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Method for binding and fixing ionic type iridium coordination compound based on covalent bond

An iridium complex, ionic technology, applied in the field of solid-phase electrochemiluminescence electrodes, can solve the problems of easy contamination, poor reproducibility, short service life, etc., and achieve stable existence, good reproducibility, and good response. Effect

Inactive Publication Date: 2014-02-05
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Poor reproducibility and short service life due to its metal iridium complex exposed on the electrode surface and easily contaminated [8]

Method used

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  • Method for binding and fixing ionic type iridium coordination compound based on covalent bond
  • Method for binding and fixing ionic type iridium coordination compound based on covalent bond
  • Method for binding and fixing ionic type iridium coordination compound based on covalent bond

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0019] Example 1. Preparation of sensor: A certain amount of EDC and NHS were dissolved in acetonitrile, and the appropriate concentration ranges were: EDC 5%, NHS 2%. After dissolving, add ionic iridium complex (amount of 2%), stir evenly, and obtain (dpq-OCH 3 ) 2Ir(dcbpy)-NHS ester intermediate. Then, 0.02% of mercaptoethylamine was added into the solution, and stirred to carry out a sufficient reaction to obtain an iridium complex solution with mercapto groups. Take another glassy carbon electrode, after it has been polished, it is cleaned with water and ethanol in sequence, and then electrodeposition is used to fix nano-gold particles for immobilizing ionic metal iridium complexes. The method of electrodeposition is: insert the glassy carbon electrode into the 2 SO 4 and 3mmol / L HAuCl 4 The glassy carbon electrode loaded with gold nanoparticles was prepared by cyclic voltammetry. The scanning potential range is -0.2~1.0V, and the scanning speed range is 10mV / S. Fin...

example 2

[0020] Example 2. Preparation of sensor: A certain amount of EDC and NHS were dissolved in acetonitrile, and the appropriate concentration ranges were: EDC 5%, NHS 2%. After dissolving, add ionic iridium complex (0.1%), stir evenly, and obtain (dpq-OCH 3 ) 2 Ir(dcbpy)-NHS ester intermediate. Then, 0.05% of mercaptoethylamine was added into the solution, and stirred for a sufficient reaction to obtain an iridium complex solution with mercapto groups. Take another glassy carbon electrode, after it has been polished, it is cleaned with water and ethanol in sequence, and then electrodeposition is used to fix nano-gold particles for immobilizing ionic metal iridium complexes. The method of electrodeposition is: the glassy carbon electrode is inserted into a layer containing 1mol / L Na 2 SO 4 and 1mmol / L HAuCl 4 The glassy carbon electrode loaded with gold nanoparticles was prepared by cyclic voltammetry. The scanning potential range is -0.2~1.0V, and the scanning speed range i...

example 3

[0021] Example 3. Preparation of the sensor: A certain amount of EDC and NHS were dissolved in acetonitrile, and the appropriate concentration ranges were: EDC 10%, NHS 5%. After dissolving, add ionic iridium complex (amount of 1%), stir evenly, and obtain (dpq-OCH 3 ) 2 Ir(dcbpy)-NHS ester intermediate. Then, 0.05% of mercaptoethylamine was added into the solution, and stirred for a sufficient reaction to obtain an iridium complex solution with mercapto groups. Take another glassy carbon electrode, after it has been polished, it is cleaned with water and ethanol in sequence, and then electrodeposition is used to fix nano-gold particles for immobilizing ionic metal iridium complexes. The method of electrodeposition is: the glassy carbon electrode is inserted into a layer containing 2mol / L Na 2 SO 4 and 1mmol / L HAuCl 4 The glassy carbon electrode loaded with gold nanoparticles was prepared by cyclic voltammetry. The scanning potential range is -0.2~1.0V, and the scanning ...

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Abstract

The invention relates to a method for binding and fixing an ionic type iridium coordination compound based on a covalent bond, belonging to the field of electrochemiluminescence detection. The method comprises the following steps: firstly, preparing an ionic type iridium coordination compound hexafluorophosphoric acid di(6-methyl-2,4-(4'-methoxy)-diphenyl quinoline (4,4'-dicarboxyl-2,2'-dipyridyl) coordination iridium ((dpq-OCH3)2Ir(dcbpy)+PF6-) with carboxyl by adopting an organic synthesis method, respectively adding 1-ethyl-(3-dimethyl aminopropyl) carbonyl diimine (EDC) and N-hydroxyl succinimide (NHS) to activate the carboxyl, then, adding mercaptoethylamine to stir and react with the carboxyl; and then, preparing nanogold on the surface of a glassy carbon electrode by adopting an electrodeposition method, inserting a prepared electrode into the solution system, and forming an Au-S covalent bond through chemical reaction of the two, and loading the ionic type iridium coordination compound on the electrode. An electrochemiluminescence solid-phase electrode prepared by the method has good response for coreactant dibutyaminoethanol (DBAE).

Description

technical field [0001] The invention immobilizes the ionic iridium complex on the electrode to prepare the solid-phase electrochemiluminescence electrode based on the force of the covalent bond, and belongs to the field of electrochemiluminescence detection. This type of sensor has a good response to inorganic ammonium salts and organic amines, and is widely used in the detection of ammonia or amines in explosives and drugs. Background technique [0002] Electrochemiluminescence (Electrochemiluminescence or ECL) is the reaction of reactants on the electrode surface through high-energy electron transfer reactions to generate excited-state substances to emit light. Electrochemiluminescence is the product of the combination of chemiluminescence and electrochemistry. Therefore, electrochemiluminescence develops the advantages of electrochemistry and uses luminescence to make up for the shortcomings of electrochemistry. It has the advantages of simple device, good reproducibility...

Claims

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Application Information

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IPC IPC(8): G01N21/76G01N27/30C07F15/00
Inventor 宋启军李彤彤韩超峰孙自淑
Owner JIANGNAN UNIV
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