CN106596481A - Method for detecting Pb<2+> by use of boron-nitrogen-doped fluorescent carbon point probe - Google Patents
Method for detecting Pb<2+> by use of boron-nitrogen-doped fluorescent carbon point probe Download PDFInfo
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- CN106596481A CN106596481A CN201611107072.1A CN201611107072A CN106596481A CN 106596481 A CN106596481 A CN 106596481A CN 201611107072 A CN201611107072 A CN 201611107072A CN 106596481 A CN106596481 A CN 106596481A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
Abstract
The invention provides a method for detecting Pb<2+> by use of a boron-nitrogen-doped fluorescent carbon point probe. The method comprises steps as follows: (1) preparation of a fluorescent carbon point: the fluorescent carbon point is synthesized with a hydrothermal method on the basis of a carbon source containing boron and nitrogen; (2) multiple parts of probe solutions are taken, different contents of Pb<2+> are added to the probe solutions, and a linear detection relation is established according to difference of fluorescence intensity of the solutions containing different concentrations of Pb<2+>; (3) a probe solution which is equal to a standard solution in content is added to a to-be-detected solution containing Pb<2+>, the fluorescence intensity of the to-be-detected solution containing Pb<2+> is detected, and the content of Pb<2+> in the to-be-detected solution is obtained. The provided fluorescent carbon point probe has the characteristics of low biotoxicity, good biocompatibility, stable performance, cheap price, simple synthesis conditions and the like and is simple in detection process, low in energy consumption, high in selectivity, high in sensitivity and the like when used for detecting Pb<2+>.
Description
Technical field
The invention belongs to field of nanometer material technology, is related to a kind of fluorescent carbon point probe in detecting Pb of utilization boron N doping2+Side
Method.
Background technology
Used as the unique unwanted trace element of human body, stable and nondegradable pollutant, the content of lead is strictly monitored
It is very necessary.Research shows that lead can make the activated protein in brain deform inactivation, make related disorders or stopping, very
To making brain death.Lead is put aside in skeleton, can be to the blood system of human body, immune system, digestive system, nervous system etc.
Produce impact.Therefore, a kind of method of detection lead content is set up very urgent.At present, detect that the method for lead mainly has atom to inhale
Spectrographic method (AAS), inductively coupled plasma mass spectrometry (ICP-MS), Electrode with Electrochemical Impedance Spectroscopy are received, but these methods presence are time-consuming
Long, the features such as energy consumption is big, and uneconomical, and fluorescent spectrometry is used as a kind of low energy consumption, and sensitivity is high, the good method of selectivity,
Extensive concern is obtained in recent years.
Carbon point is a kind of dispersibility, is smaller in size than the spherical fluorescence carbon nano-particle of 10nm, except with traditional quantum
Point excellent optical performance outside, it also have good biocompatibility, hypotoxicity and it is cheap and easy to get the features such as, be widely used
In fields such as biomarker, bio-sensing, biological detection, opto-electronic device, environmental monitoring and catalysis.Boron, nitrogen are period of element
The element adjacent with carbon phase, has similar atomic radius to carbon in table.After mixing boron nitrogen, effectively can lack on modified carbon point surface
Fall into, improve its performance.At present, it has been reported that many nitrogenous carbon points, little energy and Pb2+Effect, but Pb2+But boron nitrogen can be made
The fluorescence intensity of doped carbon point is greatly enhanced, and using this property, can develop a kind of detection Pb2+Method.Also, it is fresh at present
It is rare using carbon point as probe detecting Pb2+Work, therefore, a kind of detection Pb is developed based on carbon point2+Method have one
Fixed application prospect.
The content of the invention
For above-mentioned the deficiencies in the prior art, the present invention provides a kind of fluorescent carbon point probe in detecting of utilization boron N doping
Pb2+Method, its test limit is relatively low, improves probe to Pb2+Selectivity, reduce the interference of background.
The technical scheme that the present invention is provided：A kind of fluorescent carbon point probe in detecting Pb of utilization boron N doping2+Method, including
Following steps：
(1) fluorescent carbon point is prepared:Using boracic, nitrogen and carbon compound as raw material, boracic, nitrogen and carbon compound raw material
For amino phenylboric acid or the mixture of boric acid, carbamide and glucose, in being dissolved in ultra-pure water, NaOH solution is added；
(2) mixed solution obtained in the step (1) is put in the reactor of politef, hydrothermal temperature is
120～200 DEG C, heat time heating time is 2～8h, is reacted using hydro-thermal method, then spin dialysis, prepares fluorescent carbon point probe molten
Liquid；
(3) preparation of standard working solution：Take the Pb of different volumes2+Stock solution, and be charged with being walked described in 10 μ L respectively
Suddenly the fluorescent carbon point probe solution that (2) obtain, then it is 2mL to be diluted to volume with the PBS buffer solution that pH is 4, forms one
Series standard working solution；
(4) with fluorophotometer under certain excitation wavelength, the fluorophotometer measures Pb2+Excitation wavelength be
360nm, or excitation wavelength is 460nm, and the fluorescence intensity of above-mentioned standard working solution is measured respectively, obtains fluorescence spectra, and
With Pb2+Concentration is abscissa, and the fluorescence intensity of standard working solution is vertical coordinate mapping, obtains Working calibration curve；
(5) Pb in sample2+Measure：It is past to contain Pb2+Solution to be measured in add with standard working solution content identical
Fluorescent carbon point probe solution, and survey its fluorescence intensity, so as to obtain solution to be measured in Pb2+Content.
Further, in step (1), the addition of the mixture of the amino phenylboric acid or boric acid, carbamide and glucose
Measure as 0.1～1g.
Further, the concentration of NaOH solution is 0.1～1mol/L in the step (1).
Further, Pb in the standard working solution2+Concentration range be 9～55nM, test limit is 0.18nM.
Further, the fluorophotometer measurement Pb for selecting in the step (4) neutralization procedure (5)2+Excitation wavelength be
360nm, launch wavelength is 430nm, or excitation wavelength is 460nm, and launch wavelength is 530nm.
Beneficial effects of the present invention：
(1) the water-soluble carbon point of present invention synthesis has the advantages that low price, stable performance, nontoxic, used as a kind of latent
Fluorescent marker be expected to be applied to the fields such as photoimaging, biomarker, chemical sensor, and it is in environmental analyses, life
Change the fields such as analysis, food safety and also there is more wide application prospect.
(2) it is of the present invention with boron N doping fluorescent carbon point as probe in detecting Pb2+Method, detection process is simple, sensitive
Degree is high, and detection limit is low.
(3) present invention detects Pb with conventional fluorescent method2+Except for the difference that, this probe can be 430nm and 530nm in launch wavelength
I.e. to Pb in two regions of blue light and green glow2+There is response, greatly improve probe to Pb2+Selectivity, reduce the dry of background
Disturb.
Description of the drawings
Fig. 1 is the fluorescent emission collection of illustrative plates for preparing carbon point of the embodiment of the present invention 1；
Fig. 2 is the uv-visible absorption spectra for preparing carbon point of the embodiment of the present invention 2；
Fig. 3 prepares carbon point as probe in detecting Pb for the embodiment of the present invention 32+Canonical plotting.
Fig. 4 prepares carbon point as probe in detecting Pb for the embodiment of the present invention 22+Selectivity test.
Specific embodiment
With reference to specific embodiment, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
The preparation method of the fluorescent carbon point of boron N doping, comprises the steps：
(1) 0.1g carbamide, 0.1g boric acid and 0.1g glucoses are dissolved in the ultra-pure water of 20mL, are stirred.Toward above solution
NaOH solution 1mL of middle addition 1mol/L, and mixed solution is transferred in reactor.
(2) 200 DEG C are heated to, after reaction 4h, spin dialysis is stand-by.Gained carbon point has unique photoluminescent property, transmitting
Spectrum changes with excitation wavelength and changes, with reference to Fig. 1.
The foundation of standard curve, comprises the steps：
(1) Pb of different volumes is taken2+Stock solution, and 10 μ L probe solutions are charged with respectively, then it is slow with the PBS that pH is 4
Rush solution and be diluted to volume for 2mL, formation standard solution.
(2) fluorescence intensity of above-mentioned standard solution is measured under the excitation wavelength of 360nm, respectively with fluorophotometer, is obtained
To fluorescence spectra.And with Pb2+Concentration is abscissa, and the fluorescence intensity of standard solution is vertical coordinate mapping, obtains standard curve.
The measure of actual sample, comprises the steps of：
By PBS solution that solution to be measured, pH are 4 and the mixing of 10 μ L probe solutions, using spectrofluorophotometer in 360nm
Excitation wavelength under, detect the fluorescence intensity of solution to be measured, in carrying it into standard curve, obtain Pb in solution to be measured2+Contain
Amount.
Embodiment 2
The preparation method of the fluorescent carbon point of boron N doping, comprises the steps：
(1) 0.5g amino phenylboric acids are dissolved in the ultra-pure water of 20mL, are stirred.Add 1.5mol/L's toward above solution
NaOH solution 0.8mL, and mixed solution is transferred in reactor.
(2) 180 DEG C are heated to, after reaction 6h, spin dialysis is stand-by.By being located in UV-visible absorption spectrum
Carbon point characteristic absorption peak at 235nm and 294nm, with reference to Fig. 2, it was demonstrated that the synthesis of carbon point.
The foundation of standard curve, comprises the steps：
(1) Pb of different volumes is taken2+Stock solution, and 10 μ L probe solutions are charged with respectively, then it is slow with the PBS that pH is 4
Rush solution and be diluted to volume for 2mL, formation standard solution.
(2) fluorescence intensity of above-mentioned standard solution is measured under the excitation wavelength of 460nm, respectively with fluorophotometer, is obtained
To fluorescence spectra.And with Pb2+Concentration is abscissa, and the fluorescence intensity of standard solution is vertical coordinate mapping, obtains standard curve.
The measure of actual sample, comprises the steps of：
By PBS solution that solution to be measured, pH are 4 and the mixing of 10 μ L probe solutions, using spectrofluorophotometer in 460nm
Excitation wavelength under, detect the fluorescence intensity of solution to be measured, in carrying it into standard curve, obtain Pb in solution to be measured2+Contain
Amount.
Further selectivity is done in the simultaneously detection to the fluorescent carbon point probe solution for preparing to different metal ions
Test, its result is as shown in figure 4, the fluorescent carbon point probe prepared using the present invention is only to Pb2+There is significant positive correlation to ring
Should, only Pb2+The fluorescence intensity of this probe can be made to be strengthened, above test result indicate that, using the present invention prepare fluorescent carbon
Point probe solution detects Pb2+Detection limit it is low, compared to general fluorescent probe, the present invention can detect the Pb of lower loading2+, and
Testing result is accurate.
Embodiment 3
The preparation method of the fluorescent carbon point of boron N doping, comprises the steps：
(1) 0.2g amino phenylboric acids are dissolved in the ultra-pure water of 20mL, are stirred.Add 1mL 1.2M's toward above solution
NaOH, and mixed solution is transferred in reactor.
(2) 160 DEG C are heated to, after reaction 8h, spin dialysis is stand-by.
The foundation of standard curve, comprises the steps：
(1) Pb of different volumes is taken2+Stock solution, and 10 μ L probe solutions are charged with respectively, then it is slow with the PBS that pH is 4
Rush solution and be diluted to volume for 2mL, formation standard solution.
(2) fluorescence intensity of above-mentioned standard solution is measured under the excitation wavelength of 460nm, respectively with fluorophotometer, is obtained
To fluorescence spectra.And with Pb2+Concentration is abscissa, and the fluorescence intensity of standard solution is vertical coordinate mapping, obtains standard curve.
Standard curve is with reference to Fig. 3.
The measure of actual sample, comprises the steps of：
By PBS solution that solution to be measured, pH are 4 and the mixing of 10 μ L probe solutions, using spectrofluorophotometer in 360nm
Excitation wavelength under, detect the fluorescence intensity of solution to be measured, in carrying it into standard curve, obtain Pb in solution to be measured2+Contain
Amount.
Compare with the nitrogen-doped carbon point reported, the carbon point of boron N doping is in Pb2+Context of detection has a clear superiority.This
The fluorescent carbon point of bright boron N doping is in the wave-length coverage of blue and green light so as to Fluorescence Increasing, and the nitrogen in the document reported
The carbon point of doping is general only to be responded in blue light, but in detection Pb2+What is had is not responding to, and what is had even can make fluorescent quenching, substantially
Can not be used for detecting Pb2+, the fluorescent carbon point detection Pb of boron N doping prepared by the present invention2+With good effect, test limit
Low, measurement result is accurate.
The detailed description of specific embodiments of the present invention is the foregoing is only, the present invention is not limited with this, it is all at this
Any modification, equivalent and improvement for being made in the mentality of designing of invention etc., should be included in protection scope of the present invention it
It is interior.
Claims (4)
1. a kind of fluorescent carbon point probe in detecting Pb of utilization boron N doping2+Method, it is characterised in that comprise the following steps：
(1) fluorescent carbon point is prepared:Using boracic, nitrogen and carbon compound as raw material, boracic, nitrogen and carbon compound raw material are ammonia
The mixture of base phenylboric acid or boric acid, carbamide and glucose, in being dissolved in ultra-pure water, adds NaOH solution；
(2) mixed solution obtained in the step (1) is put in the reactor of politef, hydrothermal temperature be 120～
200 DEG C, heat time heating time is 2～8h, is reacted using hydro-thermal method, then spin dialysis, prepares fluorescent carbon point probe solution；
(3) preparation of standard working solution：Take the Pb of different volumes2+Stock solution, and step (2) described in 10 μ L is charged with respectively
The fluorescent carbon point probe solution for obtaining, then it is 2mL to be diluted to volume with the PBS buffer solution that pH is 4, forms a series of marks
Quasi- working solution；
(4) with fluorophotometer under certain excitation wavelength, the fluorophotometer measures Pb2+Excitation wavelength be 360nm,
Or excitation wavelength is 460nm, and the fluorescence intensity of above-mentioned standard working solution is measured respectively, obtains fluorescence spectra, and with Pb2+It is dense
Spend for abscissa, the fluorescence intensity of standard working solution is vertical coordinate mapping, obtains Working calibration curve；
(5) Pb in sample2+Measure：It is past to contain Pb2+Solution to be measured in add with standard working solution content identical fluorescence
Carbon point probe solution, and survey its fluorescence intensity, so as to obtain solution to be measured in Pb2+Content.
2. fluorescent carbon point probe in detecting Pb of utilization boron N doping according to claim 12+Method, it is characterised in that：
In step (1), the addition of the mixture of the amino phenylboric acid or boric acid, carbamide and glucose is 0.1～1g.
3. fluorescent carbon point probe in detecting Pb of utilization boron N doping according to claim 12+Method, it is characterised in that：
The concentration of NaOH solution is 0.1～1mol/L in the step (1).
4. fluorescent carbon point probe in detecting Pb of the utilization boron N doping according to any one of claim 1-32+Method, it is special
Levy and be：Pb in the standard working solution2+Concentration range be 9～55nM, test limit is 0.18nM.
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Cited By (8)
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| CN108333158A (en) * | 2018-01-24 | 2018-07-27 | 深圳大学 | Codope fluorescent carbon quantum dot and synthetic method and the method for detecting ferro concentration in serum |
| CN108795423A (en) * | 2018-08-03 | 2018-11-13 | 吉林大学 | A kind of preparation method of high quantum production rate solid carbon dot fluorescent powder and its application in LED lamp bead |
| CN108844935A (en) * | 2018-07-06 | 2018-11-20 | 山西大同大学 | A kind of preparation method and application of the nitrogen co-doped carbon dots of boron |
| CN109187470A (en) * | 2018-09-10 | 2019-01-11 | 广西师范大学 | A kind of mediated with aptamers mixes silver-colored carbon dots catalysis H2O2The method of fluorescence spectrometry lead is reacted with TMB |
| CN110471098A (en) * | 2019-08-27 | 2019-11-19 | 广东医科大学 | Radon dose of radiation detection method based on carbon quantum dot biological sensor |
| CN111204736A (en) * | 2020-01-09 | 2020-05-29 | 中国科学院高能物理研究所 | Preparation of boron-containing carbon quantum dots and application of boron-containing carbon quantum dots in medicines for tumor diagnosis and boron neutron capture treatment |
| KR20200082609A (en) * | 2018-12-31 | 2020-07-08 | 가천대학교 산학협력단 | Method of preparing carbon quantum dots using amino acid s and method for detecting lead |
| CN111662710A (en) * | 2020-06-15 | 2020-09-15 | 山西大学 | Boron-nitrogen double-doped blue fluorescent carbon quantum dot and preparation method and application thereof |
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| CN108333158A (en) * | 2018-01-24 | 2018-07-27 | 深圳大学 | Codope fluorescent carbon quantum dot and synthetic method and the method for detecting ferro concentration in serum |
| CN108333158B (en) * | 2018-01-24 | 2020-12-08 | 深圳大学 | Double-doped fluorescent carbon quantum dot and synthetic method thereof |
| CN108844935A (en) * | 2018-07-06 | 2018-11-20 | 山西大同大学 | A kind of preparation method and application of the nitrogen co-doped carbon dots of boron |
| CN108844935B (en) * | 2018-07-06 | 2020-07-24 | 山西大同大学 | Preparation method and application of boron-nitrogen co-doped carbon dots |
| CN108795423A (en) * | 2018-08-03 | 2018-11-13 | 吉林大学 | A kind of preparation method of high quantum production rate solid carbon dot fluorescent powder and its application in LED lamp bead |
| CN108795423B (en) * | 2018-08-03 | 2020-06-30 | 吉林大学 | Preparation method of high-quantum-yield solid carbon dot fluorescent powder and application of fluorescent powder in LED lamp beads |
| CN109187470A (en) * | 2018-09-10 | 2019-01-11 | 广西师范大学 | A kind of mediated with aptamers mixes silver-colored carbon dots catalysis H2O2The method of fluorescence spectrometry lead is reacted with TMB |
| KR20200082609A (en) * | 2018-12-31 | 2020-07-08 | 가천대학교 산학협력단 | Method of preparing carbon quantum dots using amino acid s and method for detecting lead |
| KR102197222B1 (en) | 2018-12-31 | 2020-12-31 | 가천대학교 산학협력단 | Method of preparing carbon quantum dots using amino acid s and method for detecting lead |
| CN110471098A (en) * | 2019-08-27 | 2019-11-19 | 广东医科大学 | Radon dose of radiation detection method based on carbon quantum dot biological sensor |
| CN111204736A (en) * | 2020-01-09 | 2020-05-29 | 中国科学院高能物理研究所 | Preparation of boron-containing carbon quantum dots and application of boron-containing carbon quantum dots in medicines for tumor diagnosis and boron neutron capture treatment |
| CN111662710A (en) * | 2020-06-15 | 2020-09-15 | 山西大学 | Boron-nitrogen double-doped blue fluorescent carbon quantum dot and preparation method and application thereof |
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