CN1974081A - Process of preparing phospholipid modified nanometer silver grain - Google Patents
Process of preparing phospholipid modified nanometer silver grain Download PDFInfo
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- CN1974081A CN1974081A CN 200610118119 CN200610118119A CN1974081A CN 1974081 A CN1974081 A CN 1974081A CN 200610118119 CN200610118119 CN 200610118119 CN 200610118119 A CN200610118119 A CN 200610118119A CN 1974081 A CN1974081 A CN 1974081A
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Abstract
The present invention relates to nanometer technology, and is process of preparing phospholipid modified nanometer silver grain. The present invention prepares biocompatible phospholipid modified nanometer silver grain with silver nitrate as material, and through reduction of sodium borohydride to form nanometer Ag grain of 1-2 nm size, and the subsequent adding phospholipid with mercapto group for metal and sulfur to reaction, so as to form the nanometer dispersed system. The present invention has simple process and high controllability, and provides one excellent experiment platform for developing and utilizing bioactive nanometer functional material.
Description
Technical field
The present invention relates to a kind of method of field of nanometer technology, specifically, that relate to is a kind of preparation method of phospholipid modified silver nano-grain.
Background technology
Precious metals silver is one of research object the most ancient in the modern scientific research.In recent years, along with the fast development of nanoscale science and technology, the research of metal nanoparticle has also obtained great successes, has a extensive future.Silver nano-grain is one of stabilized nano particle the most in the metal nanoparticle, behavior and performance with many uniquenesses, physical propertys (comprising quantum size effect) such as the growth behavior of the self assembly behavior of for example various interfaces, individual particle, the electricity relevant, light, magnetic, and their application in living things catalysis and biomedical engineering with size.The development of these research fields will bring the great revolution of whole nano science, also will provide of paramount importance basic factors of new century for human society simultaneously.Nanoscale based on nano particle, scientific research person is revealed more and more keen interest for the application table of the nano particle of modifying with biomolecule, and especially they are in the application in nano structure functional material and electricity, light, magnetic and bio-sensing device field.In order to obtain the stable biomolecule and the combination of nano particle, need to satisfy two crucial requirements.At first, size, shape is controlled and disperse the metal nanoparticle aqueous solution of homogeneous to help forming the combination of biomolecule and nano particle, and the existence of colloidal particles is quite necessary for the stable of biological combination.Based on this purpose, the mercaptan chemistry is introduced into and continues and uses.Another key element then is that for example enzyme, antigen, antibody, ribonucleic acid and acceptor keep their biologically active in the assembling of nano grain surface to the control biomolecule simultaneously.For example, as the base unit of material synthesis system, ribonucleic acid successfully is used for detecting attached to nano-material surface.
People can prepare the nano-colloid particle of silver by several different methods, but the nano particle that utilizes biomolecule modification silver nano-grain to prepare biologically active still rarely has report.Obviously, the Nano silver grain of this biologically active will have important application prospects in biological and field of nanometer technology.
Find through literature search prior art, Sung-Hee Park etc. are at " Colloids andSurfaces, B:Biointerfaces " (" colloid and interface, B: bioelectric interface ") delivered " Effects of silver nanoparticles on the fluidityof bilayer in phospholipid liposome " (silver nano-grain is to the influence of phospholipid liposome bilayer flowability) on the 117th to 122 page of the 44th phase in 2005, this article proposes the method for silver nano-grain absorption liposome, concrete grammar is for to be dissolved in phosphatide in the chloroform, the toluene solution that adds silver nano-grain, remove chloroform and toluene by rotary distillation method and vacuum drying, obtain containing the immobilized artificial membrane of silver nano-grain, and posthydrolysis and abundant stirring promptly get the silver nano-grain that adsorbs phosphatide.Its deficiency is that no stable chemical bond connects between silver nano-grain and the phosphatide, makes this structure not have biological and chemical stability.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of phospholipid modified silver nano-grain is provided, make it utilize this biologically active bodies of phosphatide to disperse and stable silver nano-grain, prepare phospholipid modified silver nano-grain, satisfy the needs in different application field.
The present invention is achieved by the following technical solutions, and the present invention is raw material with the silver nitrate, by the reduction of sodium borohydride, forms the silver nano-grain of 1 to 2 nanometer.Add the phosphatide that has sulfydryl then,, form the stabilized nano dispersion, can prepare novel phospholipid thus and modify silver nano-grain with biocompatibility by the effect between metal and the sulphur.
Below by step the preparation method of the phospholipid modified silver nano-grain of the present invention is described, specific as follows:
Step a: in flask, add the silver nitrate and the 10-100 ml pure water of 1-10 milligram, be mixed with solution, add the excessive phosphatide that has sulfydryl then, at room temperature stir fully.The concentration of phosphatide should be 10 times of silver nitrate concentration, and fully stirring is to be homogeneous system in order to ensure solution.
Step b: dropwise add the solution of 0.001 mol that contains 1-10 milligram sodium borohydride in the flask, continue to stir, obtain the solution of the phospholipid modified silver nano-grain of homogeneous.With solution centrifugation in the high speed rotary centrifuge, remove supernatant liquor and add pure water and continue to stir, and then centrifugation in centrifuge, remove supernatant liquor.This centrifugal process repeated several times, room temperature vacuum drying 10-30 hour obtains phospholipid modified silver nano-grain.
The pattern of phospholipid modified silver nano-grain can be analyzed with transmission electron microscope, and uv-vis spectra, infrared spectrum and granularmetric analysis etc. can be used as the assistant analysis means.
The silver nano-grain that novel phospholipid produced according to the present invention is modified, its simple synthetic method, technology is simple, controllability good, satisfies the needs in different application field, for the functionalized nano particle of development and use biologically active provides a kind of excellent experimental platform.This is a kind of new method that goes on foot the silver nano-grain of synthetic phospholipid modification at aqueous phase two.Experiment shows, by transmission electron microscope observation to the size of phospholipid modified silver nano-grain be increased to 8 nanometers by 2 nanometers, the size of thickness just in time matches with the size of phospholipid bilayer, has proved that phospholipid bilayer has been connected the surface of silver nano-grain by silver-colored sulfide linkage.The bands of a spectrum of infrared spectrum silver sulfide linkage vibration change, and near the absorption intensity variation of the ultraviolet spectra that is caused by the 4d-5sp electron transition 200 nanometers, have all correspondingly proved this modification.
Description of drawings
Fig. 1 a: the transmission electron microscope figure of the silver nano-grain before phospholipid modified.
Fig. 1 b: the transmission electron microscope figure of the silver nano-grain after phospholipid modified.
Fig. 2: the ultraviolet-visible spectrogram of the silver nano-grain of phospholipid modified front and back.
Fig. 3 a: the infrared spectrogram (3100-2700cm of the silver nano-grain of phospholipid modified front and back
-1).
Fig. 3 b: the infrared spectrogram (1500-1300cm of the silver nano-grain of phospholipid modified front and back
-1).
Fig. 3 c: the infrared spectrogram (1350-900cm of the silver nano-grain of phospholipid modified front and back
-1).
Fig. 3 d: the infrared spectrogram (900-640cm of the silver nano-grain of phospholipid modified front and back
-1).
The specific embodiment
Following examples are that concrete enforcement of the present invention is further specified, rather than limit the scope of the invention.
Embodiment 1
With the silver nitrate is initial raw material, through the reduction generation silver nano-grain of sodium borohydride, with the phosphatide reaction that has sulfydryl, prepares phospholipid modified silver nano-grain by the interaction between silver and the sulphur again.
Step a: in flask, add 1.70 milligrams silver nitrate and 10 ml pure waters, be mixed with the solution of 0.001 mol, add the excessive phosphatide that has sulfydryl then, at room temperature fully stir.The concentration of phosphatide is 10 times of silver nitrate concentration, i.e. 0.01 mol.Mixing time is 2 hours, guarantees that solution becomes homogeneous system.
Step b: dropwise adding the concentration that contains 5 milligrams of sodium borohydrides in the flask is the solution of 0.001 mol, continues to stir 48 hours, obtains the solution of the phospholipid modified silver nano-grain of homogeneous.Taking out solution is centrifugation 1 hour in 13000 rev/mins the centrifuge at rotating speed, removes supernatant liquor.Add 10 ml pure waters and continue to stir 24 hours, supernatant liquor is removed in centrifugation 1 hour in 13000 rev/mins centrifuge then.This centrifugal process repeats 2 to 3 times, and room temperature vacuum drying 24 hours obtains phospholipid modified silver nano-grain.
Embodiment 2
With the silver nitrate is initial raw material, through the reduction generation silver nano-grain of sodium borohydride, with the phosphatide reaction that has sulfydryl, prepares phospholipid modified silver nano-grain by the interaction between silver and the sulphur again.
Step a: in flask, add 1 milligram silver nitrate and 10 ml pure waters, be mixed with the solution of 0.0006 mol, add the excessive phosphatide that has sulfydryl then, at room temperature fully stir.The concentration of phosphatide is 10 times of silver nitrate concentration, i.e. 0.006 mol.Mixing time is 2 hours, guarantees that solution becomes homogeneous system.
Step b: dropwise adding the concentration that contains 1 milligram of sodium borohydride in the flask is the solution of 0.001 mol, continues to stir 48 hours, obtains the solution of the phospholipid modified silver nano-grain of homogeneous.Taking out solution is centrifugation 1 hour in 13000 rev/mins the centrifuge at rotating speed, removes supernatant liquor.Add 10 ml pure waters and continue to stir 24 hours, supernatant liquor is removed in centrifugation 1 hour in 13000 rev/mins centrifuge then.This centrifugal process repeats 2 to 3 times, and room temperature vacuum drying 10 hours obtains phospholipid modified silver nano-grain.
Embodiment 3
With the silver nitrate is initial raw material, through the reduction generation silver nano-grain of sodium borohydride, with the phosphatide reaction that has sulfydryl, prepares phospholipid modified silver nano-grain by the interaction between silver and the sulphur again.
Step a: in flask, add 10 milligrams silver nitrate and 100 ml pure waters, be mixed with the solution of 0.0006 mol, add the excessive phosphatide that has sulfydryl then, at room temperature fully stir.The concentration of phosphatide is 10 times of silver nitrate concentration, i.e. 0.006 mol.Mixing time is 2 hours, guarantees that solution becomes homogeneous system.
Step b: dropwise adding the concentration that contains 10 milligrams of sodium borohydrides in the flask is the solution of 0.001 mol, continues to stir 48 hours, obtains the solution of the phospholipid modified silver nano-grain of homogeneous.Taking out solution is centrifugation 1 hour in 13000 rev/mins the centrifuge at rotating speed, removes supernatant liquor.Add 10 ml pure waters and continue to stir 24 hours, supernatant liquor is removed in centrifugation 1 hour in 13000 rev/mins centrifuge then.This centrifugal process repeats 2 to 3 times, and room temperature vacuum drying 30 hours obtains phospholipid modified silver nano-grain.
Embodiment the results are shown in accompanying drawing.Fig. 1 a has provided the silver nano-grain figure for preparing through reduction, as can be seen from the figure about 2 nanometers of their average diameter.Fig. 1 b has provided the silver nano-grain figure after phospholipid modified, and clearly, the average diameter of particle increases to 8 nanometers after the finishing.The particle size data show that in order to form the spherical particle of 8 nanometers, the actual (real) thickness of phospholipid layer should be 3 nanometers.Consider the size of phospholipid molecule self and the situation that phosphatide forms liposome, the spherical particle structure explanation of 8 nanometers, phosphatide is with the surface of bilayer structure attached to silver nano-grain, and the interaction between phosphatide and the silver simultaneously realizes by thiol functionalities.Fig. 2 has provided the ultraviolet-visible spectrogram of silver nano-grain in phospholipid modified front and back, because the electron transition of 4d-5sp in the silver atoms structure causes the wavelength absorption of phospholipid modified silver nano-grain about 200 nanometers to disappear.Fig. 3 a-d has provided the infrared spectrogram of the silver nano-grain of phospholipid modified front and back, and what marked is the series of features bands of a spectrum of phosphatide, and 2957 in the bands of a spectrum, 2918,2850,1468,1416,1378,1285,1260,1245,1170,721cm
-1The change of absorption peak strength of position has proved that also phosphatide has been grafted to the surface of silver nano-grain by silver-colored sulfide linkage, makes to become more stable through phospholipid modified silver nano-grain.
Claims (5)
1. the preparation method of a phospholipid modified silver nano-grain, it is characterized in that, with the silver nitrate is raw material, reduction by sodium borohydride, form the silver nano-grain of 1 to 2 nanometer, add the phosphatide that has sulfydryl then, by the effect between metal and the sulphur, form the stabilized nano dispersion, preparation has the phospholipid modified silver nano-grain of biocompatibility thus.
2. the preparation method of phospholipid modified silver nano-grain according to claim 1 is characterized in that, may further comprise the steps:
Step a: in flask, add the silver nitrate and the 10-100 ml pure water of 1-10 milligram, be mixed with solution, add the excessive phosphatide that has sulfydryl then, at room temperature stir fully;
Step b: the solution that dropwise adds 0.001 mol that contains 1-10 milligram sodium borohydride in the flask, continue to stir, obtain the solution of the phospholipid modified silver nano-grain of homogeneous, with solution centrifugation in centrifuge, remove supernatant liquor and add pure water and continue to stir, and then centrifugation in centrifuge, remove supernatant liquor, this centrifugal process repeated several times, the room temperature vacuum drying obtains phospholipid modified silver nano-grain.
3. the preparation method of phospholipid modified silver nano-grain according to claim 2 is characterized in that among the step a, the concentration of phosphatide is 10 times of silver nitrate concentration.
4. the preparation method of phospholipid modified silver nano-grain according to claim 2 is characterized in that among the step b, the room temperature vacuum drying time is 10-30 hour.
5. the preparation method of phospholipid modified silver nano-grain according to claim 2 is characterized in that, among the step b, and described centrifuge, adopting rotating speed is 13000 rev/mins centrifuge.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102294492A (en) * | 2011-08-04 | 2011-12-28 | 翔瑞（泉州）纳米科技有限公司 | Polymer surface protection monodisperse nano silver particle and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102294492A (en) * | 2011-08-04 | 2011-12-28 | 翔瑞（泉州）纳米科技有限公司 | Polymer surface protection monodisperse nano silver particle and preparation method thereof |
| CN102294492B (en) * | 2011-08-04 | 2013-11-20 | 翔瑞（泉州）纳米科技有限公司 | Polymer surface protection monodisperse nano silver particle and preparation method thereof |
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