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Nitrogen-sulfur co-doped carbon quantum dot fluorescent probe for cysteine detection and preparation and application thereof

A technology of nitrogen-sulfur co-doping and fluorescent probes, applied in nanotechnology, measurement devices, fluorescence/phosphorescence, etc. for materials and surface science, can solve environmental hazards and other problems, achieve reduced interference and good reproducibility , the effect of strong signal response

Active Publication Date: 2020-04-10
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, to date, few researchers have reported the use of carbon quantum dots (N,S-CQDs) as optical probes for the detection of cysteine
[0005] Chinese patent CN110066655A discloses a silver-doped carbon quantum dot and its preparation method and application. The preparation method includes: mixing citric acid, silver nitrate and distilled water, undergoing hydrothermal reaction, and centrifuging to collect the product to obtain silver-doped carbon quantum dots. Quantum dots can realize real-time monitoring of cysteine, but the silver-doped carbon quantum dots prepared by this patent introduce noble metal ions, which have a certain harmful effect on the environment when used

Method used

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  • Nitrogen-sulfur co-doped carbon quantum dot fluorescent probe for cysteine detection and preparation and application thereof
  • Nitrogen-sulfur co-doped carbon quantum dot fluorescent probe for cysteine detection and preparation and application thereof
  • Nitrogen-sulfur co-doped carbon quantum dot fluorescent probe for cysteine detection and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Preparation of water-soluble N,S-CQDs.

[0063] Such as figure 1 As indicated, 1.16mmol of 5,5'-dithiobis(2-nitrobenzoic acid) and 7.2mL of ethylenediamine were added to 40mL of deionized water, ultrasonicated for 10min, and then placed in a 100mL liner lined with polytetrafluoroethylene In an ethylene stainless steel autoclave (YZPR-100mL), heating was continued at 200°C for 12h, and then naturally cooled to room temperature to obtain a dark brown solution.

[0064] Use a 0.22 μm filter to remove larger particles in the dark brown solution, and then use a rotary evaporator (RE-52C) to concentrate the solution to 0.05 times the original volume.

[0065] The concentrated solution was purified by silica gel column chromatography, wherein deionized water was used as the eluent, and the green fluorescent solution was collected under the irradiation of a hand-held ultraviolet lamp (365 nm). Finally, the collected solution was heated at 110 °C for 8 h. The N,S-CQDs solid m...

Embodiment 2

[0070] Preparation of Pd 2+ / N,S-CQDs probe system.

[0071] Weigh 10 mg of the N,S-CQDs solid material prepared in Example 1, dissolve it in 100 mL of PBS buffer (pH 7.4, 10 mM), and sonicate for 10 min to obtain a N,S-CQDs solution with a concentration of 0.10 mg / mL.

[0072] Under the irradiation of UV light (365nm), the N,S-CQDs solution emits green fluorescence. The N,S-CQDs solution was detected using a fluorescence spectrophotometer.

[0073] Such as figure 1 As shown, the PdCl 2 PBS solution (50 μL 150 μM) was mixed with N,S-CQDs (20 μL 0.10 mg / mL) solution to prepare Pd 2+ / N,S-CQDs solution. Detected Pd 2+ / N, S-CQDs solution has no fluorescence under UV light irradiation.

[0074] For the same concentration of PdCl 2 solution, N,S-CQDs solution and Pd 2+ / N,S-CQDs were characterized by ultraviolet absorption spectroscopy, and the characterization results are as follows:

[0075] Such as image 3 As shown, it can be seen that PdCl 2 Overlapping with the ...

Embodiment 3

[0077](1) Add 20 μL of 0.1 mg / mL N,S-CQDs solution obtained in Example 2 into a 5 mL centrifuge tube, then dilute to 4 mL with PBS buffer (pH 7.4, 10 mM), stir rapidly for 10 seconds, and transfer to 4 mL In the cuvette, the fluorescent intensity is detected and recorded by a fluorometer, which is recorded as F 0 ;

[0078] (2) Take 13 5mL centrifuge tubes, add 20μL 0.1mg / mL N,S-CQDs solution respectively, and then add 0, 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60 μL of PdCl 2 Solution (150μM), then add PBS buffer solution to dilute to 4mL respectively, after stirring rapidly for 10s, measure and record the fluorescence intensity, the test results are as follows: Figure 5 As shown, it can be seen that when Pd 2+ When the solution concentration was in the range of 0-150 μM, the fluorescence intensity of N,S-CQDs increased with the increase of Pd 2+ decrease with increasing concentration;

[0079] (3) Pd 2+ The concentration was linearly fitted with the fluorescence in...

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Abstract

The invention relates to a nitrogen-sulfur co-doped carbon quantum dot fluorescent probe for cysteine detection and preparation and application thereof. The preparation method comprises the followingsteps of: (1) uniformly mixing ethylenediamine, deionized water and DTNB at room temperature to obtain a mixed solution, 2) setting the temperature of the mixed solution in a high-pressure kettle to be 160-220 DEG C, and performing carbonization treatment to obtain a carbonization treatment solution, 3) filtering, concentrating, purifying by silica gel column chromatography and drying the carbonization treatment solution in sequence to obtain N, S-CQDs, 4) preparing N, S-CQDs into an N, S-CQDs solution, and 5) uniformly mixing the N, S-CQDs solution with a palladium source to obtain Pd<2+> / N,S-CQDs. The Pd<2+> / N, S-CQDs are used for detecting cysteine in a water sample. Compared with the prior art, the fluorescent probe has the advantages of being simple in preparation method, high in sensitivity, good in reproducibility and the like, meanwhile, the fluorescent probe shows high selectivity on cysteine, interference of other metal ions or amino acid substances on detection can be effectively reduced, and the detection result has high reliability.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation and application, and relates to a nitrogen-sulfur co-doped carbon quantum dot fluorescent probe for cysteine ​​detection and its preparation and application, in particular to a Pd 2+ Nitrogen and sulfur co-doped carbon quantum dot fluorescence probe mediated by nitrogen and sulfur, its preparation method and application in the field of cysteine ​​detection. Background technique [0002] Biothiols such as cysteine ​​(Cys), L-cysteine ​​(L-cys), homocysteine ​​(Hcy) and reduced glutathione (GSH) play an important role in human physiological activities. important role. For example, cysteine ​​is an essential amino acid and a sugar-producing amino acid required by the human body. It can be converted from methionine in the body and can be converted into cystine. At the same time, cysteine ​​weakens the structure of the protein by changing the disulfide bonds between protein molecules...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/65B82Y30/00G01N21/64
CPCC09K11/65B82Y30/00G01N21/6428
Inventor 李明中梅杰方振徐虎王宇红
Owner SHANGHAI INST OF TECH
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