CN110157422A - A kind of preparation method of amination carbon quantum dot - Google Patents
A kind of preparation method of amination carbon quantum dot Download PDFInfo
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- CN110157422A CN110157422A CN201910337299.2A CN201910337299A CN110157422A CN 110157422 A CN110157422 A CN 110157422A CN 201910337299 A CN201910337299 A CN 201910337299A CN 110157422 A CN110157422 A CN 110157422A
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Abstract
The invention discloses a kind of preparation method and applications of amination carbon quantum dot, belong to carbon quantum dot technical field.Histidine is dissolved in sodium hydroxide solution and is ultrasonically treated 5~15min by the present invention obtains mixed solution A；Mixed solution A is placed under the conditions of temperature is 180~220 DEG C and carries out 10~15h of hydro-thermal reaction, liquor B is obtained by filtration in cooled to room temperature；Liquor B is subjected to centrifugal treating, takes supernatant；Supernatant is dialysed through dialysis membrane, obtains amination carbon quantum dot solution, is stored in the refrigerator that temperature is 0~4 DEG C.The present invention serves as carbon source and nitrogen source with histidine, the amination carbon quantum dot of high-fluorescence quantum yield can be synthesized by one step hydro thermal method, method is easy, green, gained amination carbon quantum dot quantum yield with higher；During the present invention detects while the amination carbon quantum dot of synthesis is applied to electrochemistry and fluorescence, which has double stability, so that testing result is more acurrate reliable.
Description
Technical field
The present invention relates to a kind of preparation methods of amination carbon quantum dot, belong to carbon quantum dot technical field.
Background technique
Carbon quantum dot is a kind of zero dimension carbon nanomaterial, because its is nontoxic, environmental sound, good biocompatibility, valence
The advantages such as lattice are cheap, are liked by numerous researchers.Photoluminescent property is the most prominent feature of carbon quantum dot, but simple carbon amounts
Son point often has very low quantum yield, it is therefore desirable to which introducing hetero-atoms, such as nitrogen, sulphur improve its quantum yield.Carbon amounts
Son point is used as a kind of novel nano-material, has broad application prospects in fields such as catalysis, medicament transport, sensings.
Carbon quantum dot in terms of sensing using more and more, including Electrochemical Detection and fluorescence detection two major classes.Glimmering
In light detection, carbon quantum dot is chiefly used in detecting environmental contaminants, such as cation, anion, biomolecule and small molecule it is organic
Pollutant (herbicide/insecticide), but carbon quantum dot is seldom applied in Electrochemical Detection, let alone carbon quantum dot is answered simultaneously
In Electrochemical Detection and fluorescence detection.
Summary of the invention
It is numerous for the synthetic method of carbon quantum dot in the prior art, comprising: hydro-thermal method, solvent-thermal method, electrochemical process, micro-
Wave method, template method etc., but some methods are cumbersome, time-consuming, expensive, or even certain harm can be caused to environment
Technical problem, the present invention propose that a kind of preparation method of amination carbon quantum dot, amination carbon quantum dot of the invention have height
Fluorescence quantum yield can be applied to simultaneously in Electrochemical Detection and the double check of fluorescence detection.
A kind of preparation method of amination carbon quantum dot, the specific steps are as follows:
(1) histidine is dissolved in sodium hydroxide solution and is ultrasonically treated 10~15min and obtain mixed solution A；
(2) step (1) mixed solution A is placed under the conditions of temperature is 180~220 DEG C and carries out 10~15h of hydro-thermal reaction, from
It is so cooled to room temperature, liquor B is obtained by filtration；
(3) liquor B of step (2) is subjected to centrifugal treating, takes supernatant；
(4) supernatant of step (3) is dialysed through dialysis membrane, obtains amination carbon quantum dot solution, being stored in temperature is 0
In~4 DEG C of refrigerator.
The concentration of step (1) sodium hydroxide solution is 5~20mg/mL；Preferably 10mg/mL.
The solid-to-liquid ratio g:mL of step (1) histidine and sodium hydroxide solution is 1:(5~20).
The filter sizes of step (2) filtering are 0.05~0.65 μm.
The molecule interception of step (4) dialysis membrane is 500~1000Da.
Step (4) the dialysis membrane dialysis time is 18~36h.
The ultrasonic power is 15~30kHz；
The revolving speed of the centrifugal treating is 8000~12000r/min, and the time of centrifugal treating is 10~30min.
Preferably, the heating temperature in the step (2) is 200 DEG C, heating time 12h.
Application of the amination carbon quantum dot in electrochemistry and fluorescence detect simultaneously.
Beneficial effects of the present invention:
(1) present invention serves as carbon source and nitrogen source with histidine, can synthesize high-fluorescence quantum yield by one step hydro thermal method
Amination carbon quantum dot, raw materials used single, nontoxic, cheap, the hydrothermal synthesis method is easy, green, gained amino
Change carbon quantum dot quantum yield with higher；
(2) in being detected while the amination carbon quantum dot of synthesis is applied to electrochemistry and fluorescence by the present invention, the amino
Changing carbon quantum dot has double stability, so that testing result is more acurrate reliable.
Detailed description of the invention
Fig. 1 is that the TEM of 1 amination carbon quantum dot of embodiment schemes；
Fig. 2 is the grain size distribution of 1 amination carbon quantum dot of embodiment；
Fig. 3 is that the DPV of 1 amination carbon quantum dot Electrochemical Detection ascorbic acid of embodiment schemes；
When Fig. 4 is 1 amination carbon quantum dot fluorescence detection ascorbic acid of embodiment, fluorescence intensity is with ascorbic acid concentrations
Variation diagram.
Specific embodiment
Invention is further described in detail combined with specific embodiments below, but protection scope of the present invention is not limited to
The content.
Embodiment 1:
A kind of preparation method of amination carbon quantum dot, the specific steps are as follows:
(1) histidine is dissolved in sodium hydroxide solution and ultrasonic treatment 10min is obtained in the case where ultrasonic power is 20kHz
To mixed solution A；Wherein the concentration of sodium hydroxide solution is 10mg/mL, the solid-to-liquid ratio g:mL of histidine and sodium hydroxide solution
For 1:10；
(2) step (1) mixed solution A is placed under the conditions of temperature is 200 DEG C and carries out hydro-thermal reaction 12h, naturally cooled to
Room temperature is removed by filtration large particulate matter and obtains liquor B；The filter sizes wherein filtered are 0.22 μm；
(3) liquor B of step (2) is subjected to centrifugal treating, takes supernatant；Wherein the revolving speed of centrifugal treating is 10000r/
Min, the time of centrifugal treating are 20min；
(4) supernatant of step (3) is dialysed through dialysis membrane, obtains amination carbon quantum dot solution, being stored in temperature is 4
DEG C refrigerator in；Wherein the molecule interception of dialysis membrane is 500Da, and dialysis membrane dialysis time is for 24 hours；
Using quinine sulfate as standard, the quantum yield of gained amination carbon quantum dot, calculation formula are calculated are as follows:(Ф represents fluorescence quantum yield, and " ST " and " X " respectively represents quinine sulfate and ammonia
Base carbon quantum dot, Grad are the linear fit gradients obtained from the full spectrum of fluorescence intensity and absorbance figure, and η is the refraction of solvent
Rate), it is known that quantum yield of the quinine sulfate in 200~400nm excitation wavelength range is 0.54, calculates gained amination carbon amounts
The quantum yield of son point is 15.9%；
The TEM figure of the present embodiment amination carbon quantum dot is shown in that Fig. 1, the grain size distribution of amination carbon quantum dot are shown in Fig. 2, from
For Fig. 1 and Fig. 2 it is found that amination carbon quantum dot is spherical, and is uniformly distributed, particle size is 2~5nm；
The Electrochemical Detection of Ascorbic Acid
(1) successively use partial size that bright and clean mirror surface is presented for 0.3 and 0.05 μm of polishing powder polishing glass-carbon electrode to surface,
Naturally dry；
(2) chitosan solution that 5 μ L concentration are 5mg/mL, the glass carbon that modification to step (1) has been polished are drawn with liquid-transfering gun
On electrode, naturally dry；
(3) 5 μ L amination carbon quantum dot solution are drawn with liquid-transfering gun, modified on the glass-carbon electrode dried to step (2), from
So dry；
(4) use pH value for 4 phosphate buffer solution prepare a series of concentration gradients (0,10 μm of ol/L, 20 μm of ol/L,
40 μm of ol/L, 60 μm of ol/L, 80 μm of ol/L, 100 μm of ol/L, 200 μm of ol/L, 300 μm of ol/L, 400 μm of ol/L, 500 μm of ol/L,
600 μm of ol/L, 700 μm of ol/L, 800 μm of ol/L, 900 μm of ol/L, 1000 μm of ol/L) ascorbic acid solution；
It (5) is the modified electrode that is dried to electrode, step (3) for work by reference electrode, platinum electrode of calomel electrode
Electrode, various concentration ascorbic acid solution be electrolyte, test DPV curve；
The present embodiment DPV curve is shown in Fig. 3, and as can be seen from Figure 3, current signal changes with the variation of ascorbic acid concentrations,
And current signal and ascorbic acid concentrations correlation；
The fluorescence detection of Ascorbic Acid
(1) use pH value for 4 phosphate buffer solution prepare a series of concentration gradients (0,10 μm of ol/L, 20 μm of ol/L,
30 μm of ol/L, 40 μm of ol/L, 50 μm of ol/L, 60 μm of ol/L, 70 μm of ol/L, 80 μm of ol/L, 90 μm of ol/L, 100 μm of ol/L) it is anti-
Bad hematic acid solution；
(2) it is separately added into 100 μ L amination carbon quantum dot solution in 11 10mL colorimetric cylinders, then is separately added into 100 μ L
A series of ascorbic acid solution of concentration gradients in step (1) is settled to 5mL with the phosphate buffer solution that pH value is 4；
(3) with the fluorescence intensity of solution in 11 colorimetric cylinders in Fluorescence Spectrometer determination step (2)；
When the present embodiment amination carbon quantum dot fluorescence detection ascorbic acid, fluorescence intensity with ascorbic acid concentrations variation
Figure is shown in Fig. 4, and as can be seen from Figure 4, the fluorescence intensity of amination carbon quantum dot weakens with the increase of ascorbic acid concentrations, illustrates anti-
The fluorescence of carbon quantum dot can be quenched in bad hematic acid.
Embodiment 2:
A kind of preparation method of amination carbon quantum dot, the specific steps are as follows:
(1) histidine is dissolved in sodium hydroxide solution and ultrasonic treatment 15min is obtained in the case where ultrasonic power is 15kHz
To mixed solution A；Wherein the concentration of sodium hydroxide solution is 10mg/mL, the solid-to-liquid ratio g:mL of histidine and sodium hydroxide solution
For 1:5；
(2) step (1) mixed solution A is placed under the conditions of temperature is 180 DEG C and carries out hydro-thermal reaction 15h, naturally cooled to
Liquor B is obtained by filtration in room temperature；The filter sizes wherein filtered are 0.35 μm；
(3) liquor B of step (2) is subjected to centrifugal treating, takes supernatant；Wherein the revolving speed of centrifugal treating is 8000r/
Min, the time of centrifugal treating are 30min；
(4) supernatant of step (3) is dialysed through dialysis membrane, obtains amination carbon quantum dot solution, being stored in temperature is 0
DEG C refrigerator in；Wherein the molecule interception of dialysis membrane is 800Da, and dialysis membrane dialysis time is 28h；
Using quinine sulfate as standard, the quantum yield of gained amination carbon quantum dot, calculation formula are calculated are as follows:(Ф represents fluorescence quantum yield, and " ST " and " X " respectively represents quinine sulfate and ammonia
Base carbon quantum dot, Grad are the linear fit gradients obtained from the full spectrum of fluorescence intensity and absorbance figure, and η is the refraction of solvent
Rate), it is known that quantum yield of the quinine sulfate in 200~400nm excitation wavelength range is 0.54, calculates gained amination carbon amounts
The quantum yield of son point is 7.8%；
The Electrochemical Detection of Ascorbic Acid
(1) successively use partial size that bright and clean mirror surface is presented for 0.3 and 0.05 μm of polishing powder polishing glass-carbon electrode to surface,
Naturally dry；
(2) chitosan solution that 5 μ L concentration are 5mg/mL, the glass carbon that modification to step (1) has been polished are drawn with liquid-transfering gun
On electrode, naturally dry；
(3) 5 μ L amination carbon quantum dot solution are drawn with liquid-transfering gun, modified on the glass-carbon electrode dried to step (2), from
So dry；
(4) use pH value for 4 phosphate buffer solution prepare a series of concentration gradients (0,10 μm of ol/L, 20 μm of ol/L,
40 μm of ol/L, 60 μm of ol/L, 80 μm of ol/L, 100 μm of ol/L, 200 μm of ol/L, 300 μm of ol/L, 400 μm of ol/L, 500 μm of ol/L,
600 μm of ol/L, 700 μm of ol/L, 800 μm of ol/L, 900 μm of ol/L, 1000 μm of ol/L) ascorbic acid solution；
It (5) is the modified electrode that is dried to electrode, step (3) for work by reference electrode, platinum electrode of calomel electrode
Electrode, various concentration ascorbic acid solution be electrolyte, test DPV curve；
As the result is shown with embodiment 1, current signal changes with the variation of ascorbic acid concentrations, and current signal and anti-
Bad hematic acid concentration correlation；
The fluorescence detection of Ascorbic Acid
(1) use pH value for 4 phosphate buffer solution prepare a series of concentration gradients (0,10 μm of ol/L, 20 μm of ol/L,
30 μm of ol/L, 40 μm of ol/L, 50 μm of ol/L, 60 μm of ol/L, 70 μm of ol/L, 80 μm of ol/L, 90 μm of ol/L, 100 μm of ol/L) it is anti-
Bad hematic acid solution；
(2) it is separately added into 100 μ L amination carbon quantum dot solution in 11 10mL colorimetric cylinders, then is separately added into 100 μ L
A series of ascorbic acid solution of concentration gradients in step (1) is settled to 5mL with the phosphate buffer solution that pH value is 4；
(3) with the fluorescence intensity of solution in 11 colorimetric cylinders in Fluorescence Spectrometer determination step (2)；
As the result is shown with embodiment 1, the fluorescence intensity of amination carbon quantum dot subtracts with the increase of ascorbic acid concentrations
It is weak, illustrate that the fluorescence of carbon quantum dot can be quenched in ascorbic acid.
Embodiment 3:
A kind of preparation method of amination carbon quantum dot, the specific steps are as follows:
(1) histidine is dissolved in sodium hydroxide solution and ultrasonic treatment 5min is obtained in the case where ultrasonic power is 30kHz
To mixed solution A；Wherein the concentration of sodium hydroxide solution is 8mg/mL, and the solid-to-liquid ratio g:mL of histidine and sodium hydroxide solution is
1:15；
(2) step (1) mixed solution A is placed under the conditions of temperature is 220 DEG C and carries out hydro-thermal reaction 10h, naturally cooled to
Liquor B is obtained by filtration in room temperature；The filter sizes wherein filtered are 0.25 μm；
(3) liquor B of step (2) is subjected to centrifugal treating, takes supernatant；Wherein the revolving speed of centrifugal treating is 12000r/
Min, the time of centrifugal treating are 10min；
(4) supernatant of step (3) is dialysed through dialysis membrane, obtains amination carbon quantum dot solution, being stored in temperature is 2
DEG C refrigerator in；Wherein the molecule interception of dialysis membrane is 600Da, and dialysis membrane dialysis time is 26h；
Using quinine sulfate as standard, the quantum yield of gained amination carbon quantum dot, calculation formula are calculated are as follows:(Ф represents fluorescence quantum yield, and " ST " and " X " respectively represents quinine sulfate and ammonia
Base carbon quantum dot, Grad are the linear fit gradients obtained from the full spectrum of fluorescence intensity and absorbance figure, and η is the refraction of solvent
Rate), it is known that quantum yield of the quinine sulfate in 200~400nm excitation wavelength range is 0.54, calculates gained amination carbon amounts
The quantum yield of son point is 10.2%；
The Electrochemical Detection of Ascorbic Acid
(1) successively use partial size that bright and clean mirror surface is presented for 0.3 and 0.05 μm of polishing powder polishing glass-carbon electrode to surface,
Naturally dry；
(2) chitosan solution that 5 μ L concentration are 5mg/mL, the glass carbon that modification to step (1) has been polished are drawn with liquid-transfering gun
On electrode, naturally dry；
(3) 5 μ L amination carbon quantum dot solution are drawn with liquid-transfering gun, modified on the glass-carbon electrode dried to step (2), from
So dry；
(4) use pH value for 4 phosphate buffer solution prepare a series of concentration gradients (0,10 μm of ol/L, 20 μm of ol/L,
40 μm of ol/L, 60 μm of ol/L, 80 μm of ol/L, 100 μm of ol/L, 200 μm of ol/L, 300 μm of ol/L, 400 μm of ol/L, 500 μm of ol/L,
600 μm of ol/L, 700 μm of ol/L, 800 μm of ol/L, 900 μm of ol/L, 1000 μm of ol/L) ascorbic acid solution；
It (5) is the modified electrode that is dried to electrode, step (3) for work by reference electrode, platinum electrode of calomel electrode
Electrode, various concentration ascorbic acid solution be electrolyte, test DPV curve；
As the result is shown with embodiment 1, current signal changes with the variation of ascorbic acid concentrations, and current signal and anti-
Bad hematic acid concentration correlation；
The fluorescence detection of Ascorbic Acid
(1) use pH value for 4 phosphate buffer solution prepare a series of concentration gradients (0,10 μm of ol/L, 20 μm of ol/L,
30 μm of ol/L, 40 μm of ol/L, 50 μm of ol/L, 60 μm of ol/L, 70 μm of ol/L, 80 μm of ol/L, 90 μm of ol/L, 100 μm of ol/L) it is anti-
Bad hematic acid solution；
(2) it is separately added into 100 μ L amination carbon quantum dot solution in 11 10mL colorimetric cylinders, then is separately added into 100 μ L
A series of ascorbic acid solution of concentration gradients in step (1) is settled to 5mL with the phosphate buffer solution that pH value is 4；
(3) with the fluorescence intensity of solution in 11 colorimetric cylinders in Fluorescence Spectrometer determination step (2)；
As the result is shown with embodiment 1, the fluorescence intensity of amination carbon quantum dot subtracts with the increase of ascorbic acid concentrations
It is weak, illustrate that the fluorescence of carbon quantum dot can be quenched in ascorbic acid.
Embodiment 4:
A kind of preparation method of amination carbon quantum dot, the specific steps are as follows:
(1) histidine is dissolved in sodium hydroxide solution and ultrasonic treatment 8min is obtained in the case where ultrasonic power is 25kHz
To mixed solution A；Wherein the concentration of sodium hydroxide solution is 20mg/mL, the solid-to-liquid ratio g:mL of histidine and sodium hydroxide solution
For 1:10；
(2) step (1) mixed solution A is placed under the conditions of temperature is 200 DEG C and carries out hydro-thermal reaction 12h, naturally cooled to
Liquor B is obtained by filtration in room temperature；The filter sizes wherein filtered are 0.45 μm；
(3) liquor B of step (2) is subjected to centrifugal treating, takes supernatant；Wherein the revolving speed of centrifugal treating is 10000r/
Min, the time of centrifugal treating are 20min；
(4) supernatant of step (3) is dialysed through dialysis membrane, obtains amination carbon quantum dot solution, being stored in temperature is 4
DEG C refrigerator in；Wherein the molecule interception of dialysis membrane is 1000Da, and dialysis membrane dialysis time is 18h；
Using quinine sulfate as standard, the quantum yield of gained amination carbon quantum dot, calculation formula are calculated are as follows:(Ф represents fluorescence quantum yield, and " ST " and " X " respectively represents quinine sulfate and ammonia
Base carbon quantum dot, Grad are the linear fit gradients obtained from the full spectrum of fluorescence intensity and absorbance figure, and η is the refraction of solvent
Rate), it is known that quantum yield of the quinine sulfate in 200~400nm excitation wavelength range is 0.54, calculates gained amination carbon amounts
The quantum yield of son point is 9.3%；
The Electrochemical Detection of Ascorbic Acid
(1) successively use partial size that bright and clean mirror surface is presented for 0.3 and 0.05 μm of polishing powder polishing glass-carbon electrode to surface,
Naturally dry；
(2) chitosan solution that 5 μ L concentration are 5mg/mL, the glass carbon that modification to step (1) has been polished are drawn with liquid-transfering gun
On electrode, naturally dry；
(3) 5 μ L amination carbon quantum dot solution are drawn with liquid-transfering gun, modified on the glass-carbon electrode dried to step (2), from
So dry；
(4) use pH value for 4 phosphate buffer solution prepare a series of concentration gradients (0,10 μm of ol/L, 20 μm of ol/L,
40 μm of ol/L, 60 μm of ol/L, 80 μm of ol/L, 100 μm of ol/L, 200 μm of ol/L, 300 μm of ol/L, 400 μm of ol/L, 500 μm of ol/L,
600 μm of ol/L, 700 μm of ol/L, 800 μm of ol/L, 900 μm of ol/L, 1000 μm of ol/L) ascorbic acid solution；
It (5) is the modified electrode that is dried to electrode, step (3) for work by reference electrode, platinum electrode of calomel electrode
Electrode, various concentration ascorbic acid solution be electrolyte, test DPV curve；
As the result is shown with embodiment 1, current signal changes with the variation of ascorbic acid concentrations, and current signal and anti-
Bad hematic acid concentration correlation；
The fluorescence detection of Ascorbic Acid
(1) use pH value for 4 phosphate buffer solution prepare a series of concentration gradients (0,10 μm of ol/L, 20 μm of ol/L,
30 μm of ol/L, 40 μm of ol/L, 50 μm of ol/L, 60 μm of ol/L, 70 μm of ol/L, 80 μm of ol/L, 90 μm of ol/L, 100 μm of ol/L) it is anti-
Bad hematic acid solution；
(2) it is separately added into 100 μ L amination carbon quantum dot solution in 11 10mL colorimetric cylinders, then is separately added into 100 μ L
A series of ascorbic acid solution of concentration gradients in step (1) is settled to 5mL with the phosphate buffer solution that pH value is 4；
(3) with the fluorescence intensity of solution in 11 colorimetric cylinders in Fluorescence Spectrometer determination step (2)；
As the result is shown with embodiment 1, the fluorescence intensity of amination carbon quantum dot subtracts with the increase of ascorbic acid concentrations
It is weak, illustrate that the fluorescence of carbon quantum dot can be quenched in ascorbic acid.
Embodiment 5:
A kind of preparation method of amination carbon quantum dot, the specific steps are as follows:
(1) histidine is dissolved in sodium hydroxide solution and ultrasonic treatment 10min is obtained in the case where ultrasonic power is 20kHz
To mixed solution A；Wherein the concentration of sodium hydroxide solution is 10mg/mL, the solid-to-liquid ratio g:mL of histidine and sodium hydroxide solution
For 1:20；
(2) step (1) mixed solution A is placed under the conditions of temperature is 200 DEG C and carries out hydro-thermal reaction 15h, naturally cooled to
Liquor B is obtained by filtration in room temperature；The filter sizes wherein filtered are 0.22 μm；
(3) liquor B of step (2) is subjected to centrifugal treating, takes supernatant；Wherein the revolving speed of centrifugal treating is 10000r/
Min, the time of centrifugal treating are 20min；
(4) supernatant of step (3) is dialysed through dialysis membrane, obtains amination carbon quantum dot solution, being stored in temperature is 4
DEG C refrigerator in；Wherein the molecule interception of dialysis membrane is 500Da, and dialysis membrane dialysis time is 36h；
Using quinine sulfate as standard, the quantum yield of gained amination carbon quantum dot, calculation formula are calculated are as follows:(Ф represents fluorescence quantum yield, and " ST " and " X " respectively represents quinine sulfate and ammonia
Base carbon quantum dot, Grad are the linear fit gradients obtained from the full spectrum of fluorescence intensity and absorbance figure, and η is the refraction of solvent
Rate), it is known that quantum yield of the quinine sulfate in 200~400nm excitation wavelength range is 0.54, calculates gained amination carbon amounts
The quantum yield of son point is 12.8%；
The Electrochemical Detection of Ascorbic Acid
(1) successively use partial size that bright and clean mirror surface is presented for 0.3 and 0.05 μm of polishing powder polishing glass-carbon electrode to surface,
Naturally dry；
(2) chitosan solution that 5 μ L concentration are 5mg/mL, the glass carbon that modification to step (1) has been polished are drawn with liquid-transfering gun
On electrode, naturally dry；
(3) 5 μ L amination carbon quantum dot solution are drawn with liquid-transfering gun, modified on the glass-carbon electrode dried to step (2), from
So dry；
(4) use pH value for 4 phosphate buffer solution prepare a series of concentration gradients (0,10 μm of ol/L, 20 μm of ol/L,
40 μm of ol/L, 60 μm of ol/L, 80 μm of ol/L, 100 μm of ol/L, 200 μm of ol/L, 300 μm of ol/L, 400 μm of ol/L, 500 μm of ol/L,
600 μm of ol/L, 700 μm of ol/L, 800 μm of ol/L, 900 μm of ol/L, 1000 μm of ol/L) ascorbic acid solution；
It (5) is the modified electrode that is dried to electrode, step (3) for work by reference electrode, platinum electrode of calomel electrode
Electrode, various concentration ascorbic acid solution be electrolyte, test DPV curve；
As the result is shown with embodiment 1, current signal changes with the variation of ascorbic acid concentrations, and current signal and anti-
Bad hematic acid concentration correlation；
The fluorescence detection of Ascorbic Acid
(1) use pH value for 4 phosphate buffer solution prepare a series of concentration gradients (0,10 μm of ol/L, 20 μm of ol/L,
30 μm of ol/L, 40 μm of ol/L, 50 μm of ol/L, 60 μm of ol/L, 70 μm of ol/L, 80 μm of ol/L, 90 μm of ol/L, 100 μm of ol/L) it is anti-
Bad hematic acid solution；
(2) it is separately added into 100 μ L amination carbon quantum dot solution in 11 10mL colorimetric cylinders, then is separately added into 100 μ L
A series of ascorbic acid solution of concentration gradients in step (1) is settled to 5mL with the phosphate buffer solution that pH value is 4；
(3) with the fluorescence intensity of solution in 11 colorimetric cylinders in Fluorescence Spectrometer determination step (2)；
As the result is shown with embodiment 1, the fluorescence intensity of amination carbon quantum dot subtracts with the increase of ascorbic acid concentrations
It is weak, illustrate that the fluorescence of carbon quantum dot can be quenched in ascorbic acid.
Claims (7)
1. a kind of preparation method of amination carbon quantum dot, which is characterized in that specific step is as follows:
(1) histidine is dissolved in sodium hydroxide solution and is ultrasonically treated 5~15min and obtain mixed solution A；
(2) step (1) mixed solution A is placed under the conditions of temperature is 180~220 DEG C and carries out 10~15h of hydro-thermal reaction, it is naturally cold
But to room temperature, liquor B is obtained by filtration；
(3) liquor B of step (2) is subjected to centrifugal treating, takes supernatant；
(4) supernatant of step (3) is dialysed through dialysis membrane, obtains amination carbon quantum dot solution, being stored in temperature is 0~4
DEG C refrigerator in.
2. the preparation method of amination carbon quantum dot according to claim 1, it is characterised in that: step (1) sodium hydroxide
The concentration of solution is 5~20mg/mL.
3. the preparation method of amination carbon quantum dot according to claim 1 or 2, it is characterised in that: step (1) histidine
Solid-to-liquid ratio g:mL with sodium hydroxide solution is 1:(5~20).
4. the preparation method of amination carbon quantum dot according to claim 1, it is characterised in that: the filter membrane of step (2) filtering
Aperture is 0.05~0.65 μm.
5. the preparation method of amination carbon quantum dot according to claim 1, it is characterised in that: point of step (4) dialysis membrane
Sub- interception is 500~1000Da.
6. according to claim 1 or the preparation method of the 5 amination carbon quantum dots, it is characterised in that: step (4) dialysis membrane is saturating
The analysis time is 18~36h.
7. amination carbon quantum dot prepared by the preparation method of any one of the claim 1~6 amination carbon quantum dot exists
Application in electrochemistry and fluorescence detection simultaneously.
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| CN112080277A (en) * | 2020-09-22 | 2020-12-15 | 江苏普瑞康生物医药科技有限公司 | Nitrogen-doped carbon quantum dot and preparation method and application thereof |
| CN115260723A (en) * | 2022-08-30 | 2022-11-01 | 蚌埠学院 | Preparation method of carbon-aminated quantum dot degradable fluorescent film |
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| CN108483423A (en) * | 2018-04-08 | 2018-09-04 | 太原理工大学 | A kind of fast preparation method of right-handed chirality carbon dots |
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| CN108483423A (en) * | 2018-04-08 | 2018-09-04 | 太原理工大学 | A kind of fast preparation method of right-handed chirality carbon dots |
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| WEIHENG KONG等: "A facile carbon dots based fluorescent probe for ultrasensitive detection of ascorbic acid in biological fluids via non-oxidation reduction strategy", 《TALANTA》 * |
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|---|---|---|---|---|
| CN112080277A (en) * | 2020-09-22 | 2020-12-15 | 江苏普瑞康生物医药科技有限公司 | Nitrogen-doped carbon quantum dot and preparation method and application thereof |
| CN115260723A (en) * | 2022-08-30 | 2022-11-01 | 蚌埠学院 | Preparation method of carbon-aminated quantum dot degradable fluorescent film |
| CN115260723B (en) * | 2022-08-30 | 2024-03-22 | 蚌埠学院 | Preparation method of degradable fluorescent film of aminated carbon quantum dot |
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