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Method for detecting content of chlorpyrifos in vegetables based on Cu-ZrMOF multi-mode signals

A signal detection, chlorpyrifos technology, applied in the direction of measuring devices, chemical instruments and methods, biological testing, etc., can solve the problems of inability to distinguish and detect organophosphorus pesticides, poor selectivity, sensitivity and accuracy, and affect sensor sensitivity and stability.

Active Publication Date: 2020-12-25
GUANGXI NORMAL UNIV
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Problems solved by technology

[0003] Among the relevant patents for the detection of chlorpyrifos that have been published so far, CN108918747A is a method for rapid screening and quantitative determination of pesticide residues in tobacco with filter-type solid-phase extraction combined with GC-QTOF / MS, and CN108593824A is a method for the detection of pesticide residues by gas chromatography-mass spectrometry. Treatment and purification method, CN107490647A A method for quantitatively detecting organophosphorus pesticide chlorpyrifos in ambient air. The above-mentioned methods all use large-scale instruments, such as high performance liquid chromatography, gas chromatography and mass spectrometer. Although these methods are sensitive and reliable in detection data, However, the operation process is cumbersome and complicated, requiring expensive and bulky instruments, sample pretreatment and professional operation, making it unable to meet the needs of on-site rapid detection
[0004] In addition, among the existing methods for detecting chlorpyrifos based on electrochemical, fluorescent and colorimetric sensing modes, CN106442676A discloses the preparation and application of a sensor for detecting pesticides based on nano-cerium oxide / mesoporous carbon. Electrode and nanomaterials such as cerium oxide immobilize the enzyme biosensor of acetylcholinesterase, using the principle that organophosphorus pesticides poison acetylcholinesterase, and detecting the change of the current generated by the enzyme-catalyzed substrate to determine the concentration of pesticides. However, many organophosphorus pesticides can Inhibiting the activity of acetylcholinesterase, it is impossible to distinguish and detect various organophosphorus pesticides, and acetylcholinesterase itself is easily inactivated, which will directly affect the sensitivity and stability of the sensor; CN106645129A A new colorimetric sensor based on functionalized gold nanoparticles for detection Chlorpyrifos, this method uses the specific recognition of nucleic acid aptamers and the change of the ultraviolet absorption peak before and after the aggregation of gold nanoparticles to detect the concentration of chlorpyrifos colorimetrically. Requirements for quantitative detection; CN108226105A A rhodamine B-modified gold nanoparticle probe with visual detection of chlorpyrifos and its hydrolyzate and its preparation method, based on the signal response principle of fluorescence resonance energy transfer and rhodamine B and pesticide molecules in gold Competitive adsorption on the surface of nanoparticles constructs a fluorescence-enhanced sensing method for sensitive detection of pesticide residues. However, this method has poor selectivity and the fluorescence lifetime and fluorescence background will affect the sensitivity and accuracy of the detection results.

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  • Method for detecting content of chlorpyrifos in vegetables based on Cu-ZrMOF multi-mode signals
  • Method for detecting content of chlorpyrifos in vegetables based on Cu-ZrMOF multi-mode signals
  • Method for detecting content of chlorpyrifos in vegetables based on Cu-ZrMOF multi-mode signals

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Experimental program
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Embodiment

[0050] A method for detecting chlorpyrifos content in vegetables based on Cu-ZrMOF multi-mode signal, comprising the steps of:

[0051] (1) Synthesis of Cu-ZrMOF nanozyme materials with certain morphology characteristics;

[0052] Disperse 80 mg of 2,2'-bipyridine-5,5'-dicarboxylic acid in 6 mL of dimethylformamide (DMF), and sonicate;

[0053] 26.12 mg of ZrCl 4 Dissolve in 12 mL DMF, sonicate;

[0054] Then the two solutions were mixed in the reactor, 1.5 mL of acetic acid was added and sonicated, then the solution was stirred and heated at 120 °C for 16 h, a white solid was obtained by centrifugation, and washed three times with ethanol to obtain ZrMOF;

[0055] In a round-bottomed flask, 30 mg of the obtained ZrMOF was dissolved in 5 mL of THF, and after sonication, 10 mg of CuCl was added to the solution 2 • 2H 2 O, sonicated, then stirred for 2 h;

[0056] Finally, the green solid Cu-ZrMOF was collected by centrifugation and washed three times with ethanol, redisper...

experiment example

[0071] Experimental example: detection of vegetable samples: Weigh 5.0 g of lettuce and 5.0 g of lettuce and grind them into 5 mL centrifuge tubes, add 5 mL of PB (10 mM, pH 7.4) solution, then centrifuge and take out the supernatant . The supernatant of each sample was spiked with chlorpyrifos standard solution to prepare three or four spiked samples with low, medium and high concentrations. Next, use electrochemical, fluorescence and colorimetric methods to detect the signal value produced by chlorpyrifos in lettuce and lettuce samples, and substitute it into the working curve to obtain the content of chlorpyrifos in vegetable samples and the recovery rate of the standard, as shown in Table 1, Table 2 and Table 1. Three shown:

[0072] Table 1 Experimental results of detection of chlorpyrifos in spiked vegetable samples by electrochemical method

[0073] .

[0074] Table 2 Experimental results of detection of chlorpyrifos in spiked vegetable samples by fluorescence meth...

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Abstract

The invention discloses a method for detecting the content of chlorpyrifos in vegetables based on Cu-ZrMOF multi-mode signals. The method comprises the following steps of: firstly, preparing a multi-mode sensing probe of Cu-ZrMOF and a magnetic control immune probe, and when chlorpyrifos exists, combining the magnetic control immune probe and the Cu-ZrMOF multi-mode sensing probe with chlorpyrifosto form a sandwich structure similar to a sandwich; establishing a novel chlorpyrifos multi-mode sensing platform which is rapid, sensitive and high in selectivity and reliability by utilizing the synergistic catalytic performance of Cu-ZrMOF nano-enzyme and G-quadruplex DNAzyme concatemer and an oxidation product 2, 3-diaminophenazine which is generated by two mimic enzyme catalytic substrates o-phenylenediamine and has electrical activity, fluorescence emission performance and color development capability; and rapidly and semi-quantitatively screening chlorpyrifos in a large number of samples on site by combining fluorescence visual sensing analysis. The method is expected to be applied to on-site rapid detection and large-scale screening of low-concentration chlorpyrifos residues in samples such as vegetables, fruits, soil and drinking water.

Description

technical field [0001] The invention relates to a method for detecting the content of organophosphorus pesticide chlorpyrifos, in particular to a method for detecting the content of chlorpyrifos in vegetables based on Cu-ZrMOF multi-mode signals. Background technique [0002] Chlorpyrifos (O,O-diethyl-O-(3,5,6-trichloro-2-pyridyl)thiophosphoric acid) is an organophosphorus pesticide that first entered the market in 1965 and is widely used worldwide , it has the effect of sterilization, insecticide and weed control. Long-term use of such pesticides will increase the harmful substances in the environment and food, deteriorate the environment, destroy the ecological balance, and threaten the safety of human beings. It inhibits the activity of acetylcholinesterase in the human body, thereby affecting the central and peripheral cholinergic nervous system. Direct contact or ingestion may cause acute poisoning or even death. In addition, chronic poisoning caused by the accumulati...

Claims

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Application Information

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IPC IPC(8): G01N27/26G01N21/64G01N21/78G01N33/53G01N33/543B01J31/00B01J31/16B01J31/22
CPCG01N27/26G01N21/6428G01N21/78G01N33/5308G01N33/54326B01J31/003B01J31/1691B01J31/2239G01N2021/6439G01N2430/10G01N2430/20B01J2531/48B01J2531/16
Inventor 侯丽张宣晗范敏蒋高艳林天然赵书林
Owner GUANGXI NORMAL UNIV