CN110157420A - Ascorbic acid carbon nanodot fluorescence probe, preparation method and application - Google Patents
Ascorbic acid carbon nanodot fluorescence probe, preparation method and application Download PDFInfo
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- CN110157420A CN110157420A CN201910308170.9A CN201910308170A CN110157420A CN 110157420 A CN110157420 A CN 110157420A CN 201910308170 A CN201910308170 A CN 201910308170A CN 110157420 A CN110157420 A CN 110157420A
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- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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Abstract
The invention discloses the method and step of ascorbic acid carbon nanodot fluorescence probe, preparation method and application, preparation is as follows: S1: polyethyleneimine is added in the reaction kettle containing ascorbic acid solution, and sealing, then heating is reacted；S2: the solution in the S1 after reaction is cooled to room temperature, and obtains the liquid of brown, and carry out film filtering to it；S3: the filtered solution of film in the S2 is dialysed；S4: the solution after dialysing in the S3 is freeze-dried to get ascorbic acid carbon nanodot fluorescence probe is arrived.The present invention is sensitive to mercury ion response, quick, establishes corresponding linear relationship between fluorescent quenching intensity and ion concentration of mercury, realizes the quantitative detection to mercury ion, and detection is limited to 22nM.In addition to this, which has very high selectivity to mercury ion, and stability is good, can long-term preservation use, and synthesize simple, be conducive to commercialized popularization and application.
Description
Technical field
The present invention relates to technical field of chemical measurement more particularly to ascorbic acid carbon nanodot fluorescence probes, its preparation side
Method and application.
Background technique
The content of heavy metal Hg is usually no more than 1.0 μ g/L in natural water body, and the pollution of the mercury in water body is mainly derived from
Produce the factories and miness of mercury, the industrial wastewater of metal exploitation and smelting, production division's discharge of mercury, mercury especially in chemical production process
Discharge.In sediment, inorganic mercury salt is changed into severe toxicity under the intracorporal methyl cobalt ammonia methionine transfer enzyme effect of microorganism
Methyl mercury and dimethylmercury.Especially organic methyl mercury has very strong lipophilicity, is easy to be absorbed by aquatile, finally
It is enriched with step by step by food chain and human health is caused to seriously threaten.Especially to nerve system of human body, immune system, system genitale
System, kidney and heart etc. have biggish damage, lead to cognitive disorder and dyskinesia.If the famous minamata disease of Japan is exactly edible
Caused by fish containing methyl mercury.So being injured for the mercury ion in prevention and treatment water environment to environment and human health bring, answer
It prevents trouble before it happens, not only needs to control the discharge of pollution mercury from source, it is also necessary to supervise for a long time, in real time to mercury ion
It surveys.
Given this, development can effectively detect especially can fast accurate detection water environment in mercury ion analysis method
It is of crucial importance and have research significance.Currently, the detection method of mercury ion includes Atomic absorption-emission spectrometry, inductance lotus root
Close Plasma Mass Spectrometry, electrochemical method (redox potentiometry), spectrophotometry (such as dithizone colorimetric method).So
And often there is the problems such as instrument and equipment is expensive, testing cost is high, sample pretreatment is complicated in these methods, it is big in practical application
It is restricted, is difficult to be used widely in terms of environmental monitoring and control.Compared with these analysis methods, spectrofluorimetry skill
Art has the advantages that good high sensitivity, selectivity, fast response time, easy to operate, testing cost is low etc..So with fluorescence spectrum
Mercury ion detecting of the chemical sensor for aqueous solution based on signal has good development prospect.However, these are high-quality
Characteristic also depend on new fluorescent material development especially fluorescent nano material progress.Therefore, a kind of superior spy is designed
Property nano material probe in detecting environment in mercury ion have long-range meaning.
Summary of the invention
Technical problems based on background technology, the invention proposes ascorbic acid carbon nanodot fluorescence probes, its system
Preparation Method and application, ascorbic acid carbon nanodot fluorescence probe obtained have very high selectivity to mercury ion, and stability is good,
Can long-term preservation use, and synthesize simple, be conducive to commercialized popularization and application.
The method and step of the preparation of ascorbic acid carbon nanodot fluorescence probe proposed by the present invention is as follows:
S1: polyethyleneimine is added in the reaction kettle containing ascorbic acid solution, and sealing, then heating carries out anti-
It answers；
S2: the solution in the S1 after reaction is cooled to room temperature, and obtains the liquid of brown, and carry out film mistake to it
Filter；
S3: the filtered solution of film in the S2 is dialysed；
S4: the product under dialysis retention in the S3 is freeze-dried to get ascorbic acid carbon nanodot fluorescence is arrived
Probe.
Preferably, the molecular weight of polyethyleneimine is 600 or 10000 in the S1, and the concentration of the ascorbic acid is
1.5-2.5μg/mL。
Preferably, the molar ratio of polyethyleneimine and ascorbic acid is 1:1-40 in the S1.
Preferably, the reaction condition in the S1 are as follows: 180-220 DEG C of heating temperature, reaction time 6-8h.
Preferably, the film in the S2 is filtered into 0.45 μM of syringe filter.
Preferably, the dialysis condition in the S3 are as follows: the Dalton molecular weight of bag filter is 1000 or 10000, when dialysis
Between 8-12h, every 2-3h changes a ultrapure water.
Preferably, the condition of the freeze-drying in the S4 are as follows: vacuum degree 30-50Pa, -20--40 DEG C of temperature, time 40-
60h。
The ascorbic acid carbon nanodot fluorescence probe of preparation method preparation proposed by the present invention is that polyethyleneimine is amine-modified.
The ascorbic acid carbon nanodot fluorescence probe of preparation method preparation proposed by the present invention is amine-modified for polyethyleneimine, and
For the fluorescence of blue.
Application of the ascorbic acid carbon nanodot fluorescence probe proposed by the present invention in mercury ion detecting.
Compared with prior art, beneficial effects of the present invention:
(1) present invention is realized using the carbon nanomaterial using the amine-modified ascorbic acid design synthesizing new of polyethyleneimine
Detection to mercury ion, the range of linearity are 0~20 μM, minimal detectable concentration 22nM；
(2) rate of recovery in actual water sample of the present invention illustrates mercury of this method in detection of complex water sample close to 100%
Ion has very big potentiality.In addition to secondary, the method for the present invention avoids the use of large-scale instrument significantly to a certain extent, only needs
One hand-held ultraviolet lamp can carry out Visual retrieval, and the preprocessing process of very complicated is omitted；
(3) mercury ion detecting test paper of the invention, production is simple, is conducive to commercialized popularization and application.
Detailed description of the invention
Fig. 1 is selective response histogram of the fluorescence probe proposed by the present invention to mercury ion；
Fig. 2 is the fluorescent stability of carbon nanometer point sensor proposed by the present invention；
Fig. 3 is fluorescence response spectrogram of the fluorescence probe proposed by the present invention to mercury ion under various concentration；
Linear relationship chart of the Fig. 4 between fluorescent quenching intensity proposed by the present invention and ion concentration of mercury.
Specific embodiment
Combined with specific embodiments below the present invention is made further to explain.
Embodiment 1
The method and step of the preparation of ascorbic acid carbon nanodot fluorescence probe proposed by the present invention is as follows:
S1: polyethyleneimine is added in the reaction kettle containing ascorbic acid solution, and sealing, then heating carries out anti-
It answers, wherein the molecular weight of polyethyleneimine is 600, and the concentration of ascorbic acid is 1.5 μ g/mL, polyethyleneimine and ascorbic acid
Molar ratio be 1:1, reaction condition be 180 DEG C of heating temperature, reaction time 6h；
S2: the solution in the S1 after reaction is cooled to room temperature, and obtains the liquid of brown, and carry out film mistake to it
Filter, wherein film is filtered into 0.45 μM of syringe filter；
S3: the filtered solution of film in the S2 is dialysed, wherein dialysis condition is the dalton molecule of bag filter
Amount is 1000, and dialysis time 8h, every 2h change a ultrapure water；
S4: the product under dialysis retention in the S3 is freeze-dried to get ascorbic acid carbon nanodot fluorescence is arrived
Probe, the condition of freeze-drying are vacuum degree 30Pa, -20- DEG C of temperature, time 40h.
Embodiment 2
The method and step of the preparation of ascorbic acid carbon nanodot fluorescence probe proposed by the present invention is as follows:
S1: polyethyleneimine is added in the reaction kettle containing ascorbic acid solution, and sealing, then heating carries out anti-
It answers, wherein the molecular weight of polyethyleneimine is 10000, and the concentration of ascorbic acid is 2.5 μ g/mL, polyethyleneimine and Vitamin C
The molar ratio of acid is 1:40, and reaction condition is 220 DEG C of heating temperature, reaction time 8h；
S2: the solution in the S1 after reaction is cooled to room temperature, and obtains the liquid of brown, and carry out film mistake to it
Filter, wherein film is filtered into 0.45 μM of syringe filter；
S3: the filtered solution of film in the S2 is dialysed, wherein dialysis condition is the dalton molecule of bag filter
Amount is 10000, and dialysis time 12h, every 3h change a ultrapure water；
S4: the product under dialysis retention in the S3 is freeze-dried to get ascorbic acid carbon nanodot fluorescence is arrived
Probe, the condition of freeze-drying are vacuum degree 50Pa, -40 DEG C of temperature, time 60h.
Embodiment 3
The method and step of the preparation of ascorbic acid carbon nanodot fluorescence probe proposed by the present invention is as follows:
S1: polyethyleneimine is added in the reaction kettle containing ascorbic acid solution, and sealing, then heating carries out anti-
It answers, wherein the molecular weight of polyethyleneimine is 10000, and the concentration of ascorbic acid is 2 μ g/mL, polyethyleneimine and ascorbic acid
Molar ratio be 1:20, reaction condition be 200 DEG C of heating temperature, reaction time 7h；
S2: the solution in the S1 after reaction is cooled to room temperature, and obtains the liquid of brown, and carry out film mistake to it
Filter, wherein film is filtered into 0.45 μM of syringe filter；
S3: the filtered solution of film in the S2 is dialysed, wherein dialysis condition is the dalton molecule of bag filter
Amount is 1000, and dialysis time 10h, every 2.5h change a ultrapure water；
S4: the product under dialysis retention in the S3 is freeze-dried to get ascorbic acid carbon nanodot fluorescence is arrived
Probe, the condition of freeze-drying are vacuum degree 40Pa, -30 DEG C of temperature, time 50h.
Embodiment 4
Fluorescence detection of the carbon nanodot fluorescence sensor to mercury ion
Its resulting carbon nano dot powder is dispersed in ultrapure water by the present invention by taking embodiment 1 as an example, and 2 μ g/ of concentration is made
The fluorescent optical sensor dispersion liquid of mL sequentially adds the standard solution (0.0,2.5,5.0,7.5,10.0,12.5,17.5 of mercury ion
With 20 μM), with the increase of ion concentration of mercury, fluorescence intensity is gradually decreased, and fluorescence spectrum response process is as shown in Figure 2.It is glimmering
Linear relationship between optical quenching intensity and ion concentration of mercury is F0- F/F=0.0964+0.0404 [Hg (II)], it is linearly related
Coefficients R2=9878, detection is limited to 22nM, such as Fig. 4, is according to, it can be achieved that quantitative detection to mercury ion with this linear relationship.
Embodiment 5
Selective response of the carbon nanodot fluorescence sensor to mercury ion
With reference to Fig. 1, by the carbon nanodot fluorescence probe of same concentrations and sodium ion, potassium ion, calcium ion, magnesium ion, manganese
The interaction such as ion, iron ion, cobalt ions, nickel ion, zinc ion, cadmium ion, silver ion, barium ions lead ion, all cannot
The significant change for causing the fluorescence probe intensity illustrates that these metal ions influence insignificant, the probe to the fluorescence probe
With very high selectivity.Wherein ion concentration of mercury is 20 μM, sodium ion, potassium ion, calcium ion and magnesium ion concentration be mercury
50 times of ion, other heavy metal ion for example manganese ion, iron ion, cobalt ions, nickel ion, zinc ion, cadmium ion, silver ion,
The concentration of barium ions lead ion is 20 times of mercury ion.
Embodiment 6
Application of the carbon nanodot fluorescence sensor in actual water sample
Actual water sample is derived from the tap water in local Lu'an City the Pihe River river water and laboratory.Before spectrum analysis, water sample
Simple pre-treatment need to be passed through, such as stand 2h, with 0.22 μM of pin type membrane filtration, remove suspended impurity and micro- solid in water sample
Grain.Using the mercury ion in standard addition method quantitative detection water sample, specific implementation process is as follows: adding into pretreated water sample
The mercury ion standard solution for adding known quantity, is then added probe, measures its fluorescence intensity, and the standard obtained according to embodiment 4 is bent
Line computation goes out mercury ion content in unknown water sample, the results are shown in Table 1.
The recovery experiment of different ion concentration of mercury in 1 actual water sample of table
As seen from the above table, the rate of recovery of probe in detecting produced by the present invention is suitable for real between 94.4% to 117.2%
The detection of mercury ion in the water sample of border.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of ascorbic acid carbon nanodot fluorescence probe, which is characterized in that method and step is as follows:
S1: polyethyleneimine is added in the reaction kettle containing ascorbic acid solution, and sealing, then heating is reacted；
S2: the solution in the S1 after reaction is cooled to room temperature, and obtains the liquid of brown, and carry out film filtering to it；
S3: the filtered solution of film in the S2 is dialysed；
S4: the product under dialysis retention in the S3 is freeze-dried to get ascorbic acid carbon nanodot fluorescence probe is arrived.
2. the preparation method of ascorbic acid carbon nanodot fluorescence probe according to claim 1, which is characterized in that the S1
The molecular weight of middle polyethyleneimine is 600 or 10000, and the concentration of the ascorbic acid is 1.5-2.5 μ g/mL.
3. the preparation method of ascorbic acid carbon nanodot fluorescence probe according to claim 1, which is characterized in that the S1
The molar ratio of middle polyethyleneimine and ascorbic acid is 1:1-40.
4. the preparation method of ascorbic acid carbon nanodot fluorescence probe according to claim 1, which is characterized in that the S1
In reaction condition are as follows: 180-220 DEG C of heating temperature, reaction time 6-8h.
5. the preparation method of ascorbic acid carbon nanodot fluorescence probe according to claim 1, which is characterized in that the S2
In film be filtered into 0.45 μM of syringe filter.
6. the preparation method of ascorbic acid carbon nanodot fluorescence probe according to claim 1, which is characterized in that the S3
In dialysis condition are as follows: the Dalton molecular weight of bag filter is 1000 or 10000, and dialysis time 8-12h, every 2-3h change primary super
Pure water.
7. the preparation method of ascorbic acid carbon nanodot fluorescence probe according to claim 1, which is characterized in that the S4
In freeze-drying condition are as follows: vacuum degree 30-50Pa, -20--40 DEG C of temperature, time 40-60h.
8. a kind of ascorbic acid carbon nanodot fluorescence probe of preparation method preparation as described in claim 1, which is characterized in that
The fluorescence probe is that polyethyleneimine is amine-modified.
9. a kind of ascorbic acid carbon nanodot fluorescence probe of preparation method preparation as described in claim 1, which is characterized in that
The fluorescence probe is amine-modified for polyethyleneimine, and is the fluorescence of blue.
10. a kind of application of the ascorbic acid carbon nanodot fluorescence probe in mercury ion detecting as described in right wants 8 or 9.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111849475A (en) * | 2020-08-25 | 2020-10-30 | 中南民族大学 | Nitrogen and sulfur co-doped carbon dot and preparation method and application thereof |
| CN111849474A (en) * | 2020-08-03 | 2020-10-30 | 山西大学 | Nitrogen-doped carbon dots based on carnation flowers and preparation method and application thereof |
| CN112063214A (en) * | 2020-09-14 | 2020-12-11 | 山东农业大学 | Adhesive blue fluorescent coating and preparation method and application thereof |
| CN115386376A (en) * | 2022-10-27 | 2022-11-25 | 广东药科大学 | Nano platinum composite material based on carbon quantum dot assembly and preparation method and application thereof |
| CN115594845A (en) * | 2022-11-04 | 2023-01-13 | 皖西学院（Cn） | Method for synthesizing polydopamine fluorescent probe through green path and application of polydopamine fluorescent probe in selective detection of Hg & lt 2+ & gt |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111849474A (en) * | 2020-08-03 | 2020-10-30 | 山西大学 | Nitrogen-doped carbon dots based on carnation flowers and preparation method and application thereof |
| CN111849474B (en) * | 2020-08-03 | 2022-05-31 | 山西大学 | Nitrogen-doped carbon dots based on carnation flowers and preparation method and application thereof |
| CN111849475A (en) * | 2020-08-25 | 2020-10-30 | 中南民族大学 | Nitrogen and sulfur co-doped carbon dot and preparation method and application thereof |
| CN111849475B (en) * | 2020-08-25 | 2022-05-24 | 中南民族大学 | Nitrogen and sulfur co-doped carbon dot and preparation method and application thereof |
| CN112063214A (en) * | 2020-09-14 | 2020-12-11 | 山东农业大学 | Adhesive blue fluorescent coating and preparation method and application thereof |
| CN112063214B (en) * | 2020-09-14 | 2021-05-25 | 山东农业大学 | Adhesive blue fluorescent coating and preparation method and application thereof |
| CN115386376A (en) * | 2022-10-27 | 2022-11-25 | 广东药科大学 | Nano platinum composite material based on carbon quantum dot assembly and preparation method and application thereof |
| CN115386376B (en) * | 2022-10-27 | 2022-12-20 | 广东药科大学 | Nano platinum composite material based on carbon quantum dot assembly and preparation method and application thereof |
| CN115594845A (en) * | 2022-11-04 | 2023-01-13 | 皖西学院（Cn） | Method for synthesizing polydopamine fluorescent probe through green path and application of polydopamine fluorescent probe in selective detection of Hg & lt 2+ & gt |
| CN115594845B (en) * | 2022-11-04 | 2024-01-30 | 皖西学院 | Method for synthesizing polydopamine fluorescent probe through green path and application of polydopamine fluorescent probe in Hg & lt2+ & gt selective detection |
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