CN109777405A - A kind of red blue pair emits fluorescent carbon points and for detecting Al simultaneously3+And Cu2+The fluorescence analysis method of ion - Google Patents
A kind of red blue pair emits fluorescent carbon points and for detecting Al simultaneously3+And Cu2+The fluorescence analysis method of ion Download PDFInfo
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- CN109777405A CN109777405A CN201910108997.5A CN201910108997A CN109777405A CN 109777405 A CN109777405 A CN 109777405A CN 201910108997 A CN201910108997 A CN 201910108997A CN 109777405 A CN109777405 A CN 109777405A
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- 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
The present invention relates to a kind of red blue double transmitting fluorescent carbon points and for detecting Al simultaneously3+And Cu2+The fluorescence analysis method of ion.The preparation method of the fluorescent carbon point is that stem tea is ground into powder, it is added in reaction dissolvent and forms mixture, heating is reacted 1-24 hours at 140-250 DEG C after room temperature ultrasound, cooled to room temperature after reaction, it is centrifuged off big particle, then with 0.22 μm of filtering with microporous membrane, rotary evaporation removes solvent, up to red blue double transmitting fluorescent carbon points, it has the characteristics that the double transmittings of single excitation, highly sensitive can detect with high selectivity Al in the fluorescence enhancement of blue emitting area3+Ion concentration highly sensitive can detect with high selectivity Cu in the fluorescent quenching of red emitting area2+Ion concentration is detected and is not interfere with each other while two kinds of ions may be implemented.
Description
Technical field
The present invention relates to a kind of preparation methods of fluorescent carbon point, and detect Al based on fluorescent carbon point3+Ion and Cu2+From
The fluorescence analysis method of son.
Background technique
Aluminium is the most abundant metallic element of content in the earth, because it is with a variety of excellent performances, is usually used in space flight and aviation use
Aluminium, electronic appliance aluminium are packed for the industries such as aluminium and aluminium for building, aluminum aluminum sulfate and sulphur especially in food service industry
The use of sour aluminium ammonium, is exposed to the mankind for a long time in aluminum concentration environment.However, a large amount of research has proved aluminium in human body
Intake can cause serious health problem, such as Alzheimer disease, Parkinson and kidney failure disease.Therefore, aluminium ion contains
The accurate detection of amount has great importance for food safety and human health.
Copper ion is transition metal ions important in human body, its presence can be acted on certain protein into metal egg
It is white, play function in the form of enzyme, and these enzymes be all to life process it is vital, too high levels or it is too low all
Tremendous influence can be caused to body, lead to serious neurodegenerative disease, such as: Alzheimer disease and Wilson's disease.Therefore
The analysis method for establishing highly sensitive, highly selective detection copper ion is most important.
Currently, for Al3+Ion and Cu2+The detection of ion, usually using atomic absorption spectrography (AAS), inductive coupling etc. from
Sub- method, electrochemical process and chromatography etc., although some method sensitivity are higher, cumbersome operating process, complicated instrument and
Detection time length can limit its application to a certain extent.In comparison, the fluorescence analysis method based on fluorescent carbon point not only has
There are high sensitivity, easily operated, and the advantage simple with material preparation, specificity is good, therefore has been widely used for
The detection of metal ion.But so far, most of such probes are only used for the detection of single metal ion, and there has been no documents
Report about while detecting Al3+Ion and Cu2+The fluorescence analysis method of ion.For relatively single metal ion detection, it is based on
Detection while the polyion detection of double transmitting peak positions can more effectively realize two kinds and two or more metal ions, is conducive to
Actual analysis and practical application.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of red blue double transmitting fluorescent carbon points and for detecting Al simultaneously3+With
Cu2+The fluorescence analysis method of ion.
In order to solve the above technical problems, according to an aspect of the present invention, it provides a kind of red blue pair and emits fluorescent carbon points
Preparation method.
A kind of preparation methods of red blue double transmitting fluorescent carbon points are added to comprising steps of stem tea is ground into powder
Mixture is formed in reaction dissolvent, said mixture is transferred in autoclave, in 140- by room temperature ultrasound 5-15 min
Reaction 1-24 hours is heated at 250 DEG C, after reaction cooled to room temperature, be centrifuged off under the conditions of 8000-12000 rpm
Big particle, then with 0.22 μm of filtering with microporous membrane, rotary evaporation removing solvent is to get red blue double transmitting fluorescence
Carbon dots.
Further, the solvent is dehydrated alcohol, acetone or their mixed solution.
Further, the mixture 10 min of ultrasound at room temperature；After reaction terminates and is cooled to room temperature,
Big particle is centrifuged off under the conditions of 10000 rpm.
Further, red blue double transmitting fluorescent carbon points of acquisition, are dispersed into required concentration with dehydrated alcohol, 4 DEG C of preservations are standby
With.
According to a further aspect of the invention, a kind of red blue double transmitting fluorescence being prepared by one method of any of the above are provided
Carbon dots.
According to another aspect of the present invention, a kind of detection Al is provided3+The method of ion, comprising steps of
(1) by AlCl3It is dissolved in dehydrated alcohol, successively prepares the Al of various concentration3+Ion ethanol solution；It will be above-described
Red blue double transmitting fluorescent carbon points are distributed in dehydrated alcohol, obtain the fluorescent carbon point ethanol solution that concentration is 0.2 mg/mL；
(2) by the Al with various concentration3+Ion ethanol solution is added in 2.0 mL fluorescent carbon point ethanol solutions and is configured to
Mixed solution after reacting at room temperature 5 min of 1-, measures its fluorescence spectrum under 410 nm shooting conditions, draws 478 nm transmitted waves
Strong point ln(F/F0) and Al3+Standard curve between ion concentration；F0It is that there is no Al3+Fluorescence intensity when ion, F are to exist
Al3+Fluorescence intensity when ion；
(3) it takes fluorescent carbon point ethanol solution described in step (1), contain Al to be measured3+The ethanol solution of ion is configured to mix molten
Liquid is measured and is asked according to test condition described in step (2) and calculates ln(F/F0), the then standard curve according to step (2)
Calculate Al3+The concentration of ion.
According to another aspect of the present invention, a kind of detection detection Cu is provided2+The method of ion, comprising steps of
(1) by CuCl2It is dissolved in dehydrated alcohol, successively prepares the Cu of various concentration2+Ion ethanol solution；It will be above-described
Red blue double transmitting fluorescent carbon points are distributed in dehydrated alcohol, obtain the fluorescent carbon point ethanol solution that concentration is 0.2 mg/mL；
(2) by the Cu with various concentration2+Ion ethanol solution is added in 2.0 mL fluorescent carbon point ethanol solutions and is configured to mix
Solution is closed, after reacting at room temperature 30-120 min, its fluorescence spectrum is measured under 410 nm shooting conditions, draws 671 nm transmitting
Fluorescence intensity ratio F/F at wavelength0With Cu2+Standard curve between ion concentration；F0It is that there is no Cu2+Fluorescence intensity when ion, F
It is that there are Cu2+Fluorescence intensity when ion；
(3) it takes fluorescent carbon point ethanol solution described in step (1), contain Cu to be measured2+The ethanol solution of ion is configured to mix molten
Liquid is measured and is asked according to test condition described in step (2) and calculates F/F0, then the standard curve according to step (2) calculates
Cu2+The concentration of ion.
According to another aspect of the present invention, it provides a kind of while detecting Al3+Ion and Cu2+The method of ion, including step
It is rapid:
(1) by AlCl3It is dissolved in dehydrated alcohol, successively prepares the Al of various concentration3+Ion ethanol solution；By CuCl2Dissolution
In dehydrated alcohol, the Cu of various concentration is successively prepared2+Ion ethanol solution；By above-described red blue double transmitting fluorescent carbon points
It is distributed in dehydrated alcohol, obtains the fluorescent carbon point ethanol solution that concentration is 0.2 mg/mL；
(2) by the Al with various concentration3+Ion ethanol solution is added in 2.0 mL fluorescent carbon point ethanol solutions and is configured to
Mixed solution after reacting at room temperature 5 min of 1-, measures its fluorescence spectrum under 410 nm shooting conditions, draws 478 nm transmitted waves
Strong point ln(F/F0) and Al3+Standard curve between ion concentration；F0It is that there is no Al3+Fluorescence intensity when ion, F are to exist
Al3+Fluorescence intensity when ion；
By the Cu with various concentration2+Ion ethanol solution is added in 2.0 mL fluorescent carbon point ethanol solutions and is configured to mix
Solution after reacting at room temperature 30-120 min, measures its fluorescence spectrum under 410 nm shooting conditions, draws 671 nm transmitted waves
Strong point fluorescence intensity ratio F/F0With Cu2+Standard curve between ion concentration；F0It is that there is no Cu2+Fluorescence intensity when ion, F are
There are Cu2+Fluorescence intensity when ion；
(3) it takes fluorescent carbon point ethanol solution described in step (1), contain Al to be measured3+Ion and Cu2+The ethanol solution of ion is matched
Mixed solution is made, measures and asks respectively according to test condition described in step (2) and calculate Al3+The corresponding ln(F/F of ion0) and
Cu2+The corresponding F/F of ion0, then the standard curve according to step (2) calculates separately Al3+Ion and Cu2+Ion it is dense
Degree.
Further, in detection Al3+In the method for ion, in step (2), the reaction time is preferably 2 min of 1-.
Further, in detection Cu2+In the method for ion, in step (2), the reaction time is preferably 45-90 min.
The red indigo plant pair of one kind provided by the invention emits the preparations of fluorescent carbon points and for detecting Al simultaneously3+And Cu2+Ion
Fluorescence analysis method, compared with the prior art for, beneficial effect is: the 1. synthesis of fluorescence probe has that step is simple, green
The advantages that environmentally friendly, and the probe synthesized has the characteristics that the double transmittings of single excitation；2. the fluorescence enhancement of blue emitting area being capable of Gao Ling
It is quick to detect Al with high selectivity3+Ion concentration；3. the fluorescent quenching of red emitting area highly sensitive can detect with high selectivity
Cu2+Ion concentration；4. detecting and not interfereing with each other while two kinds of ions may be implemented.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of red blue double transmitting fluorescent carbon points.
Fig. 2 is the XPS photoelectron spectroscopy figure (a) and high-resolution C1s (b), O1s (c) of red blue double transmitting fluorescent carbon points
It is composed with N1s (d).
Fig. 3 is the emission spectrum in the presence of different metal ions.
Fig. 4 is the comparison of relative intensity of fluorescence in the presence of 671 nm transmitted wave strong point different metals.
Fig. 5 is the comparison of relative intensity of fluorescence in the presence of 478 nm transmitted wave strong point different metals.
Fig. 6 is different solvents to Al3+The influence of ion detection.
Fig. 7 is different solvents to Cu2+The influence of ion detection.
Fig. 8 is various concentration Al3+The fluorescence spectra of red blue double transmitting fluorescent carbon point ethanol solutions in the presence of ion.
Fig. 9 is Al3+The standard curve of ion detection.
Figure 10 is various concentration Cu2+The fluorescence spectra of red blue double transmitting fluorescent carbon point ethanol solutions in the presence of ion.
Figure 11 is Cu2+The standard curve of ion detection.
Specific embodiment
The preparation method of the red blue double transmitting fluorescent carbon points provided in a kind of typical embodiment of the present invention, including step
It is rapid: stem tea is ground into powder, is added in reaction dissolvent and forms mixture, room temperature ultrasound 5-15min, by above-mentioned mixing
Object is transferred in autoclave, heating reaction 1-24 hours at 140-250 DEG C, in the Reaction conditions range, heating temperature
Degree can be 140-160 DEG C, 160-180 DEG C, 180-200 DEG C, 200-220 DEG C, 220-240 DEG C；The heating reaction time can be
1-6 hours, 6-12 hours, 12-18 hours, 18-24 hours.Cooled to room temperature after reaction, 8000-12000 rpm
Under the conditions of be centrifuged off big particle, then use 0.22 μm of filtering with microporous membrane, rotary evaporation removing solvent to get described
Red blue double transmitting fluorescent carbon points.
According to embodiment of above, the red blue double transmitting fluorescent carbon points being prepared have the characteristics that the double transmittings of single excitation,
Highly sensitive Al can be highly selectively detected in blue emitting area3+Ion concentration, red emitting area can it is highly sensitive highly selectively
Detect Cu2+Ion concentration.And provided by the invention pair of transmitting carbon dots preparation method is simple, and it is at low cost, it is environmental-friendly.It was preparing
Cheng Zhong, stem tea can be the mixing of any one of black tea, green tea, dark green tea and other kind tealeaves or several tealeaves
Object.
In a preferred embodiment, the solvent is dehydrated alcohol, acetone or their mixed solution.
In a preferred embodiment, mixture ultrasound 10min at room temperature；Reaction terminates and is cooled to room temperature
Afterwards, big particle is centrifuged off under the conditions of 10000 rpm.
In a preferred embodiment, red blue double transmitting fluorescent carbon points of acquisition are dense needed for being dispersed into dehydrated alcohol
Degree, 4 DEG C save backup.
Based on above-described red blue double transmitting fluorescent carbon points in the fluorescence enhancement of blue emitting area, a kind of detection is provided
Al3+The fluorescence analysis method of ion concentration；Meanwhile it is sudden in the fluorescence of red emitting area based on red blue double transmitting fluorescent carbon points
It goes out, a kind of detection Cu is provided2+The fluorescence analysis method of ion concentration can obtain highly sensitive, highly selective detection effect.
Especially containing Al3+Ion and Cu2+In the mixed solution of ion, their content can be detected simultaneously, and do not interfere with each other.
Present embodiment provides a kind of detection Al3+The method of ion, comprising steps of
(1) by AlCl3It is dissolved in dehydrated alcohol, successively prepares the Al of various concentration3+Ion ethanol solution；It will be above-described
Red blue double transmitting fluorescent carbon points are distributed in dehydrated alcohol, obtain the fluorescent carbon point ethanol solution that concentration is 0.2 mg/mL；
(2) by the Al with various concentration3+Ion ethanol solution is added in 2.0 mL fluorescent carbon point ethanol solutions and is configured to
Mixed solution, after reacting at room temperature 5 min of 1-, preferably 2 min of 1-.Its fluorescence spectrum is measured under 410 nm shooting conditions,
Draw 478 nm transmitted wave strong point ln(F/F0) and Al3+Standard curve between ion concentration；F0It is that there is no Al3+It is glimmering when ion
Luminous intensity, F are that there are Al3+Fluorescence intensity when ion；
(3) it takes fluorescent carbon point ethanol solution described in step (1), contain Al to be measured3+The ethanol solution of ion is configured to mix molten
Liquid is measured and is asked according to test condition described in step (2) and calculates ln(F/F0), the then standard curve according to step (2)
Calculate Al3+The concentration of ion.
Present embodiment provides a kind of detection detection Cu2+The method of ion, comprising steps of
(1) by CuCl2It is dissolved in dehydrated alcohol, successively prepares the Cu of various concentration2+Ion ethanol solution；By the red indigo plant
Double transmitting fluorescent carbon points are distributed in dehydrated alcohol, obtain the fluorescent carbon point ethanol solution that concentration is 0.2 mg/mL；
(2) by the Cu with various concentration2+Ion ethanol solution is added in 2.0 mL fluorescent carbon point ethanol solutions and is configured to mix
Solution is closed, after reacting at room temperature 30-120 min, the reaction time is preferably 45-90 min.It is surveyed under 410 nm shooting conditions
Its fluorescence spectrum is measured, 671 nm transmitted wave strong point fluorescence intensity ratio F/F are drawn0With Cu2+Standard curve between ion concentration；F0It is
There is no Cu2+Fluorescence intensity when ion, F are that there are Cu2+Fluorescence intensity when ion；
(3) it takes fluorescent carbon point ethanol solution described in step (1), contain Cu to be measured2+The ethanol solution of ion is configured to mix molten
Liquid is measured and is asked according to test condition described in step (2) and calculates F/F0, then the standard curve according to step (2) calculates
Cu2+The concentration of ion.
Present embodiment provides one kind in Al3+Ion and Cu2+In Ar ion mixing solution, while detecting Al3+Ion and Cu2+
The method of ion, comprising steps of
(1) by AlCl3It is dissolved in dehydrated alcohol, successively prepares the Al of various concentration3+Ion ethanol solution；By CuCl2Dissolution
In dehydrated alcohol, the Cu of various concentration is successively prepared2+Ion ethanol solution；By above-described red blue double transmitting fluorescent carbon points
It is distributed in dehydrated alcohol, obtains the fluorescent carbon point ethanol solution that concentration is 0.2 mg/mL；
(2) by the Al with various concentration3+Ion ethanol solution is added in 2.0 mL fluorescent carbon point ethanol solutions and is configured to
Mixed solution, after reacting at room temperature 5 min of 1-, the reaction time is preferably 2 min of 1-.It is glimmering that its is measured under 410 nm shooting conditions
Light spectrum draws 478 nm transmitted wave strong point ln(F/F0) and Al3+Standard curve between ion concentration；F0It is that there is no Al3+From
The fluorescence intensity of the period of the day from 11 p.m. to 1 a.m, F are that there are Al3+Fluorescence intensity when ion；
By the Cu with various concentration2+Ion ethanol solution is added in 2.0 mL fluorescent carbon point ethanol solutions and is configured to mix
Solution, after reacting at room temperature 30-120 min, the reaction time is preferably 45-90 min.It is measured under 410 nm shooting conditions
Its fluorescence spectrum draws 671 nm transmitted wave strong point fluorescence intensity ratio F/F0With Cu2+Standard curve between ion concentration；F0It is not
There are Cu2+Fluorescence intensity when ion, F are that there are Cu2+Fluorescence intensity when ion；
(3) it takes fluorescent carbon point ethanol solution described in step (1), contain Al to be measured3+Ion and Cu2+The ethanol solution of ion is matched
Mixed solution is made, measures and asks respectively according to test condition described in step (2) and calculate Al3+The corresponding ln(F/F of ion0) and
Cu2+The corresponding F/F of ion0, then the standard curve according to step (2) calculates separately Al3+Ion and Cu2+Ion it is dense
Degree.
The embodiment of the present invention is illustrated below in conjunction with attached drawing, preferred embodiment described herein is merely to illustrate
It is of the invention with explaining, it is not intended to limit the present invention.
Embodiment one: the preparation of red blue double transmitting fluorescent carbon points
300 mg clovershrubs are ground into powder, are added in 10 mL acetone solvents, room temperature 10 min of ultrasound, by mixture
It is transferred in 25 mL autoclaves, heating reaction 1 hour at 180 DEG C, after reaction cooled to room temperature, 10000
Big particle is centrifuged off under the conditions of rpm, then with 0.22 μm of filtering with microporous membrane, rotary evaporation removing solvent is to get described
Red blue double transmitting fluorescent carbon points.It is dispersed into required concentration with dehydrated alcohol when use, 4 DEG C save backup.Red blue double transmittings are glimmering
For the pattern of light carbon dots as shown in Figure 1, torispherical pattern is presented, size is distributed in the nm of 2 nm ~ 4.With rhodamine 6G for 600-
Reference standard within the scope of 800 nm, prepared red blue double transmitting fluorescent carbon points are in acetone solvent, the amount of red transmitting band
Sub- yield is 6.06%, up to 8.93% in DMF solvent.It is the reference standard within the scope of 400-600 nm with Tiopronin,
For prepared red blue double transmitting fluorescent carbon points in alcohol solvent, the quantum yield of blue transmitting band is 0.80 %.Fig. 2 is shown
The photoelectron spectroscopy of prepared red blue double transmitting fluorescent carbon points shows that red blue double transmitting fluorescent carbon points include carbon, oxygen, three kinds of nitrogen
Element is primarily present C-H, C-C/C=C, C-N, C-OH, C=O, pyridine N, pyrroles N, graphitization N and N-H key.
Below using red blue double transmitting fluorescent carbon points prepared by the present embodiment as fluorescence probe study red transmitting band with
Blue transmitting band is to the selection performance and solvent of different metal ions to Cu2+Ion and Al3+The influence of ion detection.
(1) specificity of metal ion detection
The different metal ions ethanol solution for taking same concentrations is added separately to 2.0 mL and contains the bis- transmitting carbon dots of 0.2 mg/mL
Ethanol solution in, be configured to mixed solution, after reacting 30 min, measure the fluorescence emission spectrum under 410 nm excitation wavelengths.
As shown in Fig. 3, Fig. 4 and Fig. 5, at 671 nm, Cu2+The presence of ion can cause apparent fluorescent quenching, and other metals
The influence of ion can be ignored；At 478 nm, Al3+The presence of ion can cause apparent fluorescence enhancement, and other metals
The influence of ion is smaller, illustrates obtained red blue double transmitting fluorescent carbon points to Cu2+Ion and Al3+Ion is demonstrated by good
Performance is selected, can be used for the detection respectively of the two, do not generate any interference.
(2) solvent is to Cu2+Ion and Al3+The influence of ion detection
By same amount of AlCl3And CuCl2It is dissolved separately in DMSO, ethyl alcohol, acetone, DMF, acetonitrile and THF solvent, institute is made
Need stock solution.Double transmitting carbon dots solutions are also dissolved separately in DMSO, ethyl alcohol, acetone, DMF, acetonitrile and THF solvent, and institute is made
Need stock solution.Take same amount of above-mentioned Cu2+Ion or Al3+Ion DMSO solution is added separately to 2.0 mL and contains 0.2 mg/
In the DMSO solution of the bis- transmitting carbon dots of mL, it is configured to mixed solution, after reacting 30 min, is measured under 410 nm excitation wavelengths
Fluorescence emission spectrum.In addition several solvents such as ethyl alcohol, acetone, DMF, acetonitrile and THF is carried out by the above process.Such as Fig. 6 and figure
Shown in 7, in alcohol solvent, fluorescence intensity change is the most obvious, takes second place for acetone solvent.
Embodiment two: the preparation of red blue double transmitting fluorescent carbon points
500 mg Iron Guanyins are ground into powder, are added in 10 mL alcohol solvents, room temperature 10 min of ultrasound, by mixture
It is transferred in 25 mL autoclaves, heating reaction 3 hours at 200 DEG C, after reaction cooled to room temperature, 10000
Big particle is centrifuged off under the conditions of rpm, then with 0.22 μm of filtering with microporous membrane, rotary evaporation removing solvent is to get described
Red blue double transmitting fluorescent carbon points.It is dispersed into required concentration with dehydrated alcohol when use, 4 DEG C save backup.
Embodiment three: the preparation of red blue double transmitting fluorescent carbon points
1 Anhua g black brick tea is ground into powder, is added in 15 mL acetone solvents, room temperature 10 min of ultrasound, by mixture
It is transferred in 25 mL autoclaves, heating reaction 3 hours at 160 DEG C, after reaction cooled to room temperature, 10000
Big particle is centrifuged off under the conditions of rpm, then with 0.22 μm of filtering with microporous membrane, rotary evaporation removing solvent is to get described
Red blue double transmitting fluorescent carbon points.It is dispersed into required concentration with dehydrated alcohol when use, 4 DEG C save backup.
Example IV: the preparation of red blue double transmitting fluorescent carbon points
300 mg clovershrubs are ground into powder, are added in 10 mL acetone solvents, room temperature 5 min of ultrasound turn mixture
It moves in 25 mL autoclaves, heating reaction 24 hours at 140 DEG C, after reaction cooled to room temperature, 8000
Big particle is centrifuged off under the conditions of rpm, then with 0.22 μm of filtering with microporous membrane, rotary evaporation removing solvent is to get described
Red blue double transmitting fluorescent carbon points.It is dispersed into required concentration with dehydrated alcohol when use, 4 DEG C save backup.
Embodiment five: the preparation of red blue double transmitting fluorescent carbon points
300 mg clovershrubs are ground into powder, are added in 10 mL acetone solvents, room temperature 15 min of ultrasound, by mixture
It is transferred in 25 mL autoclaves, heating reaction 10 hours at 250 DEG C, after reaction cooled to room temperature,
Big particle is centrifuged off under the conditions of 12000 rpm, subsequent 0.22 μm of filtering with microporous membrane, rotary evaporation removes solvent, i.e.,
Obtain red blue double transmitting fluorescent carbon points.It is dispersed into required concentration with dehydrated alcohol when use, 4 DEG C save backup.
Embodiment six: Al3+The analysis detection of ion
The present embodiment is realized as fluorescence probe to Al using red blue double transmitting fluorescent carbon points prepared by embodiment one3+Ion
Analysis detection.
Step (1), by AlCl3It is dissolved in dehydrated alcohol, successively prepares the Al of various concentration3+Ion ethanol solution；It is red
Lan Shuan transmitting fluorescent carbon point is distributed in dehydrated alcohol, obtains the fluorescent carbon point ethanol solution that concentration is 0.2 mg/mL；
Step (2), by the Al with various concentration3+Ion ethanol solution is added to the above-mentioned fluorescent carbon point ethanol solution of 2.0 mL
It is configured to mixed solution, after reacting at room temperature 1 min, measures its fluorescence spectrum under 410 nm shooting conditions, as shown in Figure 8.So
Afterwards, 478 nm transmitted wave strong point ln(F/F are drawn0) and Al3+Standard curve between ion concentration, F0It is that there is no Al3+When ion
Fluorescence intensity, F is that there are Al3+Fluorescence intensity when ion.As the result is shown: Ln (F/F0) and Al3+Ion concentration is 0 ~ 20
μM and 25 ~ 100 μM within the scope of good linear relationship is presented.
Step (3) takes the fluorescent carbon point ethanol solution of 0.2 mg/mL, contains Al to be measured3+The ethanol solution of ion is configured to
Mixed solution measures its fluorescence spectrum under 410 nm shooting conditions, according to 478 nm launch wavelengths after reacting at room temperature 1 min
Locate ln(F/F0) and ln(F/F0) and Al3+Standard curve between ion concentration calculates Al3+Ion concentration.
Embodiment seven: Cu2+The analysis detection of ion
The present embodiment is realized as fluorescence probe to Cu using red blue double transmitting fluorescent carbon points prepared by embodiment one2+Ion
Analysis detection.
Step (1), by CuCl2It is dissolved in dehydrated alcohol, successively prepares the Cu of various concentration2+Ion ethanol solution；It is red
Lan Shuan transmitting fluorescent carbon point is distributed in dehydrated alcohol, obtains the fluorescent carbon point ethanol solution that concentration is 0.2 mg/mL；
Step (2), by the Cu with various concentration2+Ion ethanol solution is added to the above-mentioned fluorescent carbon point ethanol solution of 2.0 mL
In be configured to mixed solution, after reacting at room temperature 30 min, its fluorescence spectrum is measured under 410 nm shooting conditions, such as Figure 10 institute
Show.Then, 671 nm transmitted wave strong point fluorescence intensity ratio F/F are drawn0With Cu2+Standard curve between ion concentration；F0It is not deposit
In Cu2+Fluorescence intensity when ion, F are that there are Cu2+Fluorescence intensity when ion.As the result is shown: F/F0With Cu2+Ion concentration
Good linear relationship is presented within the scope of 0.1 ~ 50 μM.
Step (3) takes above-mentioned fluorescent carbon point ethanol solution, contains Cu to be measured2+The ethanol solution of ion is configured to mix molten
Liquid measures its fluorescence spectrum under 410 nm shooting conditions wait react at room temperature to 30 min, according to 671 nm transmitted wave strong points
Fluorescence intensity ratio F/F0And F/F0With Cu2+Standard curve between ion concentration calculates Cu2+Ion concentration.
Embodiment eight: while detecting Al3+Ion and Cu2+Ion
The present embodiment is realized as fluorescence probe to mixed solution using red blue double transmitting fluorescent carbon points prepared by embodiment one
Middle Al3+Ion and Cu2+The analysis detection of ion.
Step (1), by AlCl3It is dissolved in dehydrated alcohol, successively prepares the Al of various concentration3+Ion ethanol solution；It will
CuCl2It is dissolved in dehydrated alcohol, successively prepares the Cu of various concentration2+Ion ethanol solution；By red blue double transmitting fluorescent carbon points
It is distributed in dehydrated alcohol, obtains the fluorescent carbon point ethanol solution that concentration is 0.2 mg/mL；
Step (2), by the Al with various concentration3+Ion ethanol solution is added to the above-mentioned fluorescent carbon point ethanol solution of 2.0 mL
In be configured to mixed solution, after reacting at room temperature 5 min, its fluorescence spectrum is measured under 410 nm shooting conditions, draws 478 nm
Transmitted wave strong point ln(F/F0) and Al3+Standard curve between ion concentration；F0It is that there is no Al3+Fluorescence intensity when ion, F are
There are Al3+Fluorescence intensity when ion；
By the Cu with various concentration2+Ion ethanol solution is added in the above-mentioned fluorescent carbon point ethanol solution of 2.0 mL and is configured to
Mixed solution after reacting at room temperature 120 min, measures its fluorescence spectrum under 410 nm shooting conditions, draws 671 nm transmitted waves
Strong point fluorescence intensity ratio F/F0With Cu2+Standard curve between ion concentration；F0It is that there is no Cu2+Fluorescence intensity when ion, F are
There are Cu2+Fluorescence intensity when ion；
Step (3) takes fluorescent carbon point ethanol solution described in step (1), contains Al to be measured3+Ion and Cu2+The ethyl alcohol of ion is molten
Liquid is configured to mixed solution；After reacting at room temperature 5 min, part solution is taken to measure its fluorescence spectrum under 410 nm shooting conditions,
According to 478 nm transmitted wave strong point ln(F/F0) and ln(F/F0) and Al3+Standard curve between ion concentration calculates Al3+From
Sub- concentration.Wait react at room temperature to 120 min, remainder solution is taken to measure its fluorescence spectrum under 410 nm shooting conditions,
According to 671 nm transmitted wave strong point fluorescence intensity ratio F/F0And F/F0With Cu2+Standard curve between ion concentration calculates Cu2+From
Sub- concentration.
Embodiment nine: being in step (2) and step (3) with the difference of embodiment six, and the room temperature reaction time is 2min.
Embodiment ten: the difference with embodiment seven is in step (2) and step (3) that the room temperature reaction time is 45min.
Embodiment 11: the difference with embodiment eight is: analysis detection Al3+When ion concentration, step (2) and step
(3) in, the room temperature reaction time is 4min；Analysis detection Cu2+When ion concentration, in step (2) and step (3), when room temperature reaction
Between be 90min.
Claims (10)
1. a kind of preparation method of red blue double transmitting fluorescent carbon points, which is characterized in that comprising steps of by stem tea grind into powder
Shape is added in reaction dissolvent and forms mixture, and said mixture is transferred in autoclave by room temperature ultrasound 5-15min,
Heating reaction 1-24 hours at 140-250 DEG C, cooled to room temperature after reaction, under the conditions of 8000-12000 rpm from
The heart removes big particle, and then with 0.22 μm of filtering with microporous membrane, rotary evaporation removing solvent is to get the red Lan Shuanfa
Penetrate fluorescent carbon point.
2. according to the method described in claim 1, it is characterized by: the solvent is dehydrated alcohol, acetone or theirs is mixed
Close solution.
3. according to the method described in claim 1, it is characterized by: mixture ultrasound 10min at room temperature；Reaction knot
Beam and after being cooled to room temperature, is centrifuged off big particle under the conditions of 10000 rpm.
4. according to the method described in claim 1, it is characterized by: the red blue double transmitting fluorescent carbon points obtained, use dehydrated alcohol
It is dispersed into required concentration, 4 DEG C save backup.
5. red blue double transmitting fluorescent carbon points that -4 any one methods are prepared according to claim 1.
6. a kind of detection Al3+The method of ion, it is characterised in that: comprising steps of
(1) by AlCl3It is dissolved in dehydrated alcohol, successively prepares the Al of various concentration3+Ion ethanol solution；By claim 5
Red blue double transmitting fluorescent carbon points are distributed in dehydrated alcohol, and it is molten to obtain the fluorescent carbon point ethyl alcohol that concentration is 0.2 mg/mL
Liquid；
(2) by the Al with various concentration3+Ion ethanol solution is added in 2.0 mL fluorescent carbon point ethanol solutions and is configured to mix
Solution is closed, after reacting at room temperature 5 min of 1-, its fluorescence spectrum is measured under 410 nm shooting conditions, draws 478 nm launch wavelengths
Locate ln(F/F0) and Al3+Standard curve between ion concentration；F0It is that there is no Al3+Fluorescence intensity when ion, F are that there are Al3+
Fluorescence intensity when ion；
(3) it takes fluorescent carbon point ethanol solution described in step (1), contain Al to be measured3+The ethanol solution of ion is configured to mix molten
Liquid is measured and is asked according to test condition described in step (2) and calculates ln(F/F0), the then standard curve according to step (2)
Calculate Al3+The concentration of ion.
7. a kind of detection detects Cu2+The method of ion, which is characterized in that comprising steps of
(1) by CuCl2It is dissolved in dehydrated alcohol, successively prepares the Cu of various concentration2+Ion ethanol solution；By claim 5
Red blue double transmitting fluorescent carbon points are distributed in dehydrated alcohol, and it is molten to obtain the fluorescent carbon point ethyl alcohol that concentration is 0.2 mg/mL
Liquid；
(2) by the Cu with various concentration2+Ion ethanol solution is added in 2.0 mL fluorescent carbon point ethanol solutions and is configured to mix
Solution is closed, after reacting at room temperature 30-120 min, its fluorescence spectrum is measured under 410 nm shooting conditions, draws 671 nm transmitting
Fluorescence intensity ratio F/F at wavelength0With Cu2+Standard curve between ion concentration；F0It is that there is no Cu2+Fluorescence intensity when ion, F
It is that there are Cu2+Fluorescence intensity when ion；
(3) it takes fluorescent carbon point ethanol solution described in step (1), contain Cu to be measured2+The ethanol solution of ion is configured to mix molten
Liquid is measured and is asked according to test condition described in step (2) and calculates F/F0, then the standard curve according to step (2) calculates
Cu2+The concentration of ion.
8. a kind of detect Al simultaneously3+Ion and Cu2+The method of ion, which is characterized in that comprising steps of
(1) by AlCl3It is dissolved in dehydrated alcohol, successively prepares the Al of various concentration3+Ion ethanol solution；By CuCl2It is dissolved in
In dehydrated alcohol, the Cu of various concentration is successively prepared2+Ion ethanol solution；By red blue double transmitting fluorescence described in claim 5
Carbon dots are distributed in dehydrated alcohol, obtain the fluorescent carbon point ethanol solution that concentration is 0.2 mg/mL；
(2) by the Al with various concentration3+Ion ethanol solution is added in 2.0 mL fluorescent carbon point ethanol solutions and is configured to mix
Solution is closed, after reacting at room temperature 5 min of 1-, its fluorescence spectrum is measured under 410 nm shooting conditions, draws 478 nm launch wavelengths
Locate ln(F/F0) and Al3+Standard curve between ion concentration；F0It is that there is no Al3+Fluorescence intensity when ion, F are that there are Al3+
Fluorescence intensity when ion；
By the Cu with various concentration2+Ion ethanol solution be added in 2.0 mL fluorescent carbon point ethanol solutions be configured to mix it is molten
Liquid after reacting at room temperature 30-120 min, measures its fluorescence spectrum under 410 nm shooting conditions, draws 671 nm launch wavelengths
Locate fluorescence intensity ratio F/F0With Cu2+Standard curve between ion concentration；F0It is that there is no Cu2+Fluorescence intensity when ion, F are to deposit
In Cu2+Fluorescence intensity when ion；
(3) it takes fluorescent carbon point ethanol solution described in step (1), contain Al to be measured3+Ion and Cu2+The ethanol solution of ion is prepared
At mixed solution, measures and ask respectively according to test condition described in step (2) and calculate Al3+The corresponding ln(F/F of ion0) and Cu2+
The corresponding F/F of ion0, then the standard curve according to step (2) calculates separately Al3+Ion and Cu2+The concentration of ion.
9. the method according to claim 6 or 8, it is characterised in that: in detection Al3+In the method for ion, in step (2),
Reaction time is preferably 2 min of 1-.
10. method according to claim 7 or 8, it is characterised in that: in detection Cu2+In the method for ion, in step (2),
Reaction time is preferably 45-90 min.
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