CN107794039A - A kind of preparation and its application for being used to detect the boric acid carbon quantum dot of fluorine ion - Google Patents
A kind of preparation and its application for being used to detect the boric acid carbon quantum dot of fluorine ion Download PDFInfo
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Abstract
The present invention relates to a kind of preparation and its application for being used to detect the boric acid carbon quantum dot of fluorine ion, belong to novel nano-material preparing technical field.The present invention prepares comprising the following steps that for boric acid carbon quantum dot:By phenyl boric acid into water, after adjusting pH with NaOH solution, mixed solution is transferred in hydrothermal reaction kettle and reacted, centrifugal treating, you can obtain the boric acid carbon quantum dot with high-performance photoluminescent property.The invention provides a kind of preparation method of green, simple efficient boric acid carbon quantum dot fluorescence probe, boric acid carbon quantum dot is directly obtained by one step hydro thermal method, establishes a kind of synthetic method simple to operate, green is cheap.In addition, the boric acid carbon quantum dot prepared has good optical property and stability, also, pass through interstitial neighbour's hydroxyl structure material(Dopamine)Ability with Selective recognition and switching regulator detection fluorine ion.
Description
Technical field
The present invention relates to a kind of preparation and its application for being used to detect the boric acid carbon quantum dot of fluorine ion, belong to novel nano
Technical field of material.
Background technology
Fluorine element is widely distributed in nature, micro- necessary to be human body and animal body.Fluorine element is present in people
In the bone and tooth of body, its content and human body it is healthy closely related.The content of fluorine element is about 2-3 in general adult human body
G, the shortage of fluorine element easily triggers dental caries in human body, and Kaschin-Beck disease is formed when serious;Simultaneously excessive fluorine is absorbed in human body
Ion easily causes fluorosis of bone even life threatening.Wherein, it is the main source of fluorine element in human body to drink water and ingest, and passes through drink
The fluorine of water intake can but be absorbed by the body completely.The exceeded health that can have a strong impact on human body of content of fluoride in drinking water,
The World Health Organization(WHO)1.5 mg/L will be less than by defining the content of the fluoride in drinking water, and China is because of fluorine underground water
It is widely distributed, be world's fluorine poisoning than one of more serious country, it is specified that drinking water content of fluoride no more than 1.0
mg/L.Therefore, the detection method of effective fluorine ion is worked out to the healthy or all very urgent to environmental protection of human body.
Widely paid close attention to so the research to the detection method of fluorine ion receives people.The detection method of conventional fluorine ion have from
Son selection electrode method, chromatography, XRF etc..Although ion selective electrode method selectivity is good, detection is quick, sensitive
Degree is not high, is easily disturbed by environment temperature, potential drifting and other ions;Chromatographic preci-sion and accuracy is higher, still
Sample pretreatment is cumbersome, not easy to operate, and is primarily adapted for use in the scientific research in laboratory;And XRF has choosing because of it
Selecting property is good, high sensitivity, and operating method is easy, is quickly widely used.
In recent years, the XRF based on quantum dot fluorescence probe receives the extensive concern of researcher, because of it
There is high sensitivity, selectivity is good, apparatus structure is relatively easy, cheap, the fluorescence analysis method of foundation is
It is widely used in analysis field, such as measure inorganic matter, organic matter and large biological molecule.Quantum dot (Quantum
Dots, QDs) novel nano luminescent material is used as, it is the focus of research in recent years.Based on its unique characteristics of luminescence and optical physics
Property, available for establishing new quanta point biological sensing system.Quantum dot except with skin effect, bulk effect,
Outside Dielectric confinement effect, quantum size effect and macro quanta tunnel effect, also with absorption spectrum is wide, emission spectrum is narrow and this
The excellent optical properties such as lentor displacement is big.Therefore, quantum dot is successfully used for analysis detection, biomedical and fluorescence labeling
Deng field.
Carbon nano luminescent material is as a kind of emerging nano material, because there is hypotoxicity and hyperfluorescence property to receive for it
Increasingly closer concern.Wherein, boric acid carbon point by boron atom can with interstitial neighbour's hydroxyl structure compound on phenolic hydroxyl group
Oxygen is coordinated, and forms borate compound, and Photo-induced electron transfer process occurs for boric acid fluorescence probe, and fluorescence is quenched.So
After add fluorine ion, fluorine ion is coordinated rapidly with boron atom, and the hydroxyl in boron atom is left away, adjacent hydroxylated material and fluorine from
Hydrogen bond is formed between sub, neighbouring nitrogen-atoms, now the Photo-induced electron transfer process of boric acid fluorescent probe molecule is suppressed, glimmering
Light recovers.By boric acid and the covalent bond of Cis-hydroxyl groups compound and the complexing of fluorine ion, fluorescence intensity is utilized
Change intuitively embody object presence, so as to establish based on covalently bound specific recognition fluorescence analysis method, by it
Field is tested and analyzed applied to quantum dot fluorescence, nothing opens new road suspected of the area research.
Found through the literature search to prior art, Shen etc. was in 2014《Anal. Chem.》On deliver
“Synthesis-Modification Integration: One-Step Fabrication of Boronic Acid
Functionalized Carbon Dots for Fluorescent Blood Sugar Sensing " report boric acid carbon point
Synthesis and application.But this boric acid carbon point is only intended to detect blood glucose, the side with detecting fluorine ion is identified for switching regulator
Method is rarely reported.Therefore, using simple, green synthetic method synthesized high-performance boric acid carbon point and for switching regulator detection fluorine from
The research of son necessitates.
The content of the invention
It is an object of the invention to overcome technological deficiency present in prior art, such as:Solvent during detection fluorine ion
Consumption is big, and sample pretreatment is cumbersome, poor selectivity and sensitivity are low etc., and the present invention provides a kind of switching regulator that is used for and identifies and examine
The boric acid carbon quantum dot fluorescence probe of fluorine ion is surveyed, the boric acid carbon quantum dot fluorescence probe has good optical property and stably
Property, and with the ability of switching regulator detection fluorine ion.
The present invention also provides a kind of system that the boric acid carbon quantum dot fluorescence probe with detecting fluorine ion is identified for switching regulator
Preparation Method, specifically, the technical solution adopted by the present invention follows the steps below:
A certain amount of phenyl boric acid is dissolved into redistilled water, forms phenyl boric acid solution;Will with certain density NaOH solution
After phenyl boric acid solution is adjusted to the pH of certain value, mixed solution is obtained;Mixed solution is transferred to polytetrafluoroethyllining lining
In hydrothermal reaction kettle, N is passed through2For a period of time, reactor is placed in baking oven under certain temperature and reacts a period of time, be cooled to room
Temperature, you can obtain the dispersion liquid of boric acid carbon quantum dot fluorescence probe.By above-mentioned dispersion liquid centrifugal treating, supernatant is preserved, obtained
Boric acid carbon quantum dot fluorescence probe.
Wherein, the amount ratio of described phenyl boric acid and redistilled water is 0.1-2.0 g:30mL;The concentration of NaOH solution
For 0.1 mol/L;The pH of mixed solution is 7.0-11.0;Logical N2Time be 30min;Reaction temperature is 160-200 DEG C;Instead
It is 28-40 h between seasonable.
It is of the invention that a kind of answering for boric acid carbon quantum dot fluorescence probe for being identified for switching regulator and detecting fluorine ion is also provided
With by boric acid carbon quantum dot and excessive interstitial neighbour's hydroxylated material(Such as dopamine, catechol)Reaction makes boric acid carbon quantum dot
Fluorescent quenching, then with fluorescence recover experiment carries out switching regulator identification with quantitative analysis measure content of fluoride ion.
The principle of boric acid carbon quantum dot fluorescence probe switching regulator detection fluorine ion prepared by the present invention is as follows:
A kind of novel environment friendly, carbon amounts simple and easy to get and containing boric acid base group are successfully prepared by synthetic modification one-step method
Covalent the selection sexuality and fluorescent characteristic of boric acid carbon point fluorescence probe are combined and answered as fluorescence probe by son point CQDs
For the identification of fluorine ion, Photo-induced electron transfer process is occurred by boric acid and interstitial neighbour hydroxy compounds, is in CQDs
"off" state, Fluorescence-quenching occurs;Then matched somebody with somebody by the strong electronegativity of fluorine ion, fluorine ion with boron atom rapidly
, the hydroxyl in boron atom is left away, and now the Photo-induced electron transfer process of boric acid CQDs fluorescence probes is suppressed, and is made at CQDs
In "open" state, fluorescence occurs and recovers phenomenon, it is achieved thereby that switching regulator identification and detection fluorine ion.
The boric acid carbon quantum dot fluorescence probe of the present invention is mainly used in the measure of fluorine ion in the aqueous solution:
By the boric acid carbon quantum dot fluorescence probe stoste of preparation, interstitial neighbour's hydroxyl structure material(Dopamine, 5 mmol/L), it is to be measured
Object fluorine ion(5 mmol/L)Certain density storing solution is configured to respectively.60-200 μ L probe solution stoste is taken to add
Enter into colorimetric cylinder, and dopamine interstitial storing solution added into pipe, determine the fluorescence intensity of solution, add object fluorine from
Sub- storing solution, standard sample 8-12 that fluorinion concentration is 0-60 μM is configured to respectively, determines fluorescence spectrum.
Compared with prior art, beneficial effects of the present invention embody as follows:The technological merit of the present invention:
A kind of novel environment friendly, carbon amounts simple and easy to get and containing boric acid base group are successfully prepared by synthetic modification one-step method
Son point CQDs combines as fluorescence probe, and by covalent the selection sexuality and fluorescent characteristic of boric acid carbon quantum dot fluorescence probe
To be applied to the identification of fluorine ion.The carbon quantum dot containing boric acid base group is prepared by raw material of phenyl boric acid, not only there is green
The advantages that nontoxic, detection method is simple, high selectivity, it is thus also avoided that cumbersome modification.
It is that carbon point prepared by raw material makes its glimmering by the covalent bond effect of boric acid base group and interstitial dopamine by phenyl boric acid
Optical quenching, the complexing of boric acid base group and fluorine ion is recycled to realize the identification of its switching regulator and detection, this Fluorescence Increasing
Detection method can efficiently reduce experimental error, and the application of boric acid carbon point fluorescent optical sensor is obtained greatly
Expand.In addition, comprising only boric acid base group on the boric acid carbon quantum dot fluorescence probe prepared, property is stable, can greatly reduce
Influence of the interfering material to carbon quantum dot in environment.
Brief description of the drawings
Fig. 1:The transmission electron microscope picture of boric acid carbon quantum dot fluorescence probe;
Fig. 2:The dopamine of various concentrations represents concentration respectively with the fluorogram after the effect of boric acid carbon quantum dot fluorescence probe, a-h
Make for 0 μM, 10 μM, 20 μM, 30 μM, 40 μM, 50 μM, 60 μM, 70 μM of dopamine solution and boric acid carbon quantum dot fluorescence probe
Fluorescence intensity after;
Fig. 3:The fluorine ion of various concentrations and the fluorescence after boric acid carbon quantum dot fluorescence probe and the effect of dopamine mixed solution are extensive
Multiple figure, from bottom to up, every line represent respectively concentration as 0 μM, 5 μM, 10 μM, 15 μM, 20 μM, 25 μM, 30 μM, 35 μM, 40 μM,
45 μM, 50 μM, 55 μM, 60 μM of fluorine ion and the fluorescence after boric acid carbon quantum dot fluorescence probe and the effect of dopamine mixed solution
Intensity;
Fig. 4:It is relatively strong after the fluorine ion of various concentrations and boric acid carbon quantum dot fluorescence probe and the effect of dopamine mixed solution
Degree linear;
Fig. 5:Under same concentration(50 μmol/L)Different halogen species are molten to boric acid carbon quantum dot fluorescence probe and dopamine mixing
The quenching rate of liquid.
Embodiment
With reference to specific implementation example, the present invention will be further described.
Embodiment 1:
1.0 g phenyl boric acids are dissolved into 30 mL redistilled waters, is sufficiently stirred, is completely dissolved phenyl boric acid;Then with 0.1
The pH to 9.0 of mol/L NaOH solution regulation phenyl boric acid solution;Above-mentioned phenyl boric acid solution is transferred to in polytetrafluoroethylene (PTFE)
In 50 mL hydrothermal reaction kettles of lining, N is passed through2After 30 min, reactor is placed in baking oven, started to warm up from room temperature, 200
28 h are reacted at DEG C;Taken out with proximity gloves, after being cooled to room temperature, by obtained boric acid carbon quantum dot fluorescence probe dispersion liquid from
The heart, some big molecular impurities are removed, obtain the higher boric acid carbon quantum dot fluorescence probe of concentration, preserve stand-by under normal temperature, also may be used
Its low temperature is baked into the more convenient preservation of solid, due to the demand of this experiment, is not baked to preserve.
Embodiment 2:
2.0 g phenyl boric acids are dissolved into 30 mL redistilled waters, is sufficiently stirred, is completely dissolved phenyl boric acid;Then with 0.1
The pH to 7.0 of mol/L NaOH solution regulation phenyl boric acid solution;Above-mentioned phenyl boric acid solution is transferred to in polytetrafluoroethylene (PTFE)
In 50 mL hydrothermal reaction kettles of lining, N is passed through2After 30 min, reactor is placed in baking oven, started to warm up from room temperature, 160
40 h are reacted at DEG C;Taken out with proximity gloves, after being cooled to room temperature, by obtained boric acid carbon quantum dot fluorescence probe dispersion liquid from
The heart, some big molecular impurities are removed, obtain the higher boric acid carbon quantum dot fluorescence probe of concentration, preserve stand-by under normal temperature, also may be used
Its low temperature is baked into the more convenient preservation of solid, due to the demand of this experiment, is not baked to preserve.
Embodiment 3:
0.5 g phenyl boric acids are dissolved into 30 mL redistilled waters, is sufficiently stirred, is completely dissolved phenyl boric acid;Then with 0. 1
The pH to 11.0 of mol/L NaOH solution regulation phenyl boric acid solution;Above-mentioned phenyl boric acid solution is transferred to polytetrafluoroethylene (PTFE)
In 50 mL hydrothermal reaction kettles of liner, N is passed through2After 30 min, reactor is placed in baking oven, started to warm up from room temperature, 180
36 h are reacted at DEG C;Taken out with proximity gloves, after being cooled to room temperature, by obtained boric acid carbon quantum dot fluorescence probe dispersion liquid from
The heart, some big molecular impurities are removed, obtain the higher boric acid carbon quantum dot fluorescence probe of concentration, preserve stand-by under normal temperature, also may be used
Its low temperature is baked into the more convenient preservation of solid, due to the demand of this experiment, is not baked to preserve.
Fig. 1 is the transmission electron microscope picture of boric acid carbon quantum dot fluorescence probe.As seen from Figure 1, boric acid carbon quantum dot fluorescence
The size of probe is 3-5nm, without agglomeration, has good dispersiveness.
Fig. 2 is the dopamine of various concentrations and the fluorogram after the effect of boric acid carbon quantum dot fluorescence probe.As shown in Fig. 2
With the addition of dopamine interstitial, the gradual intensity of fluorescence of boric acid carbon quantum dot fluorescence probe gradually reduces, but adds 50 μM
After dopamine, the fluorescence intensity of boric acid carbon quantum dot fluorescence probe is preferably minimized, therefore, using 50 μM of dopamines as quenching boric acid
The optium concentration of the fluorescence of carbon quantum dot fluorescence probe.
Fig. 3 is glimmering after the fluorine ion of various concentrations acts on boric acid carbon quantum dot fluorescence probe and dopamine mixed solution
Light recovers figure.As shown in figure 3, when fluorinion concentration is from when increasing to 60 μM for 0 μM, with the increase for adding fluorinion concentration,
The fluorescence intensity of boric acid carbon quantum dot fluorescence probe gradually strengthens.
Application of the boric acid carbon quantum dot fluorescence probe of preparation in fluorine ion detection:
By the boric acid carbon quantum dot fluorescence probe of preparation(100 mg/L), dopamine interstitial( 5 mmol/L)And target to be measured
Thing sodium fluoride(5 mmol/L)Certain density storing solution is configured to respectively.Take 100 μ L boric acid carbon quantum dot fluorescence probe molten
Liquid and 50 μ L enter dopamine interstitial storing solution and are added in testing tube, and sodium fluoride storing solution is added into pipe, are configured to be fluorinated
Standard sample 6-10 that na concn is 0-60 μM, determines fluorescence spectrum.With the increase of concentration of sodium fluoride, on fluorescence spectrum
Fluorescent emission peak intensity is gradually increasing, according to Stern-Volmer equation (F0/F=1+Ksv[c]) with concentration [c] for horizontal seat
Mark, relative intensity of fluorescence (F0/ F) it is that ordinate draws fluorescence response curve.Several halogen species are selected, as a comparison material,
Participate in the research of boric acid carbon point fluorescence probe recognition performance.
Test example 1:Boric acid carbon quantum dot fluorescence probe is configured to the 100 mg/L aqueous solution, dopamine interstitial and target
Thing fluorine ion is each configured to the 5 mmol/L aqueous solution.Take the 100 μ L boric acid carbon quantum dot fluorescence probe aqueous solution and 50 μ L
Intermediate material aqueous dopamine solution is added in 5 mL colorimetric cylinders, and 3 min are stood after vibration, adds 0-60 μ L object fluorine
Solion, and with water constant volume, 20 min are stood after test fluid shaken at room temperature, the glimmering of solution is detected with sepectrophotofluorometer
Luminous intensity.According to Stern-Volmer equation (F0/ F=1+Ksv [c]) with concentration [c] for abscissa, relative intensity of fluorescence
(F0/F)Fluorescence response curve is drawn for ordinate.In colorimetric cylinder test fluid fluorinion concentration be respectively 0,2,5,10,20,30,
40th, 50,60 μm of ol/L, the fluorine ions of various concentrations is detected to boric acid carbon quantum dot fluorescence probe and dopamine mixed solution
The influence that fluorescence recovers.
As seen from Figure 4, according to Stern-Volmer equation (F0/F=1+Ksv[c]) with concentration [c] for horizontal seat
Mark, relative intensity of fluorescence (F0/ F) it is that ordinate draws fluorescence response curve, obtain corresponding equation:F/F0= 0.07172(CF -/µ
M) + 0.8677 (R2=0.9971), the range of linearity is 1.0-60 μm of ol/L, the results showed that, boric acid carbon quantum dot fluorescence is visited
It is high for the detection sensitivity of fluorine ion, it is not necessary to substantial amounts of solvent, longer detection time and tedious specimen preprocessing
Reason, there is the ability of good optical detection.
Test example 2:Boric acid carbon quantum dot fluorescence probe is configured to the 100 mg/L aqueous solution, dopamine interstitial and four kinds
Object fluorine ion, chlorion, bromide ion, iodide ion are each configured to the 5 mmol/L aqueous solution.Take 100 μ L boric acid carbon amounts
The son point fluorescence probe aqueous solution and the 50 μ L dopamine interstitial aqueous solution are added in 5 mL colorimetric cylinders, and 3 min are stood after vibration,
Add 50 μ L halide ion solution, and with water constant volume, 20 min are stood after test fluid shaken at room temperature, use fluorescence spectrophotometry
The fluorescence intensity of meter detection solution.As shown in figure 5, Cl-、Br-、I-Fluorescence amount of recovery(F/F0Value)Respectively 0.989,
1.108,0.926, and fluorine ion is 3.42 to the fluorescence amount of recovery of boric acid carbon quantum dot fluorescence probe;The fluorescence of fluorine ion recovers
Amount, which substantially compares other halide ions, to illustrate that boric acid carbon quantum dot fluorescence probe can utilize intermediate material to have fluorine ion greatly
Obvious specific recognition, fluorescence recovery effects are significantly higher than other halide ions.
Claims (8)
- A kind of 1. boric acid carbon quantum dot fluorescence probe, it is characterised in that the size of boric acid carbon quantum dot fluorescence probe is 3-5nm, There is no agglomeration.
- 2. the preparation method of boric acid carbon quantum dot fluorescence probe as claimed in claim 1, it is characterised in that including following step Suddenly:A certain amount of phenyl boric acid is dissolved into redistilled water, forms phenyl boric acid solution;Will with certain density NaOH solution After phenyl boric acid solution is adjusted to the pH of certain value, mixed solution is obtained;Mixed solution is transferred in hydrothermal reaction kettle, is passed through N2One The section time, reactor is placed in baking oven, a period of time is reacted under certain temperature, is cooled to room temperature, you can obtain boric acid carbon amounts The dispersion liquid of son point fluorescence probe;By above-mentioned dispersion liquid centrifugal treating, supernatant preserves, and obtains the spy of boric acid carbon quantum dot fluorescence Pin.
- 3. the preparation method of boric acid carbon quantum dot fluorescence probe according to claim 2, it is characterised in that phenyl boric acid with The amount ratio of redistilled water is 0.1-2.0 g:30mL;The concentration of NaOH solution is 0.1 mol/L.
- 4. the preparation method of boric acid carbon quantum dot fluorescence probe according to claim 2, it is characterised in that mixed solution Final pH be 7.0-11.0;Logical N2Time be 30 min.
- 5. the preparation method of boric acid carbon quantum dot fluorescence probe according to claim 2, it is characterised in that reaction temperature For 160-200 DEG C;Reaction time is 28-40 h.
- 6. boric acid carbon quantum dot fluorescence probe according to claim 1 is used to detect fluorine ion.
- 7. boric acid carbon quantum dot fluorescence probe according to claim 6 is used to detect fluorine ion, it is characterised in that by boric acid Carbon quantum dot is reacted with excessive interstitial neighbour hydroxylated material, makes the fluorescent quenching of boric acid carbon quantum dot, then recover to test with fluorescence It is identified and determines content of fluoride ion with quantitative analysis.
- 8. boric acid carbon quantum dot fluorescence probe according to claim 7 is used to detect fluorine ion, it is characterised in that between described Matter neighbour hydroxylated material is dopamine or catechol.
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CN109135735B (en) * | 2018-07-27 | 2021-04-20 | 中北大学 | Preparation method of water-soluble BCx quantum dots |
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