CN108083256A - The preparation method of high fluorescence property fluorescent carbon quantum dot and its in Cr（VI）Application in detection - Google Patents
The preparation method of high fluorescence property fluorescent carbon quantum dot and its in Cr（VI）Application in detection Download PDFInfo
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Abstract
The invention discloses the preparation method of high fluorescence property fluorescent carbon quantum dot, including step in detail below：A, will（0.1‑10 g）Citric acid and（0.1‑10 g）Glycine is dissolved in 1 20 mL water；B, autoclave is placed in baking oven and is heated for a period of hours rear cooled to room temperature under the high temperature conditions, obtain the dark brown suspension containing fluorescent carbon quantum dot；C, the dark brown suspension of gained is after being centrifuged off bulky grain, and by macroporous resin adsorption, the means of volume exclusion gel or dialysis using water as eluent crude product, purify fluorescent carbon quantum dot；D, purified product by under the conditions of 45 DEG C Rotary Evaporators concentrate, freeze, the fluorescent carbon quantum dot purified, be white powder.The present invention is at low cost, and preparation process is simply controllable, and gained carbon dots has high quantum yield, and fluorescence lifetime is long, has higher detection sensitivity and stability；Simple to operate, high sensitivity and selectivity is good, testing result is directly perceived, can quantify and detect.
Description
Technical field
Preparation and applied technical field more particularly to a kind of high fluorescence the present invention relates to high fluorescence property fluorescent optical sensor
The preparation method of performance fluorescent carbon quantum dot and its in Cr（VI）Application in detection.
Background technology
In the prior art, chromium is widely used industrial materials, and in the past few decades, industry and other artificial processes are not
It is disconnected to can be discharged into environment heavy metal ion, Cr（VI）It is noxious material, also causes in human body even at a low concentration a variety of
Carcinogenesis, the World Health Organization propose the Cr in drinking water the guide limit value of 0.05 mg/L, detect Cr（VI）So as to
Monitoring and reduction excess Cr（VI）The risk of intake, the risk particularly in beverage and food are very important, in recent years,
It has successfully developed and has much been used to measure the Cr in different sample substrates（VI）Analytical technology, such as spectrophotometry, light splitting
Fluorescence method, flame atomic absorption spectrometry, inductivity coupled plasma mass spectrometry, diffusing reflection-Fourier Transform Infrared Spectroscopy etc., so
And due to needing expensive equipment and complicated pretreatment, most of inconveniences in these methods limit them quick
Use in detection, hence it is highly desirable to develop for Cr（VI）Simple, sensitive, the method for selectivity and low cost of detection；
Fluorescent carbon quantum dot is a kind of new carbon nanomaterial, such as inexpensive due to its unique physics and chemical property, simply
Synthetic route, better biocompatibility, lower toxicity, high light and chemical stability, adjustable excitation and emission spectra, this
A little excellent performances make CD be used as very potential nano-sensor, and have been successfully used to pH, and metal ion and biology are big
The fluoroscopic examination of molecular substance, however, several shortcomings further applied there are still limitation fluorescent carbon quantum dot, on the one hand,
Mechanism in above-mentioned detection process（Such as fluorescence resonance energy transfer, electron energy transfer, metal-ligand charge transfer）It needs
The intermolecular interaction between chemical sensor and target molecule is wanted, hence this method is complicated and time-consuming longer, therefore
Practical application is limited, on the other hand, quantum yield is the key index of fluorescent material, is to determine whether luminescent material can be actual
The important foundation attribute of application, low quantum yield cause sensitivity relatively low in detecting system, this is to hinder fluorescence carbon quantum
One of the obstacle of point as fluorescent optical sensor, in order to overcome these shortcomings, it should synthesize the fluorescent carbon quantum dot of high quantum production rate
And design the fluorecence measurement system based on replacement mechanism, in inner filtering effect, due to absorbance variability index be transformed into
Fluorescence intensity change, in this way sensitivity enhancing and can be compared with other mechanism, the fluorescence based on inner filtering effect
Carbon quantum dot fluorecence measurement system is successfully developed, meanwhile, doping is to improve the effective ways of quantum yield, for example, B, N, S
The emission characteristic of carbon quantum dot can be improved with P, wherein, N doping is very effective one of method, therefore, develops high fluorescence
Performance fluorescent carbon quantum dot is used for Cr（VI）Detection have a very important significance.
The content of the invention
The object of the present invention is to provide a kind of preparation methods of high fluorescence property fluorescent carbon quantum dot.
Present invention technical solution used for the above purpose is：A kind of system of high fluorescence property fluorescent carbon quantum dot
Preparation Method, including step in detail below：
A, will（0.1-10 g）Citric acid and（0.1-10 g）Glycine is dissolved in 1-20 mL water；
B, autoclave is placed in baking oven and is heated for a period of hours rear cooled to room temperature under the high temperature conditions, obtained containing glimmering
The dark brown suspension of light carbon quantum dot；
C, the dark brown suspension of gained is after being centrifuged off bulky grain, by macroporous resin adsorption, volume exclusion gel or saturating
The means of analysis using water as eluent crude product, purify fluorescent carbon quantum dot；
D, purified product by under the conditions of 45 DEG C Rotary Evaporators concentrate, then freeze, the fluorescence carbon amounts purified
It is sub-, it is white powder.
The temperature of baking oven is 150 DEG C -250 DEG C in the step B.
Heating time is 5-50h to solution in an oven in the step B.
Volume exclusion gel is one in cross-link dextran, Ago-Gel and polyacrylamide gel in the step C
Kind is several.
Resin used in resin adsorption is D101 non-polar macroporous resins in the step C.
It is a further object of the present invention to provide a kind of high fluorescence property fluorescent carbon quantum dot in Cr（VI）Application in detection.
Present invention technical solution used for the above purpose is：A kind of high fluorescence property fluorescent carbon quantum dot is in Cr
（VI）Application in detection, comprises the following steps：
A, fluorescent carbon quantum dot is formulated as the fluorescent carbon quantum dot probe aqueous solution that concentration is 0.01-1 mg/mL, and configured
Know the Cr of concentration（VI）Solution；
B, Cr obtained into water and in previous step（VI）Fluorescent carbon quantum dot obtained in previous step is added in solution to visit
Pin aqueous solution, respectively as control group and experimental group, the fluorescence intensity in test experience group is compared with control group, according to Cr（VI）
Solution concentration and the modeling of corresponding fluorescent quenching intensity, obtain Cr（VI）Standard curve between concentration and fluorescence intensity；
C, Cr to be measured is taken（VI）Solution, to Cr to be measured（VI）Fluorescent carbon quantum dot probe water obtained in step A is added in solution
Solution, as Cr to be measured（VI）Solution example using the detection method identical with step B, obtains Cr to be measured（VI）Solution sample
The fluorescence intensity of product, with reference to the Cr obtained in step B（VI）Concentration and Standardization curve for fluorescence intensity obtain Cr to be measured（VI）Solution
The Cr of sample（VI）Concentration.
Cr in the step A（VI）Cr in solution（VI）Concentration be 0.1-1000 μM.
The Cr（VI）The preferred potassium bichromate solution of solution.
The concentration of fluorescent carbon quantum dot probe aqueous solution is preferably 0.05 mg/ml in the step A.
The actual conditions that fluorescence intensity detects in the step B is to cover the glimmering of 280-700 nm using Detection wavelength scope
Light spectrophotometer, excitation wavelength are 280-500 nm；The wavelength of fluorescence emission peak is 350-690 nm.
The excitation wavelength is preferably 340 nm, and launch wavelength is preferably 410 nm.
The preparation method of a kind of high fluorescence property fluorescent carbon quantum dot of the present invention and its in Cr（VI）Application in detection, it is glimmering
The preparation method of light carbon quantum dot, at low cost, preparation process is simply controllable, and gained carbon dots has high quantum yield, fluorescence longevity
Life length, has higher detection sensitivity and stability；The Cr of offer（IV）Fluorescence of the detection method based on fluorescent carbon quantum dot
Property utilizes Cr（IV）To carbon nano fluorescent quenching effect, Cr can be obtained（IV）The standard curve of concentration, and Cr（IV）Concentration is examined
High sensitivity is surveyed, detection is limited to 2.96 μM；The Cr of offer（IV）Concentration detection method has detection process side easy to operate
Just, high sensitivity and selectivity is good, testing result is directly perceived, can quantify the characteristics of detecting.
Description of the drawings
Fig. 1 is the preparation method of a kind of high fluorescence property fluorescent carbon quantum dot of the present invention and its in Cr（VI）Answering in detection
The transmission electron microscope photo of fluorescent carbon quantum dot prepared by embodiment one.
Fig. 2 is the preparation method of a kind of high fluorescence property fluorescent carbon quantum dot of the present invention and its in Cr（VI）Answering in detection
The grain size distribution of fluorescent carbon quantum dot prepared by embodiment one.
Fig. 3 is the preparation method of a kind of high fluorescence property fluorescent carbon quantum dot of the present invention and its in Cr（VI）Answering in detection
The Ultraluminescence spectrogram of middle fluorescent carbon quantum dot prepared by embodiment one.
Fig. 4 is the preparation method of a kind of high fluorescence property fluorescent carbon quantum dot of the present invention and its in Cr（VI）Answering in detection
The X- photoelectron spectroscopy figures of fluorescent carbon quantum dot prepared by embodiment one.
Fig. 5 is the preparation method of a kind of high fluorescence property fluorescent carbon quantum dot of the present invention and its in Cr（VI）Answering in detection
The infrared spectrogram of fluorescent carbon quantum dot prepared by embodiment one.
Fig. 6 is the preparation method of a kind of high fluorescence property fluorescent carbon quantum dot of the present invention and its in Cr（VI）Answering in detection
The standard curve of two fluorescent carbon quantum dot of embodiment detection Cr (IV).
Specific embodiment
As shown in Figures 1 to 6, the preparation method of high fluorescence property fluorescent carbon quantum dot, specifically includes following steps：A, will
（0.1-10 g）Citric acid and（0.1-10 g）Glycine is dissolved in 1-20 mL water；B, autoclave in baking oven in height
It is heated for a period of hours under the conditions of temperature and after cooled to room temperature, obtains the dark brown suspension containing fluorescent carbon quantum dot, wherein,
For the temperature range of baking oven at 150 DEG C -250 DEG C, baking oven heating time is 5 h-50 h；C, the dark brown suspension of gained is through centrifugation
After removing bulky grain, by macroporous resin adsorption, the means such as volume exclusion gel or dialysis are thick using water as eluent
Purification of products fluorescent carbon quantum dot, volume exclusion gel include：Sephadex cross-link dextrans, Sepharose agaroses coagulate
One or more of glue, Bio-Gel P polyacrylamide gels, resin used in resin adsorption are the nonpolar macroporous trees of D101
Fat；D, purified product by under the conditions of 45 DEG C rotary evaporation concentrate, then freeze, the fluorescence carbon quantum purified
Point is white powder；High fluorescence property fluorescent carbon quantum dot is in Cr（VI）Application in detection, comprises the following steps：A, by institute
It states fluorescent carbon quantum dot and is formulated as the fluorescent carbon quantum dot probe aqueous solution that concentration is 0.01-1 mg/mL；It configures a series of known
The Cr of concentration（VI）Solution, Cr（VI）Cr in solution（VI）Concentration range for 0.1-1000 μM, Cr（VI）The preferably heavy chromium of solution
Sour potassium solution, the concentration of fluorescent carbon quantum dot aqueous solution is preferably 0.05 mg/ml；B, into water and Cr is made in step A（VI）It is molten
Fluorescent carbon quantum dot aqueous solution made from step A is added in liquid, it is glimmering in test experience group respectively as control group and experimental group
Luminous intensity is compared with control group, according to Cr（VI）Solution concentration and the modeling of corresponding fluorescent quenching intensity, obtain Cr（VI）Concentration
Standard curve between fluorescence intensity, the actual conditions of fluorescence intensity detection are：280-700 is covered using Detection wavelength scope
The sepectrophotofluorometer of nm, excitation wavelength be 280-500 nm, it is preferable that excitation wavelength be 340 nm, the ripple of fluorescence emission peak
A length of 350-690 nm, it is preferable that launch wavelength is 410 nm；C, Cr to be measured is taken（VI）Solution, to the Cr to be measured（VI）Solution
The fluorescent carbon quantum dot aqueous solution made from middle addition step A, as Cr to be measured（VI）Solution example, using with step B phases
Same detection method, obtains Cr to be measured（VI）The fluorescence intensity of solution example, the Cr obtained with reference to step B（VI）Concentration and fluorescence
Strength criterion curve obtains Cr to be measured（VI）The Cr of solution example（VI）Concentration.
Embodiment one, the preparation of carbon namo fluorescence probe：By citric acid（0.35 g）And glycine（0.35 g）It is dissolved in 7
In mL water, then transfer the solution into poly-（Tetrafluoroethene）In the autoclave of-lining, it is small to heat 48 in an oven at 190 DEG C
When and cooled to room temperature after, obtain the dark brown suspension containing fluorescent carbon quantum dot, 4000 rpm centrifuge 10 minutes
After removing bulky grain, using D101 large pore resin absorption columns, water passes through as eluent crude product, fluorescent carbon quantum dot
Vacuum rotary evaporator concentrates, and then freezes, the fluorescent carbon quantum dot purified, is white powder, passes through transmission electron microscope TEM
（Such as Fig. 1）2.5 nm of particle favorable dispersibility and particle size average out to of detectable fluorescent carbon nano-particles, passes through fluorescence light
Compose ultraviolet spectra（Such as Fig. 2）The result is shown in 330 nm to have peak value to have n- π*The phenomenon that transition, passes through XPS（Such as Fig. 3）It was found that
Fluorescent carbon quantum dot mainly contains carbon, nitrogen, and three kinds of elements of oxygen pass through infrared spectrum（Such as Fig. 4）It was found that fluorescent carbon quantum dot surface
Mainly contain O-H,*O=C-O, C-O, and O=C-O*Group, it was demonstrated that contain the hydrophilic radicals such as hydroxyl, carboxyl in carbon dots surface.
Embodiment two, Cr（IV）The foundation of standard curve between concentration and fluorescence intensity：Fluorescence in Example one
Carbon quantum dot is configured to the carbon nano-particles solution that concentration is 0.05 g/ml, the carbon nano-particles solution that 1 ml is taken to prepare respectively
As blank control group；In addition the carbon nano-solution for being separately added into 1 ml preparations in 15 centrifuge tubes again is taken, then 15 centrifugations
5 ml Cr are sequentially added in pipe（IV）Concentration difference 5,10,20,30,40,50,60,70,80,90,100,
110,120,150,200,500,1000 μM of aqueous solution, after being sufficiently mixed, obtained carbon nano-particles and Cr（IV）
Standard solution stand 1 min after, the fluophotometer examination criteria solution of 280-700 nm is covered using Detection wavelength scope
In fluorescence intensity F1, testing conditions are that excitation wavelength is 340 nm, 410 nm of launch wavelength, the fluorescence intensity of blank control group
For F0 (excitation wavelength is 340 nm, 410 nm of launch wavelength), fluorescent quenching intensity is drawn out（（F0- F1）/ F0）With Cr
（IV）Standard curve between concentration is as shown in figure 5, equation of linear regression is（F0-F1）/ F0 = 0.00274x +
0.01637, R2=0.98, according to 3 σ standards（Signal-to-noise ratio）Calculate Cr（IV）Detection be limited to 2.96 μm of ol/L.
Embodiment three, the detection of actual sample：Fluorescent carbon quantum dot in Example one, using tap water as sample, and
Before analysis by 0.22 μm of membrane filtration, carbon dots concentration is 0.05 mg/mL, and the carbon that 1 ml pure water adds 1 ml to prepare is taken to receive
Rice corpuscles solution measures fluorescence intensity as F as blank control group0, it is that 1 ml concentration is 0.05 to take 1 ml of tap water and volume
Mg/ml carbon nano-particles mixing after fluorescence intensity F1, be according to equation of linear regression（F0-F1）/ F0 = 0.00274x
+ 0.01637, result of calculation is not detect.
Example IV, the detection of actual sample：Fluorescent carbon quantum dot in Example one, the Cr of 50 μM of configuration（IV）
Solion is sample, and before analysis by 0.22 μm of membrane filtration, carbon dots concentration is 0.05 mg/mL, takes 1 ml pure
Water adds the carbon nano-particles solution that 1 ml is prepared to measure fluorescence intensity as blank control group as F0, take 1 ml of tap water and body
Product is fluorescence intensity F after 0.05 mg/ml carbon nano-particles mix for 1 ml concentration1, it is according to equation of linear regression（F0-
F1）/ F0=0.00274x+0.01637, result of calculation are 60.4 μM, this rate of recovery is 120.8%.
Embodiment five, the detection of actual sample：Fluorescent carbon quantum dot in Example one, the Cr of 100 μM of configuration（IV）
Solion is sample, and before analysis by 0.22 μm of membrane filtration, carbon dots concentration is 0.05 mg/mL, takes 1 ml pure
Water adds the carbon nano-particles solution that 1 ml is prepared to measure fluorescence intensity as blank control group as F0, take 1 ml of tap water and body
Product is fluorescence intensity F after 0.05 mg/ml carbon nano-particles mix for 1 ml concentration1, it is according to equation of linear regression（F0-
F1）/ F0=0.00274x+0.01637, result of calculation are 60.4 μM, this rate of recovery is 120.8%.
Embodiment six, the detection of actual sample：Fluorescent carbon quantum dot in Example one, the Cr of 150 μM of configuration（IV）
Solion is sample, and before analysis by 0.22 μm of membrane filtration, carbon dots concentration is 0.05 mg/mL, takes 1 ml pure
Water adds the carbon nano-particles solution that 1 ml is prepared to measure fluorescence intensity as blank control group as F0, take 1 ml of tap water and body
Product is fluorescence intensity F after 0.05mg/ml carbon nano-particles mix for 1 ml concentration1, it is according to equation of linear regression（F0-
F1）/ F0=0.00274x+0.01637, result of calculation are 153.5 μM, this rate of recovery is 102.3%.
Claims (11)
1. a kind of preparation method of high fluorescence property fluorescent carbon quantum dot, which is characterized in that including step in detail below：
A, will（0.1-10 g）Citric acid and（0.1-10 g）Glycine is dissolved in 1-20 mL water；
B, autoclave is placed in baking oven and is heated for a period of hours rear cooled to room temperature under the high temperature conditions, obtained containing glimmering
The dark brown suspension of light carbon quantum dot；
C, the dark brown suspension of gained is after being centrifuged off bulky grain, by macroporous resin adsorption, volume exclusion gel or saturating
The means of analysis using water as eluent crude product, purify fluorescent carbon quantum dot；
D, purified product by under the conditions of 45 DEG C Rotary Evaporators concentrate, then freeze, the fluorescence carbon amounts purified
It is sub-, it is white powder.
2. a kind of preparation method of high fluorescence property fluorescent carbon quantum dot according to claim 1, it is characterised in that：It is described
The temperature of baking oven is 150 DEG C -250 DEG C in step B.
3. a kind of preparation method of high fluorescence property fluorescent carbon quantum dot according to claim 1, it is characterised in that：It is described
Heating time is 5-50h to solution in an oven in step B.
4. a kind of preparation method of high fluorescence property fluorescent carbon quantum dot according to claim 1, it is characterised in that：It is described
Volume exclusion gel is one or more of cross-link dextran, Ago-Gel and polyacrylamide gel in step C.
5. a kind of preparation method of high fluorescence property fluorescent carbon quantum dot according to claim 1, it is characterised in that：It is described
Resin used in resin adsorption is D101 non-polar macroporous resins in step C.
6. a kind of high fluorescence property fluorescent carbon quantum dot according to claim 1 is in Cr（VI）Application in detection, it is special
Sign is, comprises the following steps：
A, fluorescent carbon quantum dot is formulated as the fluorescent carbon quantum dot probe aqueous solution that concentration is 0.01-1 mg/mL, and configured
Know the Cr of concentration（VI）Solution；
B, Cr obtained into water and in previous step（VI）Fluorescent carbon quantum dot obtained in previous step is added in solution to visit
Pin aqueous solution, respectively as control group and experimental group, the fluorescence intensity in test experience group is compared with control group, according to Cr（VI）
Solution concentration and the modeling of corresponding fluorescent quenching intensity, obtain Cr（VI）Standard curve between concentration and fluorescence intensity；
C, Cr to be measured is taken（VI）Solution, to Cr to be measured（VI）Fluorescent carbon quantum dot probe water obtained in step A is added in solution
Solution, as Cr to be measured（VI）Solution example using the detection method identical with step B, obtains Cr to be measured（VI）Solution sample
The fluorescence intensity of product, with reference to the Cr obtained in step B（VI）Concentration and Standardization curve for fluorescence intensity obtain Cr to be measured（VI）Solution
The Cr of sample（VI）Concentration.
7. high fluorescence property fluorescent carbon quantum dot according to claim 6 is in Cr（VI）Application in detection, feature exist
In：Cr in the step A（VI）Cr in solution（VI）Concentration be 0.1-1000 μM.
8. high fluorescence property fluorescent carbon quantum dot according to claim 7 is in Cr（VI）Application in detection, feature exist
In：The Cr（VI）The preferred potassium bichromate solution of solution.
9. high fluorescence property fluorescent carbon quantum dot according to claim 6 is in Cr（VI）Application in detection, feature exist
In：The concentration of fluorescent carbon quantum dot probe aqueous solution is preferably 0.05 mg/ml in the step A.
10. high fluorescence property fluorescent carbon quantum dot according to claim 6 is in Cr（VI）Application in detection, feature exist
In：The actual conditions that fluorescence intensity detects in the step B is the fluorescence point for covering 280-700 nm using Detection wavelength scope
Light photometer, excitation wavelength are 280-500 nm；The wavelength of fluorescence emission peak is 350-690 nm.
11. high fluorescence property fluorescent carbon quantum dot according to claim 10 is in Cr（VI）Application in detection, feature
It is：The excitation wavelength is preferably 340 nm, and launch wavelength is preferably 410 nm.
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