CN110361371A - A kind of fluorescent optical sensor and its construction method and application based on N doping carbon dots and catalytic oxidation - Google Patents
A kind of fluorescent optical sensor and its construction method and application based on N doping carbon dots and catalytic oxidation Download PDFInfo
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- CN110361371A CN110361371A CN201910722827.6A CN201910722827A CN110361371A CN 110361371 A CN110361371 A CN 110361371A CN 201910722827 A CN201910722827 A CN 201910722827A CN 110361371 A CN110361371 A CN 110361371A
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Abstract
The invention discloses a kind of methods of fluorescent optical sensor detection copper ion, it is using N doping carbon dots as fluorescence probe, using copper ion can specificity catalysis oxidation cysteine form cystine and hydrogen peroxide, and further catalysis oxidation hydrogen peroxide generates the fluorescence that N doping carbon dots are quenched in hydroxyl radical free radical, and the fluorescent optical sensor of detection copper ion is constructed based on this.After addition various concentration copper ion is reacted, the fluorescence intensity of the fluorescent optical sensor is gradually quenched, therefore can be used for the quantitative detection of copper ion;Meanwhile the fluorescent optical sensor can also be applied to the measurement of content of copper ion in human serum.The present invention has many advantages, such as that easy to operate, applicability is wide, rapid reaction, and highly selective and highly sensitive quantitative analysis can be carried out to object.
Description
Technical field
The present invention relates to a kind of fluorescent optical sensor and its applications, belong to analytical chemistry and field of nanometer technology.
Background technique
Many transition metal ions play a crucial role in human life activity.In these metal ions,
Copper ion (Cu(II)) it is a kind of pair of essential bivalent cation of human body, it can help body to form red blood cell and serve as
The neurotransmitter of physiological function can also be used as the catalytic cofactor of various metalloenzyme, including superoxide dismutase, cell
Pigment c oxidizing ferment, tyrosinase and nuclease.When the intracorporal copper content of people occurs abnormal, have significantly to human health
Negative effect, excessive use Cu(II) oxidative stress and neurodegenerative disease, including alzheimer's disease, Parkinson can be caused
Disease, Men Kesi and hepatolenticular degeneration.Further, since extensive industrial application and agricultural application, Cu(II) have become master in environment
The heavy metal contaminants wanted.Since it is not biodegradable and is eventually accumulated in human body by food chain, open
A kind of accurate and sensitive strategy is issued to detect Cu(II) it is very necessary to human health.
Traditional Cu(II) detection means is the surface plasma resonance sensing based on graphite flame atomic absorption spectrometry
Device, inductively coupled plasma mass spectrometry, inductively coupled plasma atomic emission spectrometry, plasma resonance Rayleigh scattering
Spectrum etc..These methods all have quite high sensitivity, but its detection process is considerably complicated and needs expensive instrument
Device and well-trained personnel.In recent years, the advantages that fluorescent optical sensor is because of its non-destructive, cost-effectiveness height and high sensitivity by
To more and more concerns.
Fluorescent optical sensor is that one kind to specific analyte-sensitive and the property of can choose generates interaction with it, will
The variation of its concentration is converted to the molecular device of optical signalling or electrical signal variation output to be detected.Fluorescent optical sensor
Technology uses fluorophor, including inorganic material, such as up-conversion nano material, quantum dot, organic material, such as green fluorescence egg
The detection of the progress object such as white, red fluorescent protein or fluorescent dye.In recent years, fluorescent optical sensor is in some biological samples
It is widely used in the detection research of middle object.
N doping carbon dots (N-CDs) have become a kind of inexpensive, low toxicity, the novel light with good biocompatibility
Photoluminescence inorganic material is widely used in the detection of fluorescence sense and bioactive substance.109321237 A of patent CN
Disclose a kind of nitrogen sulphur codope carbon dots and its preparation method and application, comprising the following steps: with papermaking waste material lignin sulfonic acid
Sodium and cysteine are that raw material is placed in hydrothermal reaction kettle, carry out hydro-thermal reaction, are cooled to room temperature after reaction, by what is obtained
Black product centrifugation.The solvent portions membrane filtration of collection, the brown yellow solution obtained after filtering are blue-fluorescence carbon quantum
Point solution, the gained carbon quantum dot can be used for Fe in water body3+Analysis detection;And the invention discloses a kind of N doping carbon dots and
Preparation method and application, comprising the following steps: be placed in hydrothermal reaction kettle using urea and citric acid as raw material, it is anti-to carry out hydro-thermal
It answers, is cooled to room temperature after reaction, obtained product addition ethyl alcohol centrifugal purification is obtained.The gained N doping carbon dots are available
The analysis detection of Cu (II) in serum.The method of the present invention has following advantage in contrast: (1) only needing to mix in carbon dots
Miscellaneous nitrogen can be used to detect.Without adulterating two kinds of elements.(2) production N doping carbon dots operating procedure is simple, and the time used is shorter,
8 h are only needed,.(3) detection range of this method detection copper ion is wider, is 0.05 μM -100 μM.(4) ingredient is multiple in serum
Miscellaneous, the method for the present invention is selectively more preferable.
The present invention utilize using copper ion can specificity catalysis oxidation cysteine form cystine and hydrogen peroxide, and
Further catalysis oxidation hydrogen peroxide generates the fluorescence that N doping carbon dots are quenched in hydroxyl radical free radical, construct it is a kind of be suitable for copper from
The fluorescent optical sensor of son detection, and apply it to the detection of content of copper ion in human serum.
Summary of the invention
The problem that selectivity is bad existing for type fluorescent optical sensor is quenched for chelating copper ions by the present invention, proposes one kind
Fluorescent optical sensor based on catalytic oxidation, the cysteine in the fluorescent optical sensor can be catalyzed in specific manner by copper ion
Oxidation forms cystine and hydrogen peroxide, and further catalyzing hydrogen peroxide decomposes generation hydroxyl radical free radical destruction N doping carbon dots
Its fluorescence is quenched.After addition various concentration copper ion is reacted, the blue-fluorescence of fluorescent optical sensor can be made gradually to be quenched, from
And realize the highly selective and highly sensitive quantitative detection to copper ion.Meanwhile the fluorescent optical sensor applies also for human body blood
The quantitative detection of copper ion in clear.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of fluorescent optical sensor, be using N doping carbon dots as fluorescence probe, being capable of specificity catalysis oxidation half using copper ion
Cystine forms cystine and hydrogen peroxide, and further nitrogen-doped carbon is quenched in catalysis oxidation hydrogen peroxide generation hydroxyl radical free radical
The fluorescence of point, the fluorescent optical sensor of building detection copper ion.
The N doping carbon dots are using citric acid and urea as carbon source and nitrogen source, and water is solvent, the hydro-thermal at 160 DEG C
After reacting 8 h, obtained by addition ethyl alcohol centrifugal purification;Wherein, the mass ratio of citric acid and urea is 1:1;Urea and water
Mass volume ratio be 1:15 g/mL;The volume ratio of water and ethyl alcohol is 1:3.
The construction method of the fluorescent optical sensor are as follows: by N doping carbon dots solution and cysteine solution 1:1 by volume
It is stirred, the fluorescent optical sensor is made;Wherein, the concentration of N doping carbon dots solution is 50 μ g/mL, cysteine solution
Concentration be 1.2 mM.
A kind of application of the fluorescent optical sensor in quantitative detection copper ion, application method the following steps are included:
It is separately added into the copper ion standard solution of gradient concentration into the fluorescent optical sensor, uses fluorescence after 25 min of hybrid reaction
Spectrophotometric determination fluorescence intensity simultaneously draws the standard curve that fluorescence intensity changes with copper ion concentration.
A kind of application of the fluorescent optical sensor in human serum detection, including for content of copper ion in human serum
Detection, specifically includes the following steps:
The human serum that hospital acquires is added in the fluorescent optical sensor, after reacting 25 min, uses fluorescence spectrophotometry
Meter measurement fluorescence intensity, to realize the measurement to human serum content of copper ion.
The beneficial effects of the present invention are:
(1) the raw material N doping carbon dots used in the present invention are luminous materials a kind of convieniently synthesized and with excellent fluorescence property
Material, raw material are conveniently easy to get.
(2) fluorescent optical sensor of the present invention shows the variation of fluorescent quenching in response to various concentration copper ion, relative to
Type fluorescent optical sensor, which is quenched, in chelating copper ions has the advantages that selectivity is good, while having the advantages that easy to operate.
(3) quantitative detection of fluorescent optical sensor of the present invention copper ion suitable for human serum.
Detailed description of the invention
Fig. 1 is the schematic diagram that fluorescent optical sensor of the present invention detects content of copper ion.
Fig. 2 is the characterization map of N doping carbon dots of the present invention: (A) transmission electron microscope picture;(B) ultraviolet-ray visible absorbing
Spectrogram;(C) fluorescence excitation and emission spectra figure;(D) FTIR spectrum figure.
Fig. 3 is the figure of fluorescence intensity changes that fluorescent optical sensor of the present invention responds various concentration copper ion.
Fig. 4 is the selection Journal of Sex Research that fluorescent optical sensor of the present invention detects copper ion.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1: the synthesis of N doping carbon dots
1 g citric acid and 1 g urea ultrasonic dissolution, to solution clear, are transferred into 50 in the water of 15 mL first
In the polytetrafluoroethylene (PTFE) autoclave of mL volume, 8 h of heating reaction at 160 DEG C will after reaction kettle is cooled to room temperature
The ethyl alcohol that three times volume is added in products therefrom is uniformly mixed, and then 5000rpm centrifugation removes liquid and washs three repeatedly with ethyl alcohol
Secondary, the solid finally obtained is dried in vacuo to arrive solid crystal (the N doping carbon dots of N doping carbon dots with vacuum drying oven
Relevant characterization such as Fig. 2, wherein A be N doping carbon dots transmission electron microscope picture, show its particle diameter distribution be 2-3 nm;B mixes for nitrogen
The ultraviolet-visible absorption spectroscopy figure of miscellaneous carbon dots;C is the fluorescence excitation and fluorescence emission spectrogram of compound of N doping carbon dots;D is N doping
Fourier's external spectrum figure of carbon dots).
Embodiment 2: the building of the fluorescent optical sensor and specificity respond copper ion
1.2 mM cysteine solutions are added into 50 μ g/mL N doping carbon dots solution s in 1:1 by volume, and fluorescence is made and passes
Sensor.
Be separately added into gained fluorescent optical sensor gradient concentration copper ion standard solution (copper ion standard solution it is dense
Degree is followed successively by 0.05,0.1,0.5,1,2,4,6,9,15,20,25,40,60,80,100 μM), react 25 min fluorescence spectrophotometers
Photometric determination fluorescence intensity simultaneously draws fluorescence intensity change curve.(such as Fig. 2 be various concentration copper ion with react after it is glimmering
Intensity variation figure).
Embodiment 3: the detection of content of copper ion in human serum, specific step is as follows
The human serum that hospital acquires is added in the fluorescent optical sensor, after reacting 25 min, uses fluorescence spectrophotometry
Meter measurement fluorescence intensity, records data.Testing result shows that content of copper ion is 1.63 μM in the human serum measured.
Embodiment 3: the selectivity that fluorescent optical sensor detects copper ion
Interfering substance is separately added into fluorescent optical sensor, the concentration of copper ion is 20 μM, and the concentration of other interference substances is
200 μM.As shown in figure 4, from left to right be respectively blank, sodium ion, potassium ion, magnesium ion, zinc ion, calcium ion, aluminium from
Son, ferrous ion, iron ion, bovine serum albumin, lysine, vitamin B2, glucose, glutathione, ascorbic acid and copper from
Son.Its corresponding fluorescence intensity change as shown in figure 4, in addition to copper ion make fluorescent optical sensor fluorescence intensity be quenched other than, other
Interfering substance will not impact fluorescence intensity.As a result illustrate that the method for the invention prepares fluorescent optical sensor to copper ion
Detection have preferable selectivity.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (8)
1. it is a kind of based on N doping carbon dots and with the fluorescent optical sensor of catalytic oxidation, it is characterised in that: with N doping carbon dots
It is fluorescence probe, the hydroxyl radical free radical generated using cysteine and copper ion reaction as quencher, building detects the glimmering of copper ion
Optical sensor.
2. fluorescent optical sensor according to claim 1, it is characterised in that: the N doping carbon dots are with citric acid and urea
As carbon source and nitrogen source, water is solvent, at 160 DEG C after 8 h of hydro-thermal reaction, is obtained by the way that ethyl alcohol progress centrifugal purification is added
's.
3. fluorescent optical sensor according to claim 2, it is characterised in that: wherein, the mass ratio of citric acid and urea is 1:
1;The mass volume ratio of urea and water is 1:15 g/mL;The volume ratio of water and ethyl alcohol is 1:3.
4. a kind of construction method of fluorescent optical sensor as described in claim 1, it is characterised in that: the structure of the fluorescent optical sensor
Construction method are as follows: 1:1 is mixed by volume with cysteine solution by N doping carbon dots solution, and the fluorescence that detection copper ion is made passes
Sensor.
5. the construction method of fluorescent optical sensor according to claim 4, it is characterised in that: the concentration of N doping carbon dots solution
For 50 μ g/mL, the concentration of cysteine solution is 1.2 mM.
6. a kind of application of fluorescent optical sensor as described in claim 1 in quantitative detection copper ion, it is characterised in that: application side
Method is the following steps are included: be separately added into the copper ion standard solution of series of concentrations, hybrid reaction 25 into the fluorescent optical sensor
With fluorescent spectrophotometer assay fluorescence intensity and the standard curve that fluorescence intensity changes with copper ion concentration is drawn after min.
7. application of the fluorescent optical sensor in quantitative detection copper ion according to claim 6, it is characterised in that: be used for human body
The detection of Copper in Serum ion concentration.
8. application of the fluorescent optical sensor in quantitative detection copper ion according to claim 7, it is characterised in that: be used for human body
The detection of Copper in Serum ion concentration, comprising the following steps: the human serum that hospital acquires is added to the fluorescence sense
In device, after reacting 25 min, with fluorescent spectrophotometer assay fluorescence intensity, to realize the survey to human serum content of copper ion
It is fixed.
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