CN107345910A - Wide colourity test paper of a kind of fluorescence for Visual retrieval copper ion and its preparation method and application - Google Patents
Wide colourity test paper of a kind of fluorescence for Visual retrieval copper ion and its preparation method and application Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 53
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910001431 copper ion Inorganic materials 0.000 title claims abstract description 49
- 230000000007 visual effect Effects 0.000 title claims abstract description 30
- 239000002096 quantum dot Substances 0.000 claims abstract description 47
- 239000000523 sample Substances 0.000 claims abstract description 45
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 239000007850 fluorescent dye Substances 0.000 claims abstract description 4
- 239000007790 solid phase Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 7
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical class OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- XONPDZSGENTBNJ-UHFFFAOYSA-N molecular hydrogen;sodium Chemical compound [Na].[H][H] XONPDZSGENTBNJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910000059 tellane Inorganic materials 0.000 claims description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 239000003643 water by type Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000003086 colorant Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical class C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 3
- 238000006392 deoxygenation reaction Methods 0.000 claims description 3
- CCIVGXIOQKPBKL-UHFFFAOYSA-N ethanesulfonic acid Chemical compound CCS(O)(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-N 0.000 claims description 3
- 150000002171 ethylene diamines Chemical class 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 102000004144 Green Fluorescent Proteins Human genes 0.000 claims description 2
- 108010043121 Green Fluorescent Proteins Proteins 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- 238000006862 quantum yield reaction Methods 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 17
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000010791 quenching Methods 0.000 abstract description 4
- 230000000171 quenching effect Effects 0.000 abstract description 4
- 241000972773 Aulopiformes Species 0.000 abstract description 3
- 244000025254 Cannabis sativa Species 0.000 abstract description 3
- VAYOSLLFUXYJDT-RDTXWAMCSA-N Lysergic acid diethylamide Chemical compound C1=CC(C=2[C@H](N(C)C[C@@H](C=2)C(=O)N(CC)CC)C2)=C3C2=CNC3=C1 VAYOSLLFUXYJDT-RDTXWAMCSA-N 0.000 abstract description 3
- 240000007817 Olea europaea Species 0.000 abstract description 3
- 235000019515 salmon Nutrition 0.000 abstract description 3
- 239000010454 slate Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- PMNLUUOXGOOLSP-UHFFFAOYSA-N 2-mercaptopropanoic acid Chemical class CC(S)C(O)=O PMNLUUOXGOOLSP-UHFFFAOYSA-N 0.000 abstract 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 9
- 229910052802 copper Inorganic materials 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 210000002700 urine Anatomy 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 201000010099 disease Diseases 0.000 description 5
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6439—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" with indicators, stains, dyes, tags, labels, marks
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- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Optics & Photonics (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Wide colourity test paper of a kind of fluorescence for Visual retrieval copper ion and its preparation method and application, using three color ratio rate fluorescence probes as ink, by ink-jet printer using filter paper as solid phase carrier, surface, obtains the test paper of Visual retrieval copper ion；Three described color ratio rate fluorescence probes are blue carbon point, green quantum dot and red quantum dot, and the quantum dot is that 3 mercaptopropionic acids are modified.The present invention utilizes the principle of double quenchings first, build three color ratio rate fluorescent test papers and be used for visual detection copper ion, the Test paper of preparation possesses the advantages of wider than existing double ratio fluorescent probe test paper color change intervals, realize as detectable substance adds, test paper color from shallow red color to light salmon to darkorange to grass green to dark olive green color to slate blueness to royalblue to fine blue (Fig. 4), can clearly be identified by visually.
Description
Technical field
The invention belongs to copper ion detection technique field, and in particular to a kind of fluorescence for Visual retrieval copper ion is wide
Colourity test paper and its preparation method and application.
Background technology
Copper is the important element of health, and enzyme completes energy generation, god using the redox active of this metal
Function through mediator and pigment synthesis and epigenetic modification.On the one hand, the shortage of copper can cause many diseases, such as anaemia, entirely
Haemocyte is reduced and marrow is abnormal.On the other hand, copper metabolic disorder also with many diseases, including cancer, nervus retrogression A Er
Ci Haimo diseases, Parkinson and Huntington's disease, genetic disease such as syndrome and the Wilson's disease of perming.It is typical as one
The disease of copper mediation, Wilson's disease are the autosomal recessive diseases that copper is accumulated in a kind of tissue.Suffer from Wilson's disease
Patient be usually expressed as high urine copper content (>100 μ g/24 hours, compared with normal person).Normal person's urine copper content of 24 hours
Reported between reference value different experiments room it is different, it is most of using 40 μ g/24 hours (0.6 μm of ol/24 hour) as normally
The upper limit of value.Therefore a clinical diagnosis index can be used as by detecting urine copper.
The method of traditional detection copper ion includes inductively coupled plasma mass spectrometry, atomic absorption spectrography (AAS), atom
Emission spectrometry and mass spectrography.But traditional laboratory large-scale instrument is present that expensive, bulky is heavy, is needed before detection
Sample pre-treatments that will be complicated and must be by having received the shortcomings of professional of special training is to operate, in addition along with sample palpus
Depart from detection scene and be sent to assay laboratory, and real-time live can not be accomplished and detected.Therefore, a kind of simple and quick, cost is found
It is cheap and be easy to the method for Site Detection carried with, it is the great challenge that analysis worker faces.
In the last few years, because semiconductor-quantum-point and carbon point have obvious advantage compared to traditional organic dyestuff, because
This, which turns into, is used for the optical label that chemical/biological sensory field has much potentiality.The advantages of quantum dot, attracts vast scientific research scholar's
Concern, such as good in optical property, photochemical stability is good, fluorescence lifetime length, good water solubility etc..In addition, fluorescence sense utensil
Another unrivaled advantage having, that is, only need a portable uviol lamp can to realize with the naked eye direct
The Visual retrieval of the analyte of observation.Based on the extensive use of classical pH test paper, fluorescence detection test is usually by fluorescence probe
Molecule is fixed on substrate by way of assembling or printing, and the Test paper prepared by this method has low cost,
It is easy to operation, the advantage such as portable.
However, this fluorescence detection test the same similar to pH test paper still has an arduous problem.At present, it is glimmering
Establishing more for light test paper is realized using the fluorescence probe of solid color, but the fluorescence probe of solid color is only
Analyte can be detected by the strong and weak change of fluorescence caused by fluorescence opening or quenching, this method is greatly
Limit the quantification ability of test paper.Later, people had developed double emission ratios probes, and the strong of single color is replaced with color change
It is weak to realize to object more accurately Visual retrieval.Regrettably, double emission ratios probes are still not successful enough, because working as
When two different colors of fluorescence probe mixes, obtain the colors of ratio probes necessarily both centre it is composite coloured, from
And it have compressed the scope of color change.So when fluorescence probe is used on test paper, fluorescent test paper only actually shows two
Partial color change, and this color change and unobvious.In general, existing fluorescent test paper generally existing is directed to mesh at present
The problems such as mark agent amount colourity changes less sensitive, spectrum evolution narrow range, can not carry out visualizing quantitative detection to object,
The fluorescent test paper that quantitative detection can be carried out visualizing to object is also more rare.
The content of the invention
The technical problem of solution：The present invention is intended to provide a kind of three color ratio rate fluorescent test papers and Visual retrieval copper ion
Method, this method have selectivity height, high sensitivity, can quantify detect, testing result is directly perceived and color change is obvious
Feature.
Technical scheme：A kind of preparation method of the wide colourity test paper of fluorescence for Visual retrieval copper ion, step be with
Three color ratio rate fluorescence probes, by ink-jet printer using filter paper as solid phase carrier, surface, obtain visual as ink
Change the test paper of detection copper ion；Three described color ratio rate fluorescence probes are blue carbon point, green quantum dot and red quantum dot, institute
It is that 3- mercaptopropionic acids are modified to state quantum dot.
The preparation of above-mentioned three color ratios rate fluorescence probe comprises the following steps：(1) preparation of cadmium telluride quantum dot：In proportion,
By 0.2284g caddies (CdCl2·2.5H2O) it is added in the ultra-pure water of 100mL deoxygenations, then adds 0.21mL 3- sulfydryls
Propionic acid (MPA), then its pH value is adjusted to 10 with 1M sodium hydroxide solutions, obtain mixed solution；Take 0.0319g telluriums powder and 0.05g
Sodium borohydride adds 2mL ultra-pure waters, under nitrogen protection, ice bath 8 hours, reaction generation sodium hydrogen telluride solution；By 10mL 0.5M
Sulfuric acid solution is injected into the sodium hydrogen telluride solution of generation, by the flowing of nitrogen by the H of generation2Te is all passed through above-mentioned mixing
In solution, stir 20 minutes at room temperature, the color of mixed solution is changed into orange-yellow from colourless, continues to heat under the conditions of 100 DEG C
Backflow 50 minutes, obtain the green quantum dot of mercaptopropionic acid modification；Or 24-48 hours are heated to reflux, obtain red quantum dot；
(2) preparation of blue carbon point：In proportion, 1-2g citric acids and 100-500 μ L ethylenediamines are dissolved in 20mL ultra-pure waters, then turned
Move in 30mL ptfe autoclaves, 4-8 hours are reacted at 200 DEG C, be 500 by obtained carbon point molecular cut off
Bag filter is dialysed 24-48 hours, standby；The preparation of (3) three color ratio rate fluorescence probes：In proportion, it is 90 μ L green quantum dots are molten
Liquid, 40 μ L red quantum dots solution and 30 μ L blueness carbon dots solutions are added in beaker, add pH=7.4 20mL 10mM
The ethyl sulfonic acid cushioning liquid of N-2- hydroxyethyl piperazines-N ' -2, it is well mixed, that is, obtains three mixture of colours ratio fluorescent probe solutions.
Preferably, above-mentioned blue carbon dots solution, green quantum dot solution, the volume ratio of red quantum dot solution is 3:9:4.
Preferably, gained quantum dot stoste irradiates 1 hour to improve quantum yield under 15W uviol lamp in step (1).
Preferably, gained quantum dot is washed three times with acetone in step (1), then precipitation is scattered in ultra-pure water, standby.
The preparation of above-mentioned test paper comprises the following steps：The business for buying back is washed with deionized water with ink-cases of printers
Only, dry, chalk box of having leisure, three color ratio probes are injected into blank print cartridge with syringe, printed on common filter paper
One 7 × 3cm2Rectangular patterns, duplicate printing about 30 times, naturally place 5 minutes, rectangular patterns are cut into 3 × 1cm2Bar
The Test paper of shape.
Preferably, the thickness of above-mentioned fluorescence probe layer is 0.05-0.1 μm.
The wide colourity test paper of the fluorescence of Visual retrieval copper ion made from above-mentioned preparation method.
The wide colourity test paper of fluorescence of above-mentioned Visual retrieval copper ion, three color ratio rate fluorescence probes swash in single wavelength light source
Blueness can be launched respectively by giving, green and red fluorescence；The wavelength that wherein single wavelength light source excites is 360nm；Blueness
Fluorescence emission wavelengths are 440nm；Green-fluorescent emission wavelength is 510nm；Red fluorescence launch wavelength is 600nm.
Application of the above-mentioned wide colourity test paper of fluorescence in visual detection copper ion.
Technical scheme is exactly by blue carbon point, green quantum dot and red in brief including preparation method
Quantum dot is mixed to get a kind of fluorescence probe, and is printed on test paper.Confirm that its original position can by the method for double quenchings
Validity depending on changing detection copper ion.Blue carbon point is fluorescent stabilization to copper ion, but green quantum dot and red quantum
The fluorescence of point rapidly can be quenched by copper ion.Compared to traditional visualization test paper, when copper ion concentration is relatively low, base
There is the feature of height discernable by eye rate in the Test paper that three color probes are prepared.Such fluorescent test paper can visualize inspection
The content of copper ion surveyed in water sample and urine sample.
Beneficial effect：The present invention using the principle of double quenchings, builds three color ratio rate fluorescent test papers and for visualizing first
Detection copper ion.Test paper prepared by the present invention possesses wider than existing double ratio fluorescent probe test paper color change intervals excellent
Point, realize as detectable substance adds, test paper color is from shallow red color to light salmon to darkorange to grass green to dark olive green color
To slate blueness to royalblue to fine blue (Fig. 4), can clearly be identified by visually.The invention enables test paper inspection
Survey technology application is widened, and lacks for clinical diagnosis copper ion or copper ion metabolic disturbance diseases provide diagnosis and referred to
Mark.Preparation method of the present invention is simple, and raw material are simple and easy to get, it is not necessary to special technical staff, can keep away to a certain extent
Exempt to use large-scale instrument, it is only necessary to which a hand-held uviol lamp can carry out Visual retrieval, simple to operate, quick and convenient, sensitive
Degree is high, significant effect.This method can effectively avoid the interference of other impurities in sample, selective good.The test paper of preparation can show
Field real-time online Visual retrieval copper ion.
Brief description of the drawings
Fig. 1 is blue carbon point (a), green quantum dot (b), red quantum dot (c), quantum dot/carbon point mixed system (d)
Fluorescence spectra.
Fig. 2 is various concentrations copper ion to quantum dot/carbon point mixed system fluorescence pattern and color change figure.With copper from
Sub- concentration increase (be from left to right followed successively by 0,3,6,10,20,40,60,80,110,140,180,230,280,330,
430nM) solution colour gradually changes.
Fig. 3 is selectivity of the Test paper to other different kinds of ions.
Fig. 4 is that test paper detects copper ion in the aqueous solution and visualizes photo, test paper color change under the first behavior uviol lamp, the
Test paper color change under two behavior daylight.Copper ion concentration is from left to right followed successively by 0,6,20,60,110,180,280,430nM.
Fig. 5 is that test paper detects copper ion in urine and visualizes photo, the color change of test paper under the first behavior daylight, second
Test paper color change under behavior uviol lamp.Copper ion concentration is from left to right followed successively by 58.7,26.3,178nM.
Embodiment
Following examples further illustrate present disclosure, but should not be construed as limiting the invention.Without departing substantially from
In the case of spirit and essence of the invention, the modification and replacement made to the inventive method, step or condition, the present invention is belonged to
Scope.Unless otherwise specified, the conventional meanses that technological means used in embodiment is well known to those skilled in the art.
Embodiment 1
1. the preparation of quantum dot
By 0.2284g caddies (CdCl2·2.5H2O) it is added in the ultra-pure water of 100mL deoxygenations, then adds 0.21mL
3- mercaptopropionic acids (MPA), then its pH value is adjusted to 10 with 1M sodium hydroxide solutions, obtain mixed solution；Take 0.0319g telluriums powder and
0.05g sodium borohydrides add 2mL ultra-pure waters, under nitrogen protection, ice bath 8 hours, reaction generation sodium hydrogen telluride；By 10mL
0.5M sulfuric acid solutions are injected into the sodium hydrogen telluride solution of generation, by the flowing of nitrogen by the H of generation2Te is all passed through above-mentioned
In the mixed solution, stir 20 minutes at room temperature, the color of mixed solution is changed into orange-yellow from colourless, under the conditions of 100 DEG C
Continue to be heated to reflux 50 minutes, obtain the green cadmium telluride quantum dot of mercaptopropionic acid modification, to obtain red quantum dot, then
24-48 hours need to be heated to reflux, gained quantum dot stoste is irradiated 1 hour under 15W uviol lamp, then washs three with acetone
It is secondary, then precipitation is scattered in ultra-pure water, it is standby.
2. the preparation of carbon point
1-2g citric acids and 100-500 μ L ethylenediamines are dissolved in 20mL ultra-pure waters, are subsequently transferred to 30mL polytetrafluoroethyl-nes
In alkene reaction kettle, 4-8 hours are reacted at 200 DEG C, by the bag filter dialysis 24-48 that obtained carbon point molecular cut off is 500
Hour, it is standby.
3. the preparation of three color ratio rate fluorescence probes
By 90 μ L green quantum dots, 40 μ L red quantum dots and 30 μ L bluenesss carbon points are added in beaker, are added
The ethyl sulfonic acid cushioning liquid (pH=7.4) of 20mL10mM N-2- hydroxyethyl piperazines-N ' -2, it is well mixed, that is, it is glimmering obtains three color ratio rates
Light probe solution.Fluorescence spectrum is shown in Fig. 1.
4. three color ratio rate fluorescence probe mixed system Visual retrieval copper ions
Copper ion solution to be measured is added to progress fluorescent visual detection in three color ratio rate fluorescence probe mixed systems.
It is gradually increased with the concentration of copper ion, fluorescence color is by shallow red color to light salmon to darkorange to grass green to dark olive green color
Royalblue is arrived to fine blueness to slate blueness.Now under uviol lamp, it can be seen that the stepped change of color, realize visualization inspection
Survey.Visualization photo is shown in Fig. 2.
Embodiment 2
1. the preparation of quantum dot
Quantum dot preparation method in the present embodiment is the same as embodiment 1.
2. the preparation of carbon point
Carbon point preparation method in the present embodiment is the same as embodiment 1.
3. the preparation of three color ratio rate fluorescence probes
Three color ratio rate fluorescence probe preparation methods in the present embodiment are the same as embodiment 1.
4. 0.3mM copper ion and the other ion Standard Stock solutions of 3mM is prepared respectively.
5. certain volume is taken to be added to the molten of three color ratio rate fluorescence probes the different ions Standard Stock solutions in step 4
In liquid.
6. Test paper is as shown in Figure 3 to the selectivity of other different kinds of ions.
Embodiment 3
1. the preparation of quantum dot
Quantum dot preparation method in the present embodiment is the same as embodiment 1.
2. the preparation of carbon point
Carbon point preparation method in the present embodiment is the same as embodiment 1.
3. the preparation of three color ratio rate fluorescence probes
Three color ratio rate fluorescence probe preparation methods in the present embodiment are the same as embodiment 1.
4. the preparation of Test paper
Next business will be bought back to be washed with deionized water only with ink-cases of printers, drying, chalk box of having leisure.Three color ratio rates are visited
Pin is injected into blank print cartridge with syringe, and a 7 × 3cm is printed on common filter paper2Rectangular patterns, duplicate printing is about
30 times, place 5 minutes naturally, rectangular patterns are cut into 3 × 1cm2Strip, you can obtain having response to object copper ion
Test paper, the thickness of fluorescence probe layer is 0.05-0.1 μm.
5. copper ion in Visual retrieval water
After test paper drying, the copper ion of various concentrations is slowly added drop-wise on the test paper of preparation, at ambient temperature
After drying 5 minutes, with the 360nm ultraviolet lights excited and the change of its fluorescence color is observed.Visualization picture is shown in Fig. 4.
Embodiment 4
1. the preparation of quantum dot
Quantum dot preparation method in the present embodiment is the same as embodiment 1.
2. the preparation of carbon point
Carbon point preparation method in the present embodiment is the same as embodiment 1.
3. the preparation of three color ratio rate fluorescence probes
Three color ratio rate fluorescence probe preparation methods in the present embodiment are the same as embodiment 1.
4. the preparation of Test paper
Next business will be bought back to be washed with deionized water only with ink-cases of printers, drying, chalk box of having leisure.Three color ratio rates are visited
Pin is injected into blank print cartridge with syringe, and a 7 × 3cm is printed on common filter paper2Rectangular patterns, duplicate printing is about
30 times, place 5 minutes naturally, rectangular patterns are cut into 3 × 1cm2Strip, you can obtain having response to object copper ion
Test paper, the thickness of fluorescence probe layer is 0.05-0.1 μm.
5. copper ion in Visual retrieval urine
After test paper drying, the copper ion urine sample after the sample-adding containing various concentrations is slowly added drop-wise to the test paper of preparation
On, after drying 5 minutes at ambient temperature, with the 360nm ultraviolet lights excited and observe the change of its fluorescence color.Can
See Fig. 5 depending on changing picture.
Claims (10)
1. the preparation method of the wide colourity test paper of a kind of fluorescence for Visual retrieval copper ion, it is characterised in that step is with three
Color ratio rate fluorescence probe, by ink-jet printer using filter paper as solid phase carrier, surface, is visualized as ink
Detect the test paper of copper ion；Three described color ratio rate fluorescence probes are blue carbon point, green quantum dot and red quantum dot, described
Quantum dot is that 3- mercaptopropionic acids are modified.
2. the preparation method of the wide colourity test paper of a kind of fluorescence for Visual retrieval copper ion according to claim 1, its
It is characterised by that the preparation of the three color ratios rate fluorescence probe comprises the following steps：(1) preparation of cadmium telluride quantum dot：In proportion,
By 0.2284g caddies (CdCl2·2.5H2O) it is added in the ultra-pure water of 100mL deoxygenations, then adds 0.21mL 3- sulfydryls
Propionic acid (MPA), then its pH value is adjusted to 10 with 1M sodium hydroxide solutions, obtain mixed solution；Take 0.0319g telluriums powder and 0.05g
Sodium borohydride adds 2mL ultra-pure waters, under nitrogen protection, ice bath 8 hours, reaction generation sodium hydrogen telluride solution；By 10mL 0.5M
Sulfuric acid solution is injected into the sodium hydrogen telluride solution of generation, by the flowing of nitrogen by the H of generation2Te is all passed through above-mentioned mixing
In solution, stir 20 minutes at room temperature, the color of mixed solution is changed into orange-yellow from colourless, continues to heat under the conditions of 100 DEG C
Backflow 50 minutes, obtain the green quantum dot of mercaptopropionic acid modification；Or 24-48 hours are heated to reflux, obtain red quantum dot；
(2) preparation of blue carbon point：In proportion, 1-2g citric acids and 100-500 μ L ethylenediamines are dissolved in 20mL ultra-pure waters, then turned
Move in 30mL ptfe autoclaves, 4-8 hours are reacted at 200 DEG C, be 500 by obtained carbon point molecular cut off
Bag filter is dialysed 24-48 hours, standby；The preparation of (3) three color ratio rate fluorescence probes：In proportion, it is 90 μ L green quantum dots are molten
Liquid, 40 μ L red quantum dots solution and 30 μ L blueness carbon dots solutions are added in beaker, add pH=7.4 20mL 10mM
The ethyl sulfonic acid cushioning liquid of N-2- hydroxyethyl piperazines-N ' -2, it is well mixed, that is, obtains three mixture of colours ratio fluorescent probe solutions.
3. the preparation method of the wide colourity test paper of a kind of fluorescence for Visual retrieval copper ion according to claim 2, its
The blue carbon dots solution is characterised by, green quantum dot solution, the volume ratio of red quantum dot solution is 3:9:4.
4. the preparation method of the wide colourity test paper of a kind of fluorescence for Visual retrieval copper ion according to claim 2, its
It is characterised by step (1) that gained quantum dot stoste irradiates 1 hour to improve quantum yield under 15W uviol lamp.
5. the preparation method of the wide colourity test paper of a kind of fluorescence for Visual retrieval copper ion according to claim 2, its
It is characterised by step (1) that gained quantum dot is washed three times with acetone, then precipitation is scattered in ultra-pure water, it is standby.
6. the preparation method of the wide colourity test paper of a kind of fluorescence for Visual retrieval copper ion according to claim 1, its
It is characterised by that the preparation of the test paper comprises the following steps：The business for buying back is washed with deionized water with ink-cases of printers
Only, dry, chalk box of having leisure, three color ratio probes are injected into blank print cartridge with syringe, printed on common filter paper
One 7 × 3cm2Rectangular patterns, duplicate printing about 30 times, naturally place 5 minutes, rectangular patterns are cut into 3 × 1cm2Bar
The Test paper of shape.
7. the preparation method of the wide colourity test paper of a kind of fluorescence for Visual retrieval copper ion according to claim 6, its
The thickness for being characterised by the fluorescence probe layer is 0.05-0.1 μm.
8. according to the wide colourity test paper of fluorescence of Visual retrieval copper ion made from any preparation method of claim 1~7.
9. the wide colourity test paper of the fluorescence of Visual retrieval copper ion according to claim 7, it is characterised in that three color ratio rates are glimmering
Light probe can launch blueness, green and red fluorescence respectively in the case where single wavelength light source excites；Wherein single wavelength light source
The wavelength excited is 360nm；Blue fluorescent emissions wavelength is 440nm；Green-fluorescent emission wavelength is 510nm；Red fluorescence is sent out
The a length of 600nm of ejected wave.
10. application of the wide colourity test paper of fluorescence described in claim 9 in visual detection copper ion.
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