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Fluorescent palladium nano-cluster and synthesis method and application thereof

A synthesis method, palladium nanotechnology, applied in the field of fluorescent palladium nanoclusters and its synthesis, can solve problems such as poor stability, non-uniform nanocluster size, uncontrollable and controllable reaction conditions, etc., and achieve high stability and biocompatibility Good, the effect of shortening the detection time

Active Publication Date: 2020-04-10
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 3. Comprehensive method, microwave method, ultrasonic method to synthesize nanoclusters. Although the reaction rate is high, the uncontrollable and controllable reaction conditions make the synthesized nanoclusters non-uniform in size and poor in stability.

Method used

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  • Fluorescent palladium nano-cluster and synthesis method and application thereof
  • Fluorescent palladium nano-cluster and synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The preparation of embodiment 1 palladium nanocluster:

[0025] The synthesis of palladium nanoclusters, the specific operation method is: under the condition of 60 ℃, add 0.1mL palladium nitrate (100mM) solution to 2.1mL polyethyleneimine (100mM) solution, after stirring at a constant speed for 10min, add 100μL ascorbic acid ( 1.5 M) for 6h. The resulting solution was filtered through a microporous membrane with a pore size of 0.22 μm, centrifuged at 8000 rpm / min for 15 min, and dialyzed with a 1000 Da dialysis bag for 48 h to remove impurities. The resulting solution was stored at 4°C for future use.

[0026] On the F-4500 fluorescence spectrophotometer, set the excitation wavelength from 320nm-400nm, the slit is 10nm, test the emission spectrum under different excitation wavelengths (such as figure 1 A), wherein 1-9 are the fluorescence spectrum graphs under the excitation wavelengths of 320nm, 330nm, 340nm, 350nm, 360nm, 370nm, 380nm, 390nm, and 400nm respectively...

Embodiment 2

[0027] Embodiment 2 selectivity experiment to oxytetracycline

[0028] (1) The ethanol solutions containing ciprofloxacin (Cip), tetracycline (Tc), chloramphenicol (Chl) and erythromycin (Em) were respectively configured as 1×10 -4 M; The aqueous solution of amoxicillin (Amx), kanamycin sulfate (Km) is each 1 × 10 -4 M; Configuration contains the ethanol solution of oxytetracycline (Ot);

[0029] (2) Get the palladium nanocluster solution prepared in Example 1, add dropwise respectively ciprofloxacin, tetracycline, chloramphenicol, erythromycin, amoxicillin, kanamycin sulfate solution, and the ethanol solution of oxytetracycline ,carry out testing;

[0030] (3) On the F-4500 fluorescence spectrophotometer, the excitation wavelength is set to 360nm, and the slit is 10nm, and the fluorescence intensity of palladium nanoclusters at 495nm is tested. Profloxacin, erythromycin, chloramphenicol, amoxicillin, and kanamycin sulfate solution quenched the fluorescence, and only the ad...

Embodiment 3

[0031] Embodiment 3 establishes the standard curve that detects oxytetracycline

[0032] (1) Configure a series of oxytetracycline solutions with different concentrations;

[0033] (2) On F-4500 fluorescence spectrophotometer, setting excitation wavelength 360nm, slit is 10nm, gets the palladium nano-cluster solution test its fluorescence intensity as claimed in claim 1, and its emission wavelength is positioned at 495nm;

[0034] (3) Add different concentrations of oxytetracycline solution in the above-mentioned palladium nanocluster solution to test its fluorescence intensity, the fluorescence intensity of its palladium nanocluster solution decreases with the increase of oxytetracycline solution concentration, by the ratio of its fluorescence intensity I / I 0 Establish a standard curve with different concentrations of oxytetracycline solution (such as figure 2 B) (I is the fluorescence intensity of the palladium nanocluster solution measured by adding oxytetracycline solut...

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Abstract

The invention provides a fluorescent palladium nano-cluster and a synthesis method and application thereof. The palladium nano-cluster is obtained through the following preparation method which comprises the steps that with palladium nitrate as a raw material, polyethylenimine as a stabilizer, and ascorbic acid as a reducing agent, through a chemical reduction method, the fluorescent palladium nano-cluster is prepared at one step. The palladium nano-cluster has excellent fluorescence emission performance in an aqueous solution and good light-resistant bleaching performance and stability, and the solution is irradiated under a 365nm ultraviolet lamp to emit bright blue fluorescence. The invention further provides a method for detecting oxytetracycline by adopting the palladium nano-cluster.The oxytetracycline is detected through a fluorescence analysis method, the fluorescence intensity of the palladium nano-cluster is gradually lowered with increase of the concentration of the oxytetracycline, and the method has good selectivity. The detection method is easy to operate, capable of achieving high detection speed and greatly shortening the detection time, good in selectivity and lowin cost.

Description

technical field [0001] The invention relates to metal nanoclusters, in particular to a fluorescent palladium nanocluster and its synthesis method and application. Background technique [0002] Fluorescent nanoclusters are composed of several to hundreds of atoms, which have many properties that traditional organic fluorescent molecules do not have, including low toxicity, biocompatibility, large Stokes shift, and resistance to photobleaching. In addition to exhibiting many molecular-like optical properties, fluorescent nanoclusters also have important features such as large specific surface area, easy surface modification, and tunable emission wavelength. Fluorescent nanoclusters are widely used in biodetection, biosensors, catalysis, and bioimaging. Therefore, fluorescent nanoclusters have broad application prospects. Currently, fluorescent nanoclusters can be classified into gold (Au), silver (Ag), copper (Cu), palladium (Pd) and platinum (Pt) nanoclusters according to th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/00C09K11/87G01N21/64B82Y40/00
CPCB22F9/24G01N21/643C09K11/87B82Y40/00G01N2021/6432B22F1/07B22F1/054
Inventor 李忠平杜孝艳温广明
Owner SHANXI UNIV
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