CN108226121A - A kind of double fluorescent emission test paper of gold nanoclusters base, preparation method and its application in Cu2+ detections - Google Patents
A kind of double fluorescent emission test paper of gold nanoclusters base, preparation method and its application in Cu2+ detections Download PDFInfo
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- CN108226121A CN108226121A CN201810067009.2A CN201810067009A CN108226121A CN 108226121 A CN108226121 A CN 108226121A CN 201810067009 A CN201810067009 A CN 201810067009A CN 108226121 A CN108226121 A CN 108226121A
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Abstract
A kind of double fluorescent emission test paper of gold nanoclusters base, preparation method and its in Cu2+Etc. the application in toxic ion detection, belong to technical field of fluorescence detection.Synthesizing including gold nanoclusters, ultra-thin g C3N4The preparation of nanometer sheet and double fluorescent emission g C3N4Three steps such as preparation of/Au NCs/CS test paper.The obtained double fluorescent emission test paper g C of the present invention3N4Under 372nm ultraviolet excitations, double fluorescent emission effects of visible region 450nm blue lights and 596nm feux rouges are presented in/Au NCs/CS.There is the result of different responses using double fluorescence for different copper ion concentrations; different composite fluorescence color changes is presented; this double fluorescent emission test paper can be used for the copper ion of bore hole colorimetric detection underwater trace; and detect limit can down to 10ppb, this for environmental protection and food security intermediate ion detection provide it is convenient.
Description
Technical field
The invention belongs to technical field of fluorescence detection, and in particular to prepared by a kind of double fluorescent emission test paper of gold nanoclusters base
Method and its in Cu2+Etc. the application in toxic ion detection.
Background technology
Copper ion is one of the essential trace elements of the human body, is distributed widely in multiple tissues of human body, in human body
Important role is play, has important role to brain, heart, hematopoiesis and anticancer, however excessive copper ion can be led
Serious health problem is caused, such as ischemic heart disease, nephrosis, anaemia and skeletal diseases can be caused, can also be given dirty in human body
Device causes to bear, so as to influence health.The copper of human intake is mainly obtained from water, food and environment.Therefore, water
The analysis of middle copper ion measures, and has very important practical significance.The assay method of common copper trace mainly has electrochemistry
Analytic approach, spectrophotometry, chemoluminescence method and fluorescence method etc..Fluorescence method is due to its selective good, high sensitivity, method letter
Just the advantages that, instrument and equipment is simple and be concerned.At present, the sensing material that common fluorescent optical sensor uses mainly includes glimmering
Light organic molecule, containing rare earth compounding, metal nanometre cluster and semiconductor-quantum-point etc..
Metal nanometre cluster (NCs) sensing material due to the features such as it is easily prepared, quantum efficiency is high, fluorescent stability is strong by
The extensive concern of scientific worker is arrived.Metal nanometre cluster is that one kind is closely sized to by what several to dozens of metallic atoms formed
A kind of novel fluorescence nanosensor material of Fermi's wavelength of electronics.Due to extra small size, it being made to show to be different from
The special nature of macro nanometer particle, such as adjustable fluorescent emission, larger Stokes shift, hypotoxicity, bio-compatible
Property it is good etc..The many advantageous properties of metal nanometre cluster make it in ion and biological micromolecule detection, Enzyme assay, biology mark
The sensory fields such as note, bio-imaging have a wide range of applications.However most of fluorescence sense application all only rests on single-shot and penetrates
In the level of detection, this is just highly susceptible to the influence of concentration and probe concentration, instrument state and ambient condition, leads to test result not
Accurately.Therefore, there is an urgent need for prepare the material of more convenient, more accurate, more stable double fluorescent emissions.
Double fluorescent emissive materials have the effect that single light excites lower pair of fluorescent emission, and a kind of fluorescence is with target when detecting
The variation of detectable substance and change, another fluorescence hardly changes, you can thinks to implant correction in detection architecture
The factor, can be to avoid the influence of concentration and probe concentration, instrument state and ambient condition, and double fluorescent emissions easily can be used directly
Bore hole colorimetric detection.We devise double fluorescent emission test paper based on gold nanoclusters and can be used for colorimetric detection Cu2+。
Invention content
The technical problem to be solved by the present invention is to：The double fluorescent emissions of gold nanoclusters base are constructed by the method for Electrostatic Absorption to try
Paper g-C3N4/ Au NCs/CS, the test paper have stable structure, it is environmental-friendly, it is easy to operate the features such as.
It is of the present invention to be used for Cu2+The preparation method of the double fluorescent emission test paper of the novel gold nanoclusters base of detection, step
It is rapid as follows：
(1) synthesis of gold nanoclusters：By HAuCl4Aqueous solution and stabilizer (reduced glutathione, oxidized form gluathione
Peptide, the amino acid containing sulfydryl, sulfur alcohol compound etc.) it is sufficiently mixed, wherein HAuCl4With the molar ratio 1 of stabilizer：1~6, it mixes
Close liquid 6~10h of continuous heating at 75~105 DEG C；Then to the alcohol that above-mentioned 3~5 times of mixed solution total volume is added in system
Class (methanol, ethyl alcohol, isopropanol, n-butanol, cyclohexanol, benzyl alcohol, ethylene glycol, 1,3-PD etc.) precipitating reagent, is used after centrifugation
Volume ratio is 1：The mixed liquor washing centrifugation product of 2~8 alcohol and water 3~5 times, centrifugation again obtains gold nanoclusters, Ran Houfen
It dissipates in water, configuration concentration is the gold nanoclusters solution of 0.1~0.8g/L；
(2) ultra-thin g-C3N4The preparation of nanometer sheet：Carboritride (melamine, urea etc.) is placed in Muffle furnace,
3~8h is heated at 450~700 DEG C, yellow g-C is made3N4Powder；Weigh the g-C of 30~80mg3N4Powder is dispersed in 50~
In 300mL water, ultrasound 8~12h of stripping is then centrifuged for removing precipitation, collects supernatant, obtain a concentration of 0.1~0.8mg/mL
Ultra-thin g-C3N4Nanometer sheet dispersion liquid, and store for future use in the dark；
(3) double transmitting g-C3N4The preparation of/Au NCs/CS fluorescent test papers：Chitosan (CS) is dissolved in volumetric concentration is
2%~10% acid (carbonic acid H2CO3, acetic acid CH3COOH, hydrosulphuric acid H2S, hypochlorous acid HClO, nitrous acid HNO2, sulfurous acid
H2SO3) aqueous solution in, stir until being completely dissolved, a concentration of 2~6g/100mL of chitosan in solution；Again by step (2)
The g-C of preparation3N4Nanometer sheet dispersion liquid in mass ratio 1：300~700 are added thereto, and stir evenly, by the system mixed in 30
10~30h is dried in vacuo at~60 DEG C, then impregnates drying with the trisodium citrate aqueous solution that mass concentration is 3%~8%
1~5h of film is washed with distilled water 3~5 times after taking-up, and blue-fluorescence film is obtained after dry, finally with concentration 0.1~
The Au NCs solution of 0.8g/L impregnates 20~60min, and the double fluorescent emission test paper g-C of gold nanoclusters base are obtained after dry3N4/Au
NCs/CS。
For the obtained double fluorescent emission test paper g-C of the present invention3N4/ Au NCs/CS, under 372nm ultraviolet excitations,
Double fluorescent emission effects of visible region 450nm blue lights and 596nm feux rouges are presented.Using double fluorescence for different copper ion concentrations
It is with different responses as a result, different composite fluorescence color change is presented, this double fluorescent emission test paper can be used for bore hole
The copper ion of colorimetric detection underwater trace, and detect limit can down to 10ppb, this be environmental protection and food security intermediate ion
It is convenient that detection provides.
The remarkable advantage of the present invention is：
1. preparation method is simple and practicable, raw material is cheap, easily realizes industrialization production.
2. obtained double fluorescent emissive materials are novel, there are the double fluorescent emissions of red blue, be very beneficial for being compared
Color detects.
3. being learnt by test experience result, which can realize to Cu2+Specific hypersensitive colorimetric detection, detection limit can
With down to 10ppb, and to the Cu of separate sources2+Detection result is all it is obvious that can realize to various Cu2+Detection, therefore
Test paper Cu in water2+Context of detection has great potential.
Description of the drawings
Fig. 1：Fluorescence excitation (Ex), transmitting (Em) and the ultraviolet suction of the gold nanoclusters of 1 gained red fluorescence of present example
Receive (Abs) spectrogram；The a length of 390nm optimal fluorescence emissions wavelength of optimum excitation wave for showing gold nanoclusters is the red of 596nm
Fluorescence；
Fig. 2：The transmission electron microscope photo of the gold nanoclusters of 1 gained red fluorescence of present example；Show gold nano
The size of cluster is about 1.7nm；
Fig. 3：(a) 1 gained (blue-fluorescence g-C of present example3N4Fluorescent emission (Em) and UV absorption (Abs) spectrum
Figure；(b) present invention gained blue-fluorescence g-C3N4Transmission electron microscope photo.Show g-C3N4Optimal absorption wavelength be
313nm, optimal fluorescence emission wavelength are the blue-fluorescence of 450nm.
Fig. 4：Double fluorescent emission sensing material detection various concentration Cu in present example 22+Fluorescence spectra.Show with
Cu2+Concentration increases, being basically unchanged of blue-fluorescence, and red fluorescence intensity reduces.
Fig. 5：Double fluorescent emission sensing material detection various concentration Cu in present example 22+Fluorescence photo.Show with
Cu2+Concentration increases, and it is composite coloured that double fluorescent emission sensing materials show different fluorescence.Cu is presented2+The function of Test paper.
Fig. 6：Double fluorescent emission sensing material detection separate sources Cu in present example 32+Fluorescence spectra.Show pair
The Cu of separate sources2+Fluorescence results are similar and can be detected.
Specific embodiment
Embodiment 1
(1), the synthesis of gold nanoclusters：By HAuCl4Aqueous solution (20mmol/L) 2mL is added in 18mL deionized waters, Xiang Qi
Middle addition 0.01842g reduced glutathiones, mixed liquor is in 90 DEG C of continuous heating 6.5h, then to adding in original volume 3 in system
Times isopropanol (60mL), 4000rpm centrifugation 10min, and with isopropyl alcohol and water (volume ratio 3：1) mixed liquor washs 3 times,
Centrifugal drying obtains 16mg gold nanoclusters again, is then dispersed in the gold nanoclusters solution that a concentration of 0.4g/L is obtained in 4mL water,
It refrigerates spare.
(2), ultra-thin g-C3N4The preparation of nanometer sheet：20g melamines are placed in 650 DEG C of heating 4h of Muffle furnace high temperature i.e.
G-C can be made3N4Then yellow powder weighs the g-C of 50mg3N4Yellow powder is scattered in 100mL water, ultrasound stripping
10.5h, then 11000rpm centrifugations 20min, removes precipitation, collects supernatant and obtains the ultra-thin g-C of a concentration of 0.15mg/mL3N4
Nanometer sheet dispersion liquid, and store for future use in the dark.
(3), double transmitting g-C3N4The preparation of/Au NCs/CS fluorescent test papers：2g chitosans (CS) are dissolved in 50mL volumes
In the aqueous solution of a concentration of 3% acetic acid, stir until being completely dissolved；The g-C again prepared by step (2)3N4Nanometer sheet dispersion liquid
In mass ratio 1：400 are added thereto, and stir evenly, and the system mixed is dried in vacuo for 24 hours at 45 DEG C, then dense with quality
The trisodium citrate aqueous solution spent for 5% impregnates dry film 0.5h, takes the film out and is washed with distilled water 3 times, drying is
Blue-fluorescence film is can obtain, finally 30min is impregnated with the Au NCs solution of concentration 0.4g/L, after dry, you can is obtained double glimmering
Light emitting test paper.
Embodiment 2
(1), the synthesis of gold nanoclusters：By HAuCl4Aqueous solution (20mmol/L) 3mL is added in 27mL deionized waters, Xiang Qi
Middle addition 0.03684g reduced glutathiones, mixed liquor is in 100 DEG C of continuous heating 7h, then to adding in original volume 4 in system
Times isopropanol (120mL), 5000rpm centrifugation 8min, and with isopropyl alcohol and water (volume ratio 4:1) mixed liquor washs 4 times,
Centrifugal drying obtains 28mg gold nanoclusters again, is then dispersed in the gold nanoclusters solution that a concentration of 0.4g/L is obtained in 7mL water,
It refrigerates spare.
(2), ultra-thin g-C3N4The preparation of nanometer sheet：15g melamines are placed in 600 DEG C of heating 5h of Muffle furnace high temperature i.e.
G-C can be made3N4Then yellow powder weighs the g-C of 40mg3N4Yellow powder is scattered in 80mL water, ultrasound stripping 12h, so
10000rpm centrifuges 25min afterwards, removes precipitation, collects supernatant and obtains the ultra-thin g-C of a concentration of 0.16mg/mL3N4Nanometer sheet water
Solution, and store for future use in the dark.
(3), double transmitting g-C3N4The preparation of/Au NCs/CS fluorescent test papers：3g chitosans (CS) are dissolved in 75mL volumes
In the aqueous solution of a concentration of 5% acetic acid, stir until being completely dissolved；The g-C again prepared by step (2)3N4Nanometer sheet dispersion liquid
In mass ratio 1：300 are added thereto, and stir evenly, and the system mixed is dried in vacuo 20h at 50 DEG C, then dense with quality
The trisodium citrate aqueous solution spent for 5% impregnates dry film 1h, takes the film out and is washed with distilled water 5 times, dry
Blue-fluorescence film is obtained, finally 40min is impregnated with the Au NCs solution of concentration 0.3g/L, after dry, you can obtains double fluorescence
Emit test paper.
(4), copper nitrate is detected.First configuration various concentration copper nitrate solution (50,500ppb and 5,50,
100ppm), the double transmitting fluorescent test papers prepared are cut into 0.5 × 1.0cm fritters, test paper is then dipped into various concentration
Copper nitrate solution in 1s, dried after taking-up, its photoluminescent property detected with Fluorescence Spectrometer, as a result such as Fig. 4, can detect copper from
Sub- concentration.The fluorescence imaging that test paper is obtained under wavelength 365nm ultra violet lamps can be used, as a result such as Fig. 5, shows that fluorescent test paper has
There is the function of bore hole colorimetric detection various concentration copper ion.
Embodiment 3
(1), the synthesis of gold nanoclusters：By HAuCl4Aqueous solution (20mmol/L) 4mL is added in 36mL deionized waters, Xiang Qi
Middle addition 0.03684g reduced glutathiones, mixed liquor is in 90 DEG C of continuous heating 8h, then to adding in 4 times of original volume in system
Isopropanol (160mL), 6000rpm centrifugation 5min, and with isopropyl alcohol and water (volume ratio 4:1) mixed liquor washs 4 times, then
Secondary centrifugal drying obtains 32mg gold nanoclusters, is then dispersed in the gold nanoclusters solution that a concentration of 0.4g/L is obtained in 8mL water, cold
It hides spare.
(2), ultra-thin g-C3N4The preparation of nanometer sheet：18g melamines are placed in 550 DEG C of heating 6h of Muffle furnace high temperature i.e.
G-C can be made3N4Then yellow powder weighs the g-C of 60mg3N4Yellow powder is scattered in 150mL water, ultrasound stripping 12h,
Then 8000rpm centrifuges 30min, removes precipitation, collects supernatant and obtains the ultra-thin g-C of a concentration of 0.12mg/mL3N4Nanometer sheet
Aqueous solution, and store for future use in the dark.
(3), double transmitting g-C3N4The preparation of/Au NCs/CS fluorescent test papers：3g chitosans (CS) are dissolved in 75mL volumes
In the aqueous solution of a concentration of 4% acetic acid, stir until being completely dissolved；The g-C again prepared by step (2)3N4Nanometer sheet dispersion liquid
In mass ratio 1：500 are added thereto, and stir evenly, and the system mixed is dried in vacuo 18h at 55 DEG C, then dense with quality
The trisodium citrate aqueous solution spent for 5% impregnates dry film 1.2h, takes the film out and is washed with distilled water 5 times, drying is
Blue-fluorescence film is can obtain, finally 20min is impregnated with the Au NCs solution of concentration 0.5g/L, after dry, you can is obtained double glimmering
Light emitting test paper.
(3), double transmitting g-C3N4The preparation of/Au NCs/CS fluorescent test papers：2g chitosans (CS) are dissolved in 50mL volumes
In the aqueous solution of a concentration of 3% acetic acid, stir until being completely dissolved；The g-C again prepared by step (2)3N4Nanometer sheet dispersion liquid
In mass ratio 1：400 are added thereto, and stir evenly, and the system mixed is dried in vacuo for 24 hours at 45 DEG C, then dense with quality
The trisodium citrate aqueous solution spent for 5% impregnates dry film 0.5h, takes the film out and is washed with distilled water 3 times, drying is
Blue-fluorescence film is can obtain, finally 30min is impregnated with the Au NCs solution of concentration 0.4g/L, after dry, you can is obtained double glimmering
Light emitting test paper.
(4), the copper ion of different chemical structures (copper nitrate, copper chloride, copper sulphate) is detected.It is respectively configured
It is small to be cut into 0.5 × 1.0cm by copper nitrate, copper chloride and the copper-bath of 100ppm for the double transmitting fluorescent test papers prepared
Then test paper is dipped into different chemical structures and contains Cu by block2+1s in solution, dries after taking-up, it is detected with Fluorescence Spectrometer
Photoluminescent property, as a result such as Fig. 6, to the Cu of separate sources2+Fluoroscopic examination result is similar, can detect the copper of different chemical structures from
Son.It can also use and the fluorescence imaging that test paper detects copper ion is obtained under wavelength 365nm ultra violet lamps.
Claims (6)
1. a kind of preparation method of the double fluorescent emission test paper of gold nanoclusters base, its step are as follows：
(1) synthesis of gold nanoclusters：By HAuCl4Aqueous solution and stabilizer are sufficiently mixed, wherein HAuCl4With mole of stabilizer
Than 1：1~6, mixed liquor 6~10h of continuous heating at 75~105 DEG C, then to adding in above-mentioned mixed solution total volume in system
3~5 times of alcohol precipitating agent, it is 1 that volume ratio is used after centrifugation：The mixed liquor washing centrifugation product of 2~8 alcohol and water 3~5 times,
Centrifugation obtains gold nanoclusters again, is then dispersed in water, and configuration concentration is the gold nanoclusters solution of 0.1~0.8g/L；
(2) ultra-thin g-C3N4The preparation of nanometer sheet：Carboritride is heated into 3~8h at 450~700 DEG C, yellow g-C is made3N4
Powder；Weigh the g-C of 30~80mg3N4Powder is dispersed in 50~300mL water, and ultrasound 8~12h of stripping, it is heavy to be then centrifuged for removing
It forms sediment, collects supernatant, obtain the ultra-thin g-C of a concentration of 0.1~0.8mg/mL3N4Nanometer sheet dispersion liquid；
(3) double fluorescent emission g-C3N4The preparation of/Au NCs/CS test paper：It is 2%~10% to dissolve chitosan in volumetric concentration
Acid aqueous solution in, stir until being completely dissolved, a concentration of 2~6g/100mL of chitosan in solution；Step (2) is made again
Standby g-C3N4Nanometer sheet dispersion liquid in mass ratio 1：300~700 are added thereto, and stir evenly, by the system mixed in 30~
10~30h is dried in vacuo at 60 DEG C, then impregnates the thin of drying with the trisodium citrate aqueous solution that mass concentration is 3%~8%
1~5h of film after taking-up and is washed with distilled water 3~5 times, and blue-fluorescence film is obtained after dry, finally with concentration 0.1~
The Au NCs solution of 0.8g/L impregnates 20~60min, and the double fluorescent emission test paper g-C of gold nanoclusters base are obtained after dry3N4/Au
NCs/CS。
2. a kind of preparation method of the double fluorescent emission test paper of gold nanoclusters base as described in claim 1, it is characterised in that：Stablize
Agent is reduced glutathione, oxidized form of glutathione, amino acid or sulfur alcohol compound containing sulfydryl；Alcohol precipitating agent is first
Alcohol, ethyl alcohol, isopropanol, n-butanol, cyclohexanol, benzyl alcohol, ethylene glycol or 1,3- propylene glycol.
3. a kind of preparation method of the double fluorescent emission test paper of gold nanoclusters base as described in claim 1, it is characterised in that：Carbon nitrogen
Compound is melamine or urea.
4. a kind of preparation method of the double fluorescent emission test paper of gold nanoclusters base as described in claim 1, it is characterised in that：Acid is
Carbonic acid, acetic acid, hydrosulphuric acid, hypochlorous acid, nitrous acid or sulfurous acid H2SO3。
5. a kind of double fluorescent emission test paper of gold nanoclusters base, it is characterised in that：It is as described in Claims 1 to 4 any one
Method is prepared.
6. the double fluorescent emission test paper of gold nanoclusters base described in claim 5 are in Cu2+Application in detection.
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