CN105436516B - The preparation method of the high photon absorbing intensity racemosus shape colloid gold nanoparticle of controllable grain size - Google Patents
The preparation method of the high photon absorbing intensity racemosus shape colloid gold nanoparticle of controllable grain size Download PDFInfo
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Abstract
The present invention relates to nano material exploitation and application fields, disclose a kind of method of the racemosus shape colloid gold nanoparticle for the high photon absorbing intensity that different-grain diameter size is synthesized by colloid gold seeds mediating growth.First using conventional trisodium citrate reduction method, by the Au in gold chloride molecule3+It is reduced into Au0, obtain spherical shape colloid gold seeds.Then colloid gold seeds are added in into a kind of growth-promoting media, the main component of the growth-promoting media includes the solution such as ultra-pure water, gold chloride and trisodium citrate, it is slowly stirred on magnetic stirring apparatus, 50 DEG C are heated to after solution mixing, it revs up at this time, while disposably adds in enough quinol solutions, mixed solution temperature maintains 50 DEG C, stop heating after the reaction was continued 10min, be cooled to room temperature the racemosus shape colloidal gold solution for obtaining high photon absorbing intensity.The method of the present invention has easy to operate, and flow is simple, is swift in response, the features such as controllability is good, repeatability is high.
Description
Technical field
The present invention relates to nano material exploitations and the exploitation of noble metal nano particles in application field, are specifically related to one kind
Different-grain diameter size, the side of the racemosus shape colloid gold nanoparticle of high photon absorbing intensity are synthesized by colloid gold seeds mediating growth
Method.
Background technology
Colloidal gold (colloid gold) is also referred to as nanogold (nanogold), refers to dispersed phase particles diameter in 1-150nm
Between aurosol, belong to multiphase heterogeneous system.Colloid gold particle is by the golden core (Au atoms) in a basis and is enclosed in outer pair
Sheath is formed, as shown in Figure 1, it is internal layer anion to be close on golden core surface, outer layer sheath is then dispersed in colloidal solution
In, with the suspension state that colloidal gold is maintained to be free between colloidal sol.Colloidal gold solution color depend on nanogold granular size,
Particle shape shape and GOLD FROM PLATING SOLUTION particle monodispersity etc..In spherical or ellipsoid gold particle, minimum colloidal gold (2~5nm)
It is orange-yellow, medium sized colloidal gold (10~20nm) is claret, and the colloidal gold (30~80nm) of larger particles is then
It is aubergine.The irregular colloidal gold particle of some grain shapes then shows purple, blue and bluish violet etc..Colloidal gold
Have a series of unique photoelectricity characteristics, as (1) electrostatic it is mutually exclusive bring extremely strong chemistry and mechanical stability；
(2) significant photoelectricity physical characteristic；(3) it is easy to surface-functionalized；(4) surface plasma resonance effect；(5) special catalysis
Activity；(6) non-toxic, bio-compatibility；(7) it is anti-oxidant, crystallizable；(8) it is easily-synthesized and form is controllable；(9) good particle
Dispersibility etc..Wherein, stiff stability and significant photoelectricity characteristic are the most important property of colloidal gold.In addition, the property of colloidal gold
Matter is largely vulnerable to the influence of external condition, such as the hairs such as granular size, shape, solution ph and configuration of surface
The change of its property can be caused during changing.In recent years since, it is deep that the characteristic of colloidal gold obtains vast researchers
Research, while also attempt to open up new method to improve the characteristic of nanogold.
Application of the colloidal gold in immunochemistry is otherwise known as Immuno gold (immunogold).Colloid gold label
(Immunogold labeling) is substantially the coating that the macromolecules such as antibody protein are adsorbed to colloid gold particle surface
Journey, adsorption mechanism may be：(1) gold particle surface is negatively charged, and protein surface is positively charged, and the two is mutual by electrostatic attraction
Attract, reach and firm combine is formed in the range of Van der Waals force；(2) albumen by certain amino acid residues include tryptophan with
The hydrophobic adsorbent effect on gold particle surface；(3) it is covalent by coordinate bond between the sulfydryl of the cysteine in albumen and gold particle
With reference to.Gold particle is mainly utilized with high electronics in immuno-gold labeling technology (Immunogold labeling technique)
The characteristic of density, at gold mark protein binding, visible dark brown coloured particles under microscope, when these markers are in corresponding ligand
When place largely assembles, it may appear that the clearly visible red of naked eyes or pink spot, thus can be used for qualitative or sxemiquantitative quick
Immune detection, this reaction can also be amplified by the deposition of Argent grain, referred to as immunogold silver staining.Electronic Speculum is horizontal at present
Immuno-gold staining (IGS), the dot immunogold dyeing skill of the immunogold silver staining (IGSS) of light microscopic level and macroscopic level
Art has become the powerful of scientific research and clinical diagnosis.In addition, colloidal gold is in flow cytometer, immunoblot assay,
Also have in immunochromatography quick diagnosis technology and be widely applied very much, it is contemplated that with the continuous development of nanometer technology, colloidal gold
Will increasingly it be paid attention to by Related Research Domain.
It is well known that the unique photoelectricity characteristic of colloidal gold depends not only on the size of its particle size, Er Qieyu
Its grain shape and GOLD FROM PLATING SOLUTION particle concentration are closely related.Along with the variation of gold nanoparticle shape, its own each
Kind physicochemical property such as surface plasma resonance absorbtion peak (surface plasmon resonance absorption band,
SPR) and molar extinction coefficient (extinction coefficient) also accordingly changes a lot.Research shows that with normal
It advises spherical nanogold (particle diameter is about 20-40nm) to compare, racemosus shape nanogold has a series of unique advantages, such as racemosus
The surface plasma resonance absorbtion peak (λ max) of shape nanogold will appear apparent red shift while have higher Molar Extinction system
Several, stronger Surface enhanced Raman scattering (surface enhance Raman scattering, SERS) activity and more
Significant surface plasma resonance effect, the main reason for this phenomenon is caused to occur are because in racemosus shape nanogold particle table
Stronger local electromagnetic field is dispersed on the furcella in face.The scientific research personnel such as Ji Yanwei prepare grain size as 75nm using seed mediated growth method
Racemosus shape Au colloidal nanoparticles, realized by the use of it as label probe structure racemosus shape colloidal gold immuno-chromatography test paper strip to big
The quantitative detection of aflatoxin (AFB1) in the crops such as rice.The experimental results showed that with conventional spherical nanogold immunochromatography
Test strips are compared, and in terms of detection sensitivity, racemosus shape colloidal gold immune chromatography test obtains the raising more than 10 times.Existing kind
Sub- mediating growth method is prepared for racemosus shape Au colloidal nanoparticles.Colloid gold seeds are synthesized first with trisodium citrate reduction method
Solution, then using colloid gold seeds as core, by the i.e. gold atom selectivity of core surface anisotropy growth in colloid gold seeds
Surface deposits, and forms racemosus shape Au colloidal nanoparticles.This method is disadvantageous in that the racemosus shape colloidal gold solution of its synthesis
Middle gold particle concentration is relatively low, and the photon absorbing intensity of solution itself is very weak, caused the result is that being first had to during use to glue
Body gold solution carries out concentration to improve its photon absorbing intensity, and solution pretreatment process not only increases workload, and significantly
Waste human and material resources and financial resources.
Invention content
The present invention provides it is a kind of it is more simpler than existing method, the more rapid, controllability of reaction is more preferable, repeatability higher
By colloid gold seeds mediating growth synthesize different-grain diameter size, the racemosus shape colloid gold nanoparticle of high photon absorbing intensity
Method.
Specifically technical scheme of the present invention comprises the steps of：
The high photon absorbing intensity racemosus shape colloid gold nanoparticle of controllable grain size, synthetic method include the following steps：(1) ball
The synthesis of shape colloidal gold seed solution：Using classical trisodium citrate reduction method, 1mL 1%HAuCl are accurately pipetted4Solution is extremely
It is slowly stirred in the conical flask for filling 99mL ultra-pure waters, on magnetic stirring apparatus and is heated to boiling, revved up at this time and rapidly
It is disposable to add in 2.7mL 1%Na3C6H5O7Solution continues the 15min that boils, treats that solution colour becomes claret and no longer sends out
Changing stops heating, and at the uniform velocity stirring is cooled to room temperature to get the spherical shape colloidal gold seed solution to grain size for 18 ± 2nm
That is spherical shape colloidal gold seed solution；
(2) particle size is the preparation of 33 ± 3nm high photon absorbing intensity racemosus shape Au colloidal nanoparticles：It accurately pipettes above-mentioned
In spherical shape colloidal gold seed solution 9mL to growth-promoting media, the growth-promoting media is by ultra-pure water 100mL, 1%HAuCl4Solution 1.2mL,
1%Na3C6H5O7Solution 2.64mL is formed；It is slowly stirred on magnetic stirring apparatus, 50 DEG C is heated to after mixing, is revved up at this time,
Rapid disposable simultaneously to add in 30mmol/L quinol solution 24mL, solution temperature maintains 50 DEG C, the reaction was continued 10min, stops
It only heats, is cooled to room temperature and obtains particle size as 33 ± 3nm high photon absorbing intensity racemosus shape Au colloidal nanoparticles solution, 4
It DEG C saves backup.
Particle size is the preparation of 68 ± 2nm high photon absorbing intensity racemosus shape Au colloidal nanoparticles：It is accurate with liquid-transfering gun first
It really pipettes in above-mentioned spherical shape colloidal gold seed solution 6mL to growth-promoting media, the growth-promoting media is by ultra-pure water 100mL, 1%HAuCl4It is molten
Liquid 1.2mL, 1%Na3C6H5O7Solution 2.64mL is formed；It is slowly stirred on magnetic stirring apparatus, 50 DEG C is heated to after mixing, at this time
It revs up, while rapid disposable addition 30mmol/L quinol solution 24mL, solution temperature maintain 50 DEG C, the reaction was continued
10min stops heating, is cooled to room temperature the racemosus shape colloidal gold solution for obtaining that particle size is 68 ± 2nm high photon absorbing intensities.
Particle size is the preparation of 88 ± 4nm high photon absorbing intensity racemosus shape Au colloidal nanoparticles：It is accurate with liquid-transfering gun first
It really pipettes in above-mentioned spherical shape colloidal gold seed solution 6mL to growth-promoting media, the growth-promoting media is by ultra-pure water 100mL, 1%HAuCl4It is molten
Liquid 1.2mL, 1%Na3C6H5O7Solution 2.64mL is formed；It is slowly stirred on magnetic stirring apparatus, 50 DEG C is heated to after mixing, at this time
It revs up, while rapid disposable addition 30mmol/L quinol solution 24mL, solution temperature maintain 50 DEG C, the reaction was continued
10min stops heating, is cooled to room temperature and obtains particle size as 88 ± 4nm, high photon absorbing intensity racemosus shape colloid gold nano
Grain solution.
Signified room temperature refers generally to 0-35 DEG C herein.
Racemosus shape colloid gold nanoparticle the invention further relates to above-mentioned high photon absorbing intensity is analyzed in immuno-chromatographic test paper strip
Above-mentioned racemosus shape colloid gold nanoparticle and antibody are passed through Electrostatic Absorption, hydrophobic effect or Van der Waals force by the application in detection
It carries out coupling and prepares gold labeling antibody nano-probe, then realized by the specific reaction of antigen in immunology and antibody to be checked
The detection of substance.
Inventor has synthesized spherical colloid gold with trisodium citrate reduction method and seed mediating growth method respectively, and short furcella is more
Dendritic colloidal gold and long furcella racemosus shape colloid gold nanoparticle, particle diameter is 30-40nm, is used as label probe
It is more that spherical nanogold immuno-chromatographic test paper strip, short furcella racemosus shape colloidal gold immuno-chromatography test paper strip and long furcella are constructed respectively
Dendritic colloidal gold immuno-chromatography test paper strip, it is target molecule to select ochratoxin (OTA), is realized using Immunological Mode is competed
To the Quantitative detection of OTA.Experimental result again shows that, for more spherical nanogold immuno-chromatographic test paper strip, either exists
In terms of detection sensitivity or in terms of the material consumptions such as antibody needed for individual test strips, the examination of racemosus shape colloidal gold immunochromatographimethod
Paper slip all shows very significant superiority.On the one hand, racemosus shape colloidal gold immuno-chromatography test paper strip is improved more than 4 times
Sensitivity；On the other hand, individual test strips antibody consumption amount of racemosus shape colloidal gold immuno-chromatography test paper strip is only spherical colloid
20% or so of golden immuno-chromatographic test paper strip, is greatly saved material.Experimental result is also shown, in immuno-chromatographic test paper strip
On, racemosus shape colloidal gold has stronger affinity with the gold labeling antibody nano-probe that antibody coupling is formed and antigen, simultaneously also
Have faster capillary and spring up rate, greatly reduce detection time.Result above is explainable to be based on racemosus shape
The more unique optical characteristics of colloid gold nanoparticle is used as label probe and substitutes traditional spherical colloid gold, not only has
Conducive to the sensitivity for improving immuno-chromatographic test paper strip, and from the point of view of cost, cost can greatly be reduced, this for
For large batch of industrialized production, meaning is undoubtedly very great.
At the same time, colloidal gold particle concentration has certain decisive role, high extinction to its optical characteristics in solution
The colloidal gold solution of intensity possesses significantly more photon absorbing intensity (optical density), and inventor utilizes seed mediation life
Regular way synthesizes two kinds of racemosus shape colloidal gold solutions by adjusting the proportion of colloid gold seeds in growth-promoting media, passes through ultraviolet spectrometry light
Degree measurement examination, photon absorbing intensity are respectively 0.2 and 1.0, are applied to immuno-chromatographic test paper strip, experiment knot as label probe
Fruit shows either in terms of the sensitivity or in terms of individual test strips material consumption, the colloid gold immune layer of high photon absorbing intensity
Analysing test strips has better detection performance.
Existing seed mediating growth method is prepared for racemosus shape Au colloidal nanoparticles.First with trisodium citrate reduction method
Colloid gold seeds solution is synthesized, is gold atom selectivity by the growth of core surface anisotropy then using colloid gold seeds as core
Colloidal gold the surface of the seed deposit, formed racemosus shape Au colloidal nanoparticles.This method is disadvantageous in that the more of its synthesis
Gold particle concentration is relatively low in dendritic colloidal gold solution, and the photon absorbing intensity of solution itself is very weak, caused the result is that in the mistake used
It first has to carry out concentration to colloidal gold solution to improve its photon absorbing intensity in journey, solution pretreatment process not only increases work
It measures, and greatly wastes human and material resources and financial resources.
The racemosus shape colloid gold nanoparticle for the high photon absorbing intensity that the present invention is synthesized by colloid gold seeds mediating growth has
Effect compensates for the shortcomings that conventional colloidal gold light absorption value is on the weak side, this is either for scientific research or industrialized production, all
It is significantly.
Technical solution of the present invention has the following advantages that：
1st, the racemosus shape colloidal gold solution photon absorbing intensity of the high photon absorbing intensity of the present invention program synthesis is high, and can direct plunge into makes
With, need not move through concentration etc. pre-treatment steps.The method of the present invention is easy to operate, and flow is simple.By can hot type magnetic agitation
Device can directly synthesize different-grain diameter size, the racemosus shape colloid gold nano of high photon absorbing intensity by colloid gold seeds mediating growth
Particle.
2nd, the method for the present invention reaction time is short, and speed is fast.Time-consuming 10min can obtain the racemosus shape colloid of high photon absorbing intensity
Gold solution greatly improves reaction rate, shortens the reaction time.
3rd, the method for the present invention controllability is good, can realize the controlledly synthesis to racemosus shape nanogold particle size.Pass through
The proportion of colloidal gold seed solution is adjusted, (30-100nm) of different-grain diameter size, the racemosus shape glue of high photon absorbing intensity can be obtained
Body gold solution.The racemosus shape colloidal gold solution particle monodispersity of prepared high photon absorbing intensity is good, and nano-particle is in solution
In be uniformly distributed, without wadding collection, size uniformity.
4th, the method for the present invention repeatability is high.The racemosus shape colloidal gold solution repeatability that this method synthesizes high photon absorbing intensity is high, respectively
The Au colloidal nanoparticles particle size coefficient of variation is less than 10% between batch.
Description of the drawings
Fig. 1 colloidal gold seed grain structure charts of the present invention；
The ultraviolet characterization collection of illustrative plates of racemosus shape colloid gold particle of Fig. 2 colloid gold seeds of the present invention and different-grain diameter；
The racemosus shape colloid gold particle transmission electron microscope picture of Fig. 3 colloid gold seeds of the present invention and different-grain diameter；
Specific embodiment
In order to which the present invention is more clearly understood, with reference to embodiments, the present invention will be described in further detail.It should
Work as understanding, specific embodiment described herein only to explain the present invention, is not intended to limit the present invention.
Solution is prepared：1st, 1%HAuCl4Solution：1.0g gold chloride powder is dissolved in ultra-pure water, is added until completely dissolved
Ultra-pure water is settled to 100mL, is made into the aqueous solution of final concentration of 1% (w/v).Prepared chlorauric acid solution is stored
In brown reagent bottle, 4 DEG C save backup.2nd, 1%Na3C6H5O7Solution：Accurately weigh 1.0g two citric acid monohydrate trisodiums solids
Powder is dissolved in ultra-pure water, and until completely dissolved plus ultra-pure water is settled to 100mL, is made into the water-soluble of final concentration of 1% (w/v)
Liquid, through 0.22 μm of membrane filtration, 4 DEG C save backup.3rd, 30mmol/L quinol solutions：Accurately weigh 330mg hydroquinones
Solid powder is dissolved in ultra-pure water, and until completely dissolved plus ultra-pure water is settled to 100mL, is made into final concentration of 30mmol/L's
Aqueous solution, through 0.22 μm of membrane filtration, 4 DEG C save backup.
1 particle size of embodiment be 33 ± 3nm, the preparation of high photon absorbing intensity racemosus shape Au colloidal nanoparticles
It is the spherical shape colloid gold nanoparticle of 18 ± 2nm for seed using grain size：
(1) synthesis of spherical shape colloidal gold seed solution (spherical shape colloid gold nanoparticle)：Using classical citric acid
Three sodium reductions accurately pipette 1mL 1%HAuCl4In solution to the conical flask for filling 99mL ultra-pure waters, delay on magnetic stirring apparatus
Slowly boiling is heated with stirring to, revs up at this time and rapid disposable adds in 2.7mL 1%Na3C6H5O7Solution continues to boil
15min treats that solution colour becomes claret and no longer changes, stop heating, at the uniform velocity stirring be cooled to room temperature to get to
Grain size is the spherical shape colloidal gold seed solution (Fig. 3 A) of 18 ± 2nm.Such as Fig. 2, after measured its maximum surface plasma resonance suction
Receipts wavelength is 520nm, and maximum photon absorbing intensity (OD) saves backup for 0.9,4 DEG C.
(2) preparation of high photon absorbing intensity racemosus shape Au colloidal nanoparticles：Above-mentioned ball is accurately pipetted with liquid-transfering gun first
In shape colloidal gold seed solution 9mL to growth-promoting media, the growth-promoting media is by ultra-pure water 100mL, 1%HAuCl4Solution 1.2mL, 1%
Na3C6H5O7Solution 2.64mL is formed；It is slowly stirred on magnetic stirring apparatus, 50 DEG C is heated to after mixing, is revved up at this time, together
When disposably add in 30mmol/L quinol solution 24mL rapidly, solution temperature maintains 50 DEG C, the reaction was continued 10min, stops
Heating, be cooled to room temperature obtain particle size be 33 ± 3nm high photon absorbing intensities racemosus shape colloidal gold solution (Fig. 3 B), 4 DEG C
It saves backup.
(3) preparation of conventional racemosus shape Au colloidal nanoparticles (the racemosus shape colloidal gold of low photon absorbing intensity)：First with shifting
Liquid rifle is accurately pipetted in above-mentioned spherical shape colloidal gold seed solution 2mL to growth-promoting media, and the growth-promoting media is by ultra-pure water 100mL, 1%
HAuCl4375 μ L of solution, 1%Na3C6H5O7220 μ L of solution are formed；Quick stirring, the rapid disposable 30mmol/L that adds in is to benzene two
Phenol solution 1mL, the reaction was continued 30min obtain particle size as 33 ± 3nm, the racemosus shape colloidal gold solution of low photon absorbing intensity, and 4
It DEG C saves backup.
By ultraviolet specrophotometer, to the above-mentioned high photon absorbing intensity prepared and conventional racemosus shape colloidal gold solution into
Row characterization, 500 μ L high photon absorbing intensities and low photon absorbing intensity racemosus shape colloidal gold solution to two colorimetrics are pipetted with liquid-transfering gun respectively
In ware, by ultraviolet specrophotometer instrument, scanned under the conditions of wavelength 450-750nm, under the same terms, high photon absorbing intensity racemosus
The photon absorbing intensity of shape colloidal gold solution is 0.9, and the photon absorbing intensity of low photon absorbing intensity racemosus shape colloidal gold solution is only 0.2.
Embodiment 2 is based on high photon absorbing intensity and low photon absorbing intensity racemosus shape Au colloidal nanoparticles immuno-chromatographic test paper strip
Structure
Using ochratoxin (OTA) as analyte, using Competitive assays pattern.Test strips are by sample pad, bonding pad, nitre
Acid cellulose film, blotting paper and polyvinyl chloride bottom plate form, and coating ochratoxin antigen and donkey resist on nitrocellulose filter
Mouse secondary antibody is respectively as detection line (T) and nature controlling line (C)：
(1) grain size be 33 ± 3nm, the structure of high photon absorbing intensity racemosus shape Au colloidal nanoparticles immuno-chromatographic test paper strip：
Using grain size as 33 ± 3nm, the high photon absorbing intensity racemosus shape Au colloidal nanoparticles (racemosus of the 1 high photon absorbing intensity of gained of Example
Shape colloidal gold solution, does not do concentration) as marker material, the effects that passing through Electrostatic Absorption power and anti-ochratoxin Dan Ke
Grand antibody coupling (antibody label concentration is 4.5 μ g/mL colloidal gold solutions), obtains colloidal gold and antibody nano-probe compound,
Compound is coated on bonding pad by spraying film instrument, assembles test strips.
(2) grain size be 33 ± 3nm, the structure of low photon absorbing intensity racemosus shape Au colloidal nanoparticles immuno-chromatographic test paper strip：
Using the above-mentioned grain size prepared as 33 ± 3nm, (1 gained of Example is low for low photon absorbing intensity racemosus shape Au colloidal nanoparticles
Photon absorbing intensity racemosus shape Au colloidal nanoparticles, do not do concentration) as marker material, the effects that passing through Electrostatic Absorption power with
Anti- ochratoxin monoclonal antibody coupling (antibody label concentration is 4.5 μ g/mL colloidal gold solutions), obtains colloidal gold and antibody
Compound is coated on bonding pad by nano-probe compound by spraying film instrument, assembles test strips.
(3) high photon absorbing intensity and the comparison of low photon absorbing intensity racemosus shape colloidal gold immuno-chromatography test paper strip detection performance：
Ensure anti-ochratoxin labeling of monoclonal antibody concentration, colloidal gold and antibody nano-probe compound consumption, cellulose nitrate
Under conditions of the conditions such as detection line antigen concentration and the anti-mouse secondary antibody concentration of donkey are consistent on plain film, read by corresponding colloidal gold
Instrument is taken to carry out interpretation to two kinds of test strips, it is strong come the high extinction of comparison by the band of ELISA test strip line and nature controlling line colour developing situation
The performance of degree and low photon absorbing intensity racemosus shape colloidal gold immuno-chromatography test paper strip.
Instrument (HG-8, Shanghai Huguo Science Instrument Co., Ltd.) is read using colloidal gold, and test strips are carried out with interpretation, experiment
The results show that even if in optimal conditions, low photon absorbing intensity racemosus shape colloidal gold immuno-chromatography test paper strip detection line and nature controlling line
Band reading value be only 66 ± 3 and 60 ± 5, can not meet scientific research and the requirement of industrialized production at all, and high photon absorbing intensity
Racemosus shape colloidal gold immuno-chromatography test paper strip detection line and nature controlling line are respectively provided with very deep colored intensity, band reading value difference
500 ± 15 and 450 ± 25 are can reach, are fully able to the requirement for meeting industrialized production.High photon absorbing intensity racemosus shape colloidal gold is exempted from
Epidemic disease chromatograph test strip has good sensitivity, can reach 0.07ng/ to the minimum detection limit of ochratoxin A in sample
ML, meanwhile, high photon absorbing intensity racemosus shape colloidal gold immuno-chromatography test paper strip also has good accuracy and precision.Racemosus shape glue
Individual test strips antibody consumption amount of body gold immuno-chromatographic test paper strip is only 20% left side of spherical colloid gold immuno-chromatographic test paper strip
The right side is greatly saved material.
On immuno-chromatographic test paper strip, gold labeling antibody nano-probe and antigen that racemosus shape colloidal gold is formed with antibody coupling
It with stronger affinity, while is also equipped with faster capillary and springs up rate, greatly reduce detection time.Result above
It is explainable to be based on the more unique optical characteristics of racemosus shape colloid gold nanoparticle, it is used as label probe and substitutes biography
The spherical colloid gold of system, not only contributes to improve the sensitivity of immuno-chromatographic test paper strip, and from the point of view of cost, can
Cost is significantly reduced, for large batch of industrialized production, meaning is undoubtedly very great for this.
3 particle size of embodiment be 68 ± 2nm, the preparation of high photon absorbing intensity racemosus shape Au colloidal nanoparticles
It is the spherical shape colloid gold nanoparticle of 18 ± 2nm for seed using grain size：
(1) synthesis of spherical shape colloidal gold seed solution (spherical shape colloid gold nanoparticle)：Using classical citric acid
Three sodium reductions accurately pipette 1mL 1%HAuCl4In solution to the conical flask for filling 99mL ultra-pure waters, delay on magnetic stirring apparatus
Slowly boiling is heated with stirring to, revs up at this time and rapid disposable adds in 2.7mL 1%Na3C6H5O7Solution continues to boil
15min treats that solution colour becomes claret and no longer changes, stop heating, at the uniform velocity stirring be cooled to room temperature to get to
Grain size is the spherical shape colloidal gold seed solution (Fig. 3 A) of 18 ± 2nm.Such as Fig. 2, after measured its maximum surface plasma resonance suction
Receipts wavelength is 520nm, and maximum photon absorbing intensity (OD) saves backup for 0.9,4 DEG C.
(2) preparation of high photon absorbing intensity racemosus shape Au colloidal nanoparticles：Above-mentioned ball is accurately pipetted with liquid-transfering gun first
In shape colloidal gold seed solution 6mL to growth-promoting media, the growth-promoting media is by ultra-pure water 100mL, 1%HAuCl4Solution 1.2mL, 1%
Na3C6H5O7Solution 2.64mL is formed；It is slowly stirred on magnetic stirring apparatus, 50 DEG C is heated to after mixing, is revved up at this time, together
When disposably add in 30mmol/L quinol solution 24mL rapidly, solution temperature maintains 50 DEG C, the reaction was continued 10min, stops
Heating, be cooled to room temperature obtain particle size be 68 ± 2nm high photon absorbing intensities the i.e. high extinction of racemosus shape colloidal gold solution it is strong
Racemosus shape Au colloidal nanoparticles solution (Fig. 3 C) is spent, 4 DEG C save backup.
(3) it characterizes：By ultraviolet specrophotometer, to the above-mentioned high photon absorbing intensity racemosus shape colloidal gold solution prepared
It is characterized, is pipetted in 500 μ L high photon absorbing intensity racemosus shape colloidal gold solutions to cuvette with liquid-transfering gun, by ultraviolet spectrometry light
Degree counts instrument, is scanned under the conditions of wavelength 450-750nm, as shown in Fig. 2, the extinction of high photon absorbing intensity racemosus shape colloidal gold solution is strong
It is 0.9 to spend, and maximum surface plasmon resonance absorption wavelength is 610nm.
The racemosus shape colloidal gold solution repeatability that this method synthesizes high photon absorbing intensity is high, Au colloidal nanoparticles between each batch
The particle size coefficient of variation is less than 10%.Equally have significantly in absorbance compared with conventional racemosus shape Au colloidal nanoparticles
Advantage.
5 particle size of embodiment be 88 ± 4nm, the preparation of high photon absorbing intensity racemosus shape Au colloidal nanoparticles
It is the spherical shape colloid gold nanoparticle of 18 ± 2nm for seed using grain size：
(1) synthesis of spherical shape colloidal gold seed solution (spherical shape colloid gold nanoparticle)：Using classical citric acid
Three sodium reductions accurately pipette 1mL 1%HAuCl4In solution to the conical flask for filling 99mL ultra-pure waters, delay on magnetic stirring apparatus
Slowly boiling is heated with stirring to, revs up at this time and rapid disposable adds in 2.7mL 1%Na3C6H5O7Solution continues to boil
15min treats that solution colour becomes claret and no longer changes, stop heating, at the uniform velocity stirring be cooled to room temperature to get to
Grain size is the spherical shape colloidal gold seed solution (Fig. 3 A) of 18 ± 2nm.Such as Fig. 2, after measured its maximum surface plasma resonance suction
Receipts wavelength is 520nm, and maximum photon absorbing intensity (OD) saves backup for 0.9,4 DEG C.
(2) preparation of high photon absorbing intensity racemosus shape Au colloidal nanoparticles：Above-mentioned ball is accurately pipetted with liquid-transfering gun first
In shape colloidal gold seed solution 6mL to growth-promoting media, the growth-promoting media is by ultra-pure water 100mL, 1%HAuCl4Solution 1.2mL, 1%
Na3C6H5O7Solution 2.64mL is formed；It is slowly stirred on magnetic stirring apparatus, 50 DEG C is heated to after mixing, is revved up at this time, together
When disposably add in 30mmol/L quinol solution 24mL rapidly, solution temperature maintains 50 DEG C, the reaction was continued 10min, stops
Heating is cooled to room temperature and obtains particle size as 88 ± 4nm, and racemosus shape colloidal gold solution, that is, high extinction of high photon absorbing intensity is strong
Racemosus shape Au colloidal nanoparticles solution (Fig. 3 D) is spent, 4 DEG C save backup.
(3) it characterizes：By ultraviolet specrophotometer, to the above-mentioned high photon absorbing intensity racemosus shape colloidal gold solution prepared
It is characterized, is pipetted in 500 μ L high photon absorbing intensity racemosus shape colloidal gold solutions to cuvette with liquid-transfering gun, by ultraviolet spectrometry light
Degree counts instrument, is scanned under the conditions of wavelength 450-750nm, and the extinction of high photon absorbing intensity racemosus shape colloidal gold solution as shown in Figure 2 is strong
It is 0.9 to spend, and maximum surface plasmon resonance absorption wavelength is 630nm.
The racemosus shape colloidal gold solution repeatability that this method synthesizes high photon absorbing intensity is high, Au colloidal nanoparticles between each batch
The particle size coefficient of variation is less than 10%.Equally have significantly in absorbance compared with conventional racemosus shape Au colloidal nanoparticles
Advantage.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
All any modification, equivalent and improvement made within principle etc., should all be included in the protection scope of the present invention.
Claims (2)
1. the preparation method of the high photon absorbing intensity racemosus shape Au colloidal nanoparticles of controllable grain size, it is characterised in that including walking as follows
Suddenly：
(1) synthesis of spherical shape colloidal gold seed solution：Using classical trisodium citrate reduction method, 1mL 1% is accurately pipetted
It is slowly stirred in HAuCl4 solution to the conical flask for filling 99mL ultra-pure waters, on magnetic stirring apparatus and is heated to boiling, accelerated at this time
Rotating speed and rapid disposable addition 2.7mL 1%Na3C6H5O7 solution, continue the 15min that boils, it is red to treat that solution colour becomes wine
It color and no longer changes, stops heating, at the uniform velocity stirring is cooled to room temperature to get to the spherical shape glue that grain size is 18 ± 2nm
Body gold seeds solution；
(2) particle size is the preparation of 33 ± 3nm high photon absorbing intensity racemosus shape Au colloidal nanoparticles：Accurately pipette above-mentioned ball
In shape colloidal gold seed solution 9mL to growth-promoting media, the growth-promoting media is by ultra-pure water 100mL, 1%HAuCl4 solution 1.2mL, 1%
Na3C6H5O7 solution 2.64mL is formed；It is slowly stirred on magnetic stirring apparatus, 50 DEG C is heated to after mixing, is revved up at this time, together
When disposably add in 30mmol/L quinol solution 24mL rapidly, solution temperature maintains 50 DEG C, the reaction was continued 10min, stops
Heating is cooled to room temperature and obtains particle size as 33 ± 3nm high photon absorbing intensity racemosus shape Au colloidal nanoparticles solution, 4 DEG C
It saves backup.
2. prepared by the high photon absorbing intensity racemosus shape Au colloidal nanoparticles of controllable grain size that synthetic method described in claim 1 obtains
Application in colloidal gold immuno-chromatography test paper strip.
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