2-(2'-hydroxyl styryl) naphthyridine probe reagent and preparation and application thereof

A technology of hydroxystyrene and methylnaphthyridine, used in chemical instruments and methods, analysis by chemical reaction of materials, material analysis by observing the effect on chemical indicators, etc.

Inactive Publication Date: 2016-10-26
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There have been many reports on the research of life and environment-related ions by fluorescent probe method, but most of them are single-probe single-target tests, that is, one probe can only detect one kind of ion, and there are few reports that can realize single-probe multi-target detection

Method used

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  • 2-(2'-hydroxyl styryl) naphthyridine probe reagent and preparation and application thereof
  • 2-(2'-hydroxyl styryl) naphthyridine probe reagent and preparation and application thereof
  • 2-(2'-hydroxyl styryl) naphthyridine probe reagent and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0110] 2-(2'-hydroxystyryl) naphthyridine probe reagent synthesis, specifically comprises the following steps

[0111] a. Synthesis of intermediate 2-methylnaphthyridine:

[0112] Under the condition of ice bath, add concentrated H 2 SO 4 41g (22mL), under stirring, add 17.5g (78mmol) of sodium m-nitrobenzenesulfonate, 2.4g (39mmol) of boric acid, FeSO 4 ·7H 2 O 1.4g (5mmol), glycerol 12.5mL, 2-amino-6-picoline 4.3g (40mmol), mix well, then add 22.5mL of warm water at 50°C, reflux at 135°C for 2-3h, cool After that, adjust to alkaline with 50% NaOH solution, filter with suction, extract the aqueous solution with chloroform three times, and use anhydrous MgSO as the organic layer 4 Drying, rotary evaporation to remove the solvent to obtain a crude product, recrystallization of the crude product with cyclohexane to obtain 2-methylnaphthyridine, namely the probe reagent; the concentration of the concentrated sulfuric acid is 95-98%;

[0113] b. Synthesis of 2-(2'-hydroxystyr...

Embodiment 2

[0116] The preparation method of various reagents in the analytical method of the present invention:

[0117] (1) Preparation of probe stock solution: Weigh 25 mg of the probe reagent prepared in Example 1, dissolve N,N-dimethylformamide and prepare N,N-dimethylformamide with a concentration of 0.1 mM Probe stock solution 10mL;

[0118] Weigh 25 mg of the probe reagent prepared in Example 1, dissolve 1,4-dioxane and prepare 10 mL of 1,4-dioxane probe stock solution with a concentration of 0.1 mM.

[0119] Weigh 25 mg of the probe reagent prepared in Example 1, dissolve in acetonitrile and prepare 10 mL of acetonitrile probe stock solution with a concentration of 0.1 mM.

[0120] (2)Hg 2+ Preparation of stock solution: Weigh 90.4 mg of mercury perchlorate tetrahydrate, dissolve it in water and prepare 10 mL of a solution with a concentration of 20 mM.

[0121] (3)Ag + Preparation of stock solution: Weigh 41.5 mg of silver perchlorate monohydrate, dissolve it in water and pr...

Embodiment 3

[0128] Embodiment 3: fluorescence spectrometry is to Hg 2+ 、Ag + , F - detection

[0129] 1. Detection of Hg 2+ :

[0130] Set the fluorescence excitation wavelength to 375nm, add N,N-dimethylformamide probe stock solution (0.1mM, 1mL) into a 10mL volumetric flask, and use N,N-dimethylformamide / H 2 Dilute O to the mark to make N,N-dimethylformamide / H 2 O is 19 / 1 (v / v), shake well to make a probe solution, take 3mL of the solution in a 1cm cuvette for fluorescence spectrum measurement. After adding N,N-dimethylformamide probe stock solution (0.1mM, 1mL) to a series of 10mL volumetric flasks, add metal ion Hg 2+ , Ag + , Li + , Na + , K + , Mg 2+ , Ca 2+ , Ba 2+ ,Sr 2+ , Zn 2+ , Al 3+ ,Co 2+ , Ni 2+ , Cu 2+ , Zn 2+ , Pb 2+ , Cd 2+ , La 3+ Stock solution (20mM, 0.1mL);

[0131] In N,N-dimethylformamide / H 2 In O(v / v, 19 / 1) solution, the probe solution with a concentration of 10μM emits a strong blue fluorescence at 475nm under excitation at a wavelength of...

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Abstract

The invention discloses a 2-(2'-hydroxyl styryl) naphthyridine probe reagent and preparation and application thereof. The probe reagent is mainly prepared by concentrated sulfuric acid, sodium 3-nitrobenzene sulfonate, boric acid, FeSO4.7H2O, 2-amino-6-picoline, salicylide, glycerol and acetic anhydride. The 2-(2'-hydroxyl styryl) naphthyridine probe reagent has the advantages that the probe reagent can selectively detect various target ions, single-probe, multi-target and multi-mode identification and detection are achieved, and the probe reagent can be used for detecting Hg<2+>, Ag<+> and F<-> ions; a probe is simple in structure, low in preparation cost, diversified in detection and identification manners, high in detection sensitivity, good in selectivity, excellent in performance, easy in operation condition control and promising in application prospect.

Description

technical field [0001] The invention relates to a probe reagent and its preparation method and application, in particular to a 2-(2'-hydroxystyryl)naphthyridine probe reagent and its preparation method and application. Background technique [0002] Among the methods for detecting ions, atomic emission, atomic fluorescence and ion chromatography methods require large-scale instruments and equipment, and the detection cost is high and time-consuming. At the same time, it is difficult to realize the simultaneous detection of metal ions and acid anions. However, the fluorescent probe method is different. Through appropriate condition control, the simultaneous and separate detection of multiple ions can be quickly realized. Usually, the recognition detection of the fluorescence spectrum is accompanied by the simultaneous detection of the absorption spectrum, that is, dual mode recognition detection. The structural design of the probe molecule and the realization of the synthesis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04C09K11/06G01N21/64G01N21/31G01N21/78
CPCC07D471/04C09K11/06C09K2211/1029G01N21/314G01N21/64G01N21/6428G01N21/643G01N21/6447G01N21/78G01N2021/3155G01N2021/6417G01N2021/6432G01N2021/6443
Inventor 曾晞阮琴牟兰李钊张红
Owner GUIZHOU UNIV
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