utilized to clean magnetic particle; Thus by magnetic particle surface Pegylation;
(3) magnetic particle surface functional modification gold nano grain: magnetic particle step (2) obtained, adds gold nano grain chloroformic solution, reaction a period of time, utilizes ultra-pure water, and cleaning magnetic particle, normal temperature saves backup.
2. the functional method of a kind of magnetic-particle finishing gold nano grain according to claim 1, it is characterized in that, in step (1) carbonate buffer solution used to be pH condition be 8.2 0.05mol/L aqueous sodium carbonate, the carbonate buffer solution concentration of polymine used is 2-20%, and the reaction time is 1-3 hour.
3. the functional method of a kind of magnetic-particle finishing gold nano grain according to claim 1, it is characterized in that, in polyethylene glycol mixed liquor used in step (2), HS-PEG-3000-NHS Mole percent ratio is 1%-40%, total PEG concentration is 1-40mM, and the reaction time is 1-3 hour.
4. the functional method of a kind of magnetic-particle finishing gold nano grain according to claim 1, it is characterized in that, in step (3), gold nano grain is solid gold nano particle, gold nanorods, gold nanometer cage, gold nanoshell spheroid, particle diameter is 1-1000nm, and concentration is 0.01-2nmoL, and the lucifuge reaction time is 2-24 hour.
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| CN108176846B (en) * | 2017-12-21 | 2020-11-10 | 青岛大学 | Method for preparing purified polypeptide or PEG modified gold nanoparticles without centrifugation |
| CN110496232B (en) * | 2019-09-06 | 2020-11-17 | 西安电子科技大学 | Magnetic-gold dimer multifunctional nano probe and preparation method and application thereof |
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| KR100862973B1 (en) * | 2007-06-28 | 2008-10-13 | 연세대학교 산학협력단 | Cationic magnetic nanocomposite for magnetic targeted drug delivery and contrast agent |
| CN102766191B (en) * | 2012-07-31 | 2013-12-25 | 上海交通大学 | Simple magnetic particle functionally-modifying method |
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