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Fluorescent probe capable of identifying iodide ions as well as preparation method and identification method thereof

A technology of fluorescent probe and identification method, which is applied in the field of fluorescent probe for identifying iodide ion and its preparation, can solve the problems of time-consuming, expensive instruments, complicated sample preparation process, etc., and achieves direct analysis, simple operation, and reliable test results. visual effect

Active Publication Date: 2018-07-13
GUIZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, commonly used iodide ion analysis methods include capillary electrophoresis, chromatography, electrochemical methods, and atomic spectroscopy, etc., but these methods are relatively high in cost, time-consuming, complicated in sample preparation, and require expensive instruments, which limit these methods. Application of detection method in practice

Method used

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  • Fluorescent probe capable of identifying iodide ions as well as preparation method and identification method thereof
  • Fluorescent probe capable of identifying iodide ions as well as preparation method and identification method thereof
  • Fluorescent probe capable of identifying iodide ions as well as preparation method and identification method thereof

Examples

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Effect test

Embodiment 1

[0048] Embodiment 1: a kind of preparation method of the fluorescent probe of recognition iodide ion, the steps are as follows:

[0049] 1) Dissolve 2g of 4-bromobenzaldehyde in every 30ml of ethanol to obtain product A;

[0050] 2) Dissolve 2.42g of 2-acetylpyridine, 1.7g of potassium hydroxide and 29ml of ammonia water in every 40ml of ethanol to obtain product B;

[0051] 3) Mix product A and product B at 0°C at a mass ratio of 1:2, stir for 1 hour, reflux for 1 day, and stir at room temperature for 1 hour, filter the precipitate, and recrystallize with ethanol to obtain product C;

[0052] 4) Mix 150mg of 4-pyridineethylene, 30mg of palladium acetate, 102mg of triphenylphosphine and 10ml of triethylamine into each 500mg of product C, and seal the mixture in N 2 In a high-pressure reaction flask under atmosphere, react at 120°C for 70 h, wash the organic phase with distilled water for 3 times, and then wash the organic phase with saturated brine for 3 times, dissolve in ch...

Embodiment 2

[0056] Embodiment 2: a kind of preparation method of the fluorescent probe of recognition iodide ion, the steps are as follows:

[0057] 1) Dissolve 2g of 4-bromobenzaldehyde in every 30ml of ethanol to obtain product A;

[0058] 2) Dissolve 2.42g of 2-acetylpyridine, 1.7g of potassium hydroxide and 29ml of ammonia water in every 40ml of ethanol to obtain product B;

[0059] 3) Mix product A and product B at -5°C at a mass ratio of 1:2, stir for 0.5 h, reflux for 0.5 days, and stir at room temperature for 0.5 h, filter the precipitate, and recrystallize with ethanol to obtain product C;

[0060] 4) Mix 150mg of 4-pyridineethylene, 30mg of palladium acetate, 102mg of triphenylphosphine and 10ml of triethylamine into each 500mg of product C, and seal the mixture in N 2 In a high-pressure reaction flask under atmosphere, react at 110°C for 75h, wash the organic phase with distilled water for 3 times, and then wash the organic phase with saturated brine for 3 times, dissolve in c...

Embodiment 3

[0064] Embodiment 3: a kind of preparation method of the fluorescent probe of recognition iodide ion, the steps are as follows:

[0065] 1) Dissolve 2g of 4-bromobenzaldehyde in every 30ml of ethanol to obtain product A;

[0066] 2) Dissolve 2.42g of 2-acetylpyridine, 1.7g of potassium hydroxide and 29ml of ammonia water in every 40ml of ethanol to obtain product B;

[0067] 3) Mix product A and product B at 5°C at a mass ratio of 1:2, stir for 1.5 hours, reflux for 1.5 days, and stir at room temperature for 1.5 hours, filter the precipitate, and recrystallize with ethanol to obtain product C;

[0068] 4) Mix 150mg of 4-pyridineethylene, 30mg of palladium acetate, 102mg of triphenylphosphine and 10ml of triethylamine into each 500mg of product C, and seal the mixture in N 2 In a high-pressure reaction flask under atmosphere, react at 130°C for 65h, wash the organic phase with distilled water for 3 times, and then wash the organic phase with saturated saline for 3 times, disso...

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Abstract

The invention discloses a fluorescent probe capable of identifying iodide ions and a preparation method and an identification method thereof. The preparation method comprises the following steps of (1) dissolving 4-bromobenzaldehyde into ethyl alcohol, so as to obtain a product A; (2) dissolving 2-acetylpyridine, potassium hydroxide and ammonium hydroxide into ethyl alcohol, so as to obtain a product B; (3) enabling the product A and the product B to react, filtering precipitate, and re-crystallizing, so as to obtain a product C; (4) adding the product C, 4-pyridine vinyl, palladium acetate and triphenylphosphine into triethylamine to mix, dissolving the product into chloroform, spin-drying, and re-crystallizing, so as to obtain a product D; (5) suspending 1,8-naphthalimide into a mixtureof N,N-dimethylformamide and DMSO (dimethylsulfoxide), adding sodium methoxide, stirring, standing, adding 1,4-dibromobutane, filtering precipitate, and re-crystallizing, so as to obtain a product E;(6) adding the product D into N,N-dimethylformamide, adding into the product E, adding diethyl ether until the precipitate is separated out, sucking and filtering, and drying, so as to obtain the fluorescent probe. The fluorescent probe has the characteristics that the identification cost is low, the operation is simple and quick, the sensitivity is high, and the selectivity is good.

Description

technical field [0001] The invention relates to a fluorescent probe and its preparation method and recognition method, in particular to a fluorescent probe for recognizing iodide ions and its preparation method and recognition method. Background technique [0002] The identification and detection of anions plays an important role in the fields of biosensing, chemical analysis, and environmental detection. Among many anions, iodide ion has received extensive attention because of its important biomedical significance. Iodine is one of the essential trace elements for the human body, which plays a vital role in the normal growth, neurodevelopment and thyroid function of the human body. However, abnormal iodine ion concentration levels are usually related to diseases. Iodine deficiency or iodine excess can lead to diseases such as goiter, hypothyroidism and hyperthyroidism, which affect people's health. Therefore, the detection of iodine ions is very important. Significance. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/14C09K11/06G01N21/64
CPCC07D401/14C09K11/06C09K2211/1007C09K2211/1029G01N21/643G01N2021/6439
Inventor 倪新龙殷婷周桂林张晓东李孟轩
Owner GUIZHOU UNIV
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