2-[2-hydroxy-5-(4-nitroazobenzene)styryl]-8-hydroxyquinoline colorimetric reagent, preparation and application

A kind of nitroazobenzene, styryl technology, applied in the field of colorimetric reagent and preparation

Active Publication Date: 2016-12-07
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There have been many reports on anion detection probe reagents, but the same reagent can selectively detect F at near-infrared wavelengths. - 、AcO - , and can also be applied to pH, H 2 No colorimetric reagent for visual detection of O has been reported

Method used

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  • 2-[2-hydroxy-5-(4-nitroazobenzene)styryl]-8-hydroxyquinoline colorimetric reagent, preparation and application
  • 2-[2-hydroxy-5-(4-nitroazobenzene)styryl]-8-hydroxyquinoline colorimetric reagent, preparation and application
  • 2-[2-hydroxy-5-(4-nitroazobenzene)styryl]-8-hydroxyquinoline colorimetric reagent, preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] The chemical structural formula of 2-[2-hydroxy-5-(4-nitroazobenzene) styryl]-8-hydroxyquinoline is:

[0088]

[0089] Its preparation method is:

[0090] a, intermediate: the synthesis of 2-hydroxyl-5-(4-nitroazobenzene) benzaldehyde:

[0091] In a 100ml three-necked flask, add p-nitroaniline (1.38g, 10mmol), 4ml of concentrated hydrochloric acid and 5ml of water, after it dissolves, cool to 0-5°C in an ice-salt bath, slowly drop 5ml of sodium nitrite aqueous solution into Among them, after the addition, the reaction was continued for 2 hours under ice bath, and the pH was adjusted to 7 with sodium hydroxide solution, and then 20 ml of an aqueous solution containing salicylaldehyde (1.22 g, 10 mmol) was added to it, and the reaction was continued for 4 hours, and a red precipitate appeared after the reaction Precipitate, filter, vacuum dry overnight, and recrystallize from tetrahydrofuran to obtain 2-hydroxy-5-(4-nitroazobenzene)benzaldehyde. Yield 53.5%.

[0092...

Embodiment 2

[0095] The preparation method of various reagents in the analytical method of the present invention:

[0096] (1) Preparation of colorimetric reagent dimethyl sulfoxide stock solution: Weigh 20.6 mg of colorimetric reagent (prepared according to Example 1), dissolve it with dimethyl sulfoxide and prepare a colorimetric reagent 2 with a concentration of 1 mM Methyl sulfoxide stock solution 50mL;

[0097] Preparation of colorimetric reagent acetonitrile stock solution: Weigh 20.6 mg of colorimetric reagent (prepared according to Example 1), dissolve it with acetonitrile and prepare 50 mL of colorimetric reagent acetonitrile stock solution with a concentration of 1 mM;

[0098] (2)F - Preparation of stock solution: Weigh 0.3155 g of tetrabutylammonium fluoride, dissolve it in acetonitrile and prepare 50 mL of tetrabutylammonium fluoride acetonitrile stock solution with a concentration of 20 mM.

[0099] (3) AcO - Preparation of stock solution: Weigh 0.3015 g of tetrabutylammon...

Embodiment 3

[0107] (1) Detection of F by UV-Vis absorption spectrometry -

[0108] Add colorimetric reagent acetonitrile stock solution (1mM, 0.1mL) into a 10mL volumetric flask, dilute to the mark with acetonitrile, shake well to obtain a colorimetric reagent solution, take about 3mL of the colorimetric reagent solution in a 1cm cuvette for UV - Determination of visible absorption spectroscopy;

[0109] Add the colorimetric reagent acetonitrile stock solution (1mM, 0.1mL) to a series of 10mL volumetric flasks, and then add the anion F - , AcO - , Cl - , Br - , I - , HSO 4 - , NO 3 - , ClO 4 - , H 2 PO 4 - , PF 6 - The stock solution (20mM, 0.1mL) was diluted to the mark with acetonitrile, shaken well, and about 3mL of the solution was taken in a 1cm cuvette for UV-visible absorption spectrum measurement.

[0110] Add the colorimetric reagent acetonitrile stock solution (1mM, 0.1mL) to a series of 10mL volumetric flasks, and then add the anion F - , AcO - The stock solu...

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Abstract

The invention discloses a 2-[2-hydroxy-5-(4-nitroazobenzene)styryl]-8-hydroxyquinoline colorimetric reagent, as well as a preparation method and application thereof. The colorimetric reagent which can be applied to analytic chemistry for detecting F<->, AcO<->, pH and H2O is prepared from a quinoline derivative and a nitroazobenzene derivative which serve as main raw materials. The colorimetric reagent selectively detects F<-> and AcO<-> by controlling different solvents through a ratio absorption method; meanwhile, the colorimetric reagent can be easily and quickly applied to visual detection of F<->, AcO<->, pH and H2O. The preparation cost is low, the detection sensitivity is high, the selectivity is high, the operating conditions are easy to control, and the application prospect is good.

Description

technical field [0001] The present invention relates to a kind of colorimetric reagent and its preparation method and application, especially a kind of 2-[2-hydroxy-5-(4-nitroazobenzene) styryl]-8-hydroxyquinoline colorimetric reagent and Its preparation method and application. Background technique [0002] Colorimetric reagents can detect specific ions with high sensitivity and high selectivity, and have the characteristics of low detection cost, fast speed, simple equipment, simple and intuitive method, etc., and are widely used in the field of analysis and detection. Colorimetric reagents can not only visually detect and qualitatively analyze, but also use the spectral properties of ratio absorption to form isoabsorbing points during detection, and at the same time, there are changes in the ratio of absorption peaks at different wavelengths for measurement, which has higher detection sensitivity and Accuracy. Using the ratio of absorbance, that is, the ratio absorption ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/26G01N21/31G01N21/78
CPCC07D215/26G01N21/314G01N21/78G01N2021/3155
Inventor 牟兰张红曾晞李钊阮琴
Owner GUIZHOU UNIV
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