CN105820814A - Gold-nanoparticle fluorescence probe and preparation method and application thereof - Google Patents
Gold-nanoparticle fluorescence probe and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a gold-nanoparticle fluorescence probe and a preparation method and application thereof. The preparation method comprises the steps that 1-10 parts of 3-5 mmol/L chloroauric acid aqueous solution is heated to 80 DEG C to 120 DEG C, 1-5 parts of 4-6 mmol/L 2-mercapto-4-methyl-5-thiazoleacetic acid aqueous solution is added to the chloroauric acid aqueous solution, continuous heating stirring is conducted for 5 min to 30 min, and the gold-nanoparticle fluorescence probe is obtained. The preparation method is simple in reaction condition, rapid and friendly to environment. 2-mercapto-4-methyl-5-thiazoleacetic acid serves as a reducing agent and a protective agent, 2-mercapto-4-methyl-5-thiazoleacetic acid itself has the reducing property, and addition of a frequently-used reducing agent sodium borohydride, surfactants and the like is avoided. The gold-nanoparticle fluorescence probe presents intense blue fluorescence on the fluorescence emission peak near 430 nm, the gold-nanoparticle fluorescence probe is good in stability when preserved at room temperature and can be used for high-sensitivity and high-selectivity detection of Fe<3+>, the detection process is simple, convenient and rapid, and the detection result is accurate.
Description
Technical field
The present invention relates to fluorescent probe, particularly a kind of water solublity blueness gold nano fluorescent probe and preparation method thereof and should
With.
Background technology
Ferrum is one of most important constituent of hemoglobin, participates in the transport of oxygen, to maintaining other oxygen carrying albumen as sub-
Ferri-hemoglobin enzyme, Myoglobin, cytochrome normal function the most essential, it is also many to participate in energy metabolisms simultaneously
The important composition of enzyme, has serious impact, especially blood system to health.Iron deficiency can cause erythrocyte the leanest
Blood, on the contrary, Fe supply also can give rise to diseases, such as parkinsonism, Alzheimer's disease and cancer.At present, tradition
Science detection ferrum method have multiple, such as: atomic absorption spectrography (AAS), inductive coupling ICP-MS and gas chromatogram
Methods etc., also document report uses organic dyestuff or quantum dots characterization ferrum.But most methods cost length high, time-consuming or needs are multiple
Miscellaneous precision instrument, therefore develops a kind of side novel, easy and simple to handle, that sample is tractable, instrument is relatively inexpensive
Method becomes a focus in analytical chemistry field.Fluorimetry have highly sensitive, can detect in real time, the most lossless to sample
The advantages such as wound and have broad application prospects.
Gold nano is of great interest due to the physicochemical property of its uniqueness in recent years, also obtains in analytical chemistry field
To being widely applied, the gold nano of functionalization as probe be widely used to pharmaceutical analysis, food safety, environmental analysis,
The field such as bioanalysis, biomarker.It is more likely to generate receiving of greater particle size it is said that in general, gold ion is reduced in the solution
Rice grain rather than have the small particle nano-cluster of fluorescence, this is because the specific surface area of nano-cluster is big, apparent activation energy is high, more
Easily assemble.Based on this, the synthesis of nano-cluster needs protecting against it and being gathered into further and do not have fluorescence of special groups
Nano-particle.The photoluminescent property tool of gold nano-probe is played a very important role by blocking group, therefore selects suitable protection group
Group seems most important.The blocking group being presently used for synthesizing gold nano fluorescent probe generally comprises the biology such as protein, polypeptide
Macromole and mercaptan micromolecular.When employing protein and other is protective agent, because the tyrosine institute in protein
The phenolic groups contained just has reproducibility at pH=12, Au (III) can be reduced into Au atom, so NaOH to be used will
Solution regulates to strong basicity.During with polypeptide for blocking group, the traditional chemical reduction method of general employing i.e. uses NaBH4By chlorine gold
Acid reduction obtains the gold nano grain that photoluminescent property is more weak, between recycling cetyl trimethylammonium bromide and gold nano grain
Electrostatic interaction gold nano grain is proceeded in organic facies toluene, organic facies is obtained the gold with photoluminescent property by etching
Nano-probe.When employing mercaptan micromolecular is protective agent, many reports use NaBH4For reducing agent, gold chloride is passed through power
Learn control method reduction and obtain the gold nano grain that photoluminescent property is more weak, the most under proper condition (such as heating and addition excess
Mercaptan etc.) obtain gold nano fluorescent probe further.The method reported needs to use strong reductant NaBH4, surface activity
Agent (cetyl trimethylammonium bromide) or strong basic reagent NaOH etc., and preparation process is loaded down with trivial details, required time is longer.
Summary of the invention
It is an object of the invention to provide a kind of gold nano fluorescent probe and its preparation method and application.Described gold nano is glimmering
Light probe preparation method is simple, and ferric ion is had high selectivity, can be used for detecting ferric ion, and detection means
Simply.
For solving above technical problem, the technical solution used in the present invention is:
The preparation method of a kind of gold nano fluorescent probe, including step: in terms of volume parts, by 1-10 part 3-5mmol/L
Aqueous solution of chloraurate is heated to 80-120 DEG C, then by 1-5 part 4-6mmol/L 2-sulfydryl-4-methyl-5-thiazole acetic acid aqueous solution
Join above-mentioned aqueous solution of chloraurate continuous heating stirring 5-30min, i.e. can get gold nano fluorescent probe.
As preferred technical scheme, aqueous solution of chloraurate and the volume of 2-sulfydryl-4-methyl-5-thiazole acetic acid aqueous solution
Ratio is 7-9:2-4.
As preferred technical scheme, the concentration of aqueous solution of chloraurate is 4mmol/L.
As preferred technical scheme, the concentration of 2-sulfydryl-4-methyl-5-thiazole acetic acid aqueous solution is 5mmol/L.
As preferred technical scheme, aqueous solution of chloraurate is heated to 100 DEG C.
As preferred technical scheme, 2-sulfydryl-4-methyl-5-thiazole acetic acid aqueous solution is joined aqueous solution of chloraurate
And continuous heating stirring 20min.
Prepared gold nano fluorescent probe has high selectivity to ferric ion, can be in detection ferric ion
Application.
The detection method of a kind of ferric ion, comprises the steps: gold nano fluorescent probe of the present invention
(200 μ L) and phosphate buffer solution (2.5mL, 10mmol/L) join in fluorescence cuvette, together at above-mentioned fluorescence cuvette
In be separately added into the Fe of variable concentrations again3+Standard solution or solution to be measured, with 350nm as excitation wavelength, measure its fluorescence spectrum,
Along with Fe3+The increase of concentration of standard solution, the fluorescence of gold nano fluorescent probe is gradually quenched, and establishes detection Fe based on this3+
Working curve.Fe3+Concentration and the relative intensity of fluorescence (I of gold nano fluorescent probe0/ I) in two sections of good linear relationships, its
The range of linearity is respectively 9.9 × 10-9-3.0×10-6Mol/L (Y=1.06+0.171X, linear coefficient R2=0.998) and 3.2 ×
10-6-1.1×10-3Mol/L (Y=1.68+0.00309X, linear coefficient R2=0.987), wherein, I0Fe is represented respectively with I3+No
Exist and in the presence of the fluorescence intensity of gold nano fluorescent probe, detection is limited to 3.3 × 10-9mol/L.Above-mentioned working curve can be applied
Fe in solution to be measured3+Detection.
Compared with prior art, the present invention uses " one kettle way " to be prepared for the blue-fluorescence nanometer material that a kind of water solublity is good
Material probe, reaction condition is simple, is swift in response, environmentally friendly.Selected 2-sulfydryl-4-methyl-5-thiazole acetic acid is reduction
Agent and protective agent self have reproducibility, it is to avoid the addition of conventional borane reducing agent sodium hydride, surfactant etc..
The gold nano fluorescent probe that the present invention provides, under uviol lamp, presents strong blue-fluorescence, fluorescence quantum yield
Up to 4.5%;Have under good light stability, room temperature and can preserve more than 12 months;There is height to ferric ion select
Property, can apply in detection ferric ion, and detection means is simple, it is only necessary to can realize by fluorescence spectrophotometer, detection
Result is accurate.
Accompanying drawing explanation
The preparation of Fig. 1 embodiment 1 gold nano fluorescent probe and the schematic diagram to ferric ion mensuration.
The fluorescence excitation of Fig. 2 embodiment 1 gold nano fluorescent probe and emission spectrum figure.
Fluorescence block diagram after Fig. 3 embodiment 1 gold nano fluorescent probe and various cation sites.
The working curve that ferric ion is responded by Fig. 4 embodiment 1 gold nano fluorescent probe.
Detailed description of the invention
Below by specific embodiment, the method for the present invention is illustrated.Method described in subordinate's embodiment, as without special
Different explanation, is conventional method;Described reagent and material, if no special instructions, the most commercially obtain.In experimentation
The glass drying oven chloroazotic acid of all uses is cleaned standby by distilled water rinsing post-drying again.Experiment uses fluorescence spectrophotometer
(F4500) fluorescence spectrum and the fluorescence quantum yield of gold nano-probe are measured.
Embodiment 1
7mL 4mmol/L aqueous solution of chloraurate is heated to 100 DEG C, then by 2mL 5mmol/L 2-sulfydryl-4-methyl-5-
Thiazolyl acetic acid aqueous solution joins above-mentioned aqueous solution of chloraurate continuous heating stirring 20min, i.e. can get gold nano fluorescence and visits
Pin.The fluorescence emission peak of this gold nano fluorescent probe, near 430nm, presents strong blue-fluorescence, and quantum yield is
4.5%.
Embodiment 2
10mL 4mmol/L aqueous solution of chloraurate is heated to 120 DEG C, then by 1mL 5mmol/L 2-sulfydryl-4-methyl-
5-thiazolyl acetic acid aqueous solution joins above-mentioned aqueous solution of chloraurate continuous heating stirring 30min, i.e. can get gold nano fluorescence
Probe.The fluorescence emission peak of this gold nano fluorescent probe, near 430nm, presents strong blue-fluorescence, and quantum yield is
3.5%.
Embodiment 3
1mL 4mmol/L aqueous solution of chloraurate is heated to 110 DEG C, then by 5mL 5mmol/L 2-sulfydryl-4-methyl-5-
Thiazolyl acetic acid aqueous solution joins above-mentioned aqueous solution of chloraurate continuous heating stirring 20min, i.e. can get gold nano fluorescence and visits
Pin.The fluorescence emission peak of this gold nano fluorescent probe, near 430nm, presents strong blue-fluorescence, and quantum yield is
2.7%.
Embodiment 4
3mL 4mmol/L aqueous solution of chloraurate is heated to 90 DEG C, then by 3mL 5mmol/L 2-sulfydryl-4-methyl-5-
Thiazolyl acetic acid aqueous solution joins above-mentioned aqueous solution of chloraurate continuous heating stirring 5min, i.e. can get gold nano fluorescence and visits
Pin.The fluorescence emission peak of this gold nano fluorescent probe, near 430nm, presents strong blue-fluorescence, and quantum yield is
3.3%.
Embodiment 5
5mL 4mmol/L aqueous solution of chloraurate is heated to 80 DEG C, then by 4mL 5mmol/L 2-sulfydryl-4-methyl-5-
Thiazolyl acetic acid aqueous solution joins above-mentioned aqueous solution of chloraurate continuous heating stirring 10min, i.e. can get gold nano fluorescence and visits
Pin.The fluorescence emission peak of this gold nano fluorescent probe, near 430nm, presents strong blue-fluorescence, and quantum yield is
3.0%.
Embodiment 6
9mL 4mmol/L aqueous solution of chloraurate is heated to 100 DEG C, then by 4mL 5mmol/L 2-sulfydryl-4-methyl-5-
Thiazolyl acetic acid aqueous solution joins above-mentioned aqueous solution of chloraurate continuous heating stirring 20min, i.e. can get gold nano fluorescence and visits
Pin.The fluorescence emission peak of this gold nano fluorescent probe, near 430nm, presents strong blue-fluorescence, and quantum yield is
4.3%.
Embodiment 7
7mL 3mmol/L aqueous solution of chloraurate is heated to 100 DEG C, then by 3mL 6mmol/L 2-sulfydryl-4-methyl-5-
Thiazolyl acetic acid aqueous solution joins above-mentioned aqueous solution of chloraurate continuous heating stirring 30min, i.e. can get gold nano fluorescence and visits
Pin.The fluorescence emission peak of this gold nano fluorescent probe, near 430nm, presents strong blue-fluorescence, and quantum yield is
3.6%.
Embodiment 8
7mL 5mmol/L aqueous solution of chloraurate is heated to 100 DEG C, then by 5mL 4mmol/L 2-sulfydryl-4-methyl-5-
Thiazolyl acetic acid aqueous solution joins above-mentioned aqueous solution of chloraurate continuous heating stirring 20min, i.e. can get gold nano fluorescence and visits
Pin.The fluorescence emission peak of this gold nano fluorescent probe, near 430nm, presents strong blue-fluorescence, and quantum yield is
3.4%.
Embodiment 9
Gold nano fluorescent probe solution (200 μ L) prepared by embodiment 1 and the phosphate buffer solution (10mmol/ of 2.5mL
L) it is added in fluorescence cuvette, above-mentioned fluorescence cuvette is separately added into the Fe of 10 μ L 0.5mmol/L again3+With 10 μ L
Other cation K of 1mol/L+,Na+,Li+,Ni+,Zn2+,Mn2+,Ba2+,Ca2+,Cd2+,Mg2+,Pb2+,Co2+,Hg2+,Cu2+,
Fe2+,Al3+,Cr3+Solution, surveys its fluorescence spectrum respectively, draws the block diagram of fluorescence intensity at different ions correspondence 430nm, sees
Fig. 3.The experiment proved that, the detection to ferric ion of other cation not interference system.
Embodiment 10
Gold nano fluorescent probe solution (200 μ L) prepared by embodiment 1 and phosphate buffer solution (2.5mL, 10mmol/
L) join together in fluorescence cuvette, above-mentioned fluorescence cuvette is separately added into the Fe of variable concentrations again3+Standard solution or
Solution to be measured, with 350nm as excitation wavelength, measures its fluorescence spectrum.Along with Fe3+The increase of concentration of standard solution, gold nano is glimmering
The fluorescence of light probe is gradually quenched, as shown in Figure 4, and the change of fluorescence intensity and Fe3+Concentration linear, fluorescence in figure
The change of intensity is with I0/ I represents, wherein I0With I represent respectively iron ion do not exist and in the presence of the fluorescence of gold nano fluorescent probe
Intensity, obtains Fe by linear fit3+Concentration and the relative intensity of fluorescence (I of gold nano fluorescent probe0/ I) good in two sections
Linear relationship, its range of linearity is respectively 9.9 × 10-9-3.0×10-6Mol/L (Y=1.06+0.171X, linear coefficient R2=
0.998) and 3.2 × 10-6-1.1×10-3Mol/L (Y=1.68+0.00309X, linear coefficient R2=0.987), Fe3+Detection
It is limited to 3.3 × 10-9mol/L.This gold nano fluorescent probe can be applicable to the detection of ferric ion in serum.
Claims (7)
1. the preparation method of a gold nano fluorescent probe, it is characterised in that include step: in terms of volume parts, by 1-10 part
3-5mmol/L aqueous solution of chloraurate is heated to 80-120 DEG C, then by 1-5 part 4-6mmol/L 2-sulfydryl-4-methyl-5-thiazole second
Aqueous acid joins above-mentioned aqueous solution of chloraurate continuous heating stirring 5-30min, i.e. obtains gold nano fluorescent probe.
The preparation method of a kind of gold nano fluorescent probe the most as claimed in claim 1, it is characterised in that described gold chloride water
The volume ratio of solution and 2-sulfydryl-4-methyl-5-thiazole acetic acid aqueous solution is 7-9:2-4.
The preparation method of a kind of gold nano fluorescent probe the most as claimed in claim 1, it is characterised in that described gold chloride water
The concentration of solution is 4mmol/L.
The preparation method of a kind of gold nano fluorescent probe the most as claimed in claim 1, it is characterised in that described 2-sulfydryl-
The concentration of 4-methyl-5-thiazole acetic acid aqueous solution is 5mmol/L.
The preparation method of a kind of gold nano fluorescent probe the most as claimed in claim 1, it is characterised in that described gold chloride water
Solution is heated to 100 DEG C.
The preparation method of a kind of gold nano fluorescent probe the most as claimed in claim 1, it is characterised in that described heated and stirred
Time is 20min.
7. the gold nano fluorescent probe that as claimed in claim 1 prepared by method is applied in detection ferric ion.
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CN108690603A (en) * | 2018-06-08 | 2018-10-23 | 河南师范大学 | A kind of AuNCs@APAP fluorescence probes and its preparation method and application |
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CN108690603A (en) * | 2018-06-08 | 2018-10-23 | 河南师范大学 | A kind of AuNCs@APAP fluorescence probes and its preparation method and application |
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