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Iodide ion recognition probe and preparation method thereof

An iodide ion and probe technology, applied in the field of analysis and detection, can solve the problems of expensive instruments and equipment, cumbersome procedures, and many steps, and achieve the effects of easy industrial production, simple synthesis method, and strong anti-interference ability.

Active Publication Date: 2019-07-19
HARBIN ENG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chemical analysis generally has many steps, and the error of trace detection results is large, and the detection results are greatly affected by coexisting impurities, such as iron ions, alkaline calcium ions and sulfides
Using the arsenic-cerium catalytic kinetic method to determine the iodide ion content in brine, the reaction reagent is very toxic and does not meet the actual detection requirements
In addition, some scholars use electrochemical methods, as well as atomic spectroscopy and inductively coupled plasma mass spectrometry to determine the content of iodine ions. These methods require expensive instruments and equipment, and have high requirements for sample processing. The procedures are cumbersome and do not meet the requirements for rapid detection.

Method used

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  • Iodide ion recognition probe and preparation method thereof
  • Iodide ion recognition probe and preparation method thereof
  • Iodide ion recognition probe and preparation method thereof

Examples

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preparation example Construction

[0031] A method for preparing the above-mentioned iodide ion-recognizing probe has the following synthetic technical route:

[0032] first step:

[0033]

[0034] The second step:

[0035]

[0036] The specific method is as follows:

[0037] The first step: This method uses (9,9-bis(6-bromohexyl)-2,7-difluorenaldehyde) as a raw material and reacts with 2,5-diaminopyridine under the condition of anhydrous LiCl as a catalyst. The intermediate product II is obtained.

[0038] In some embodiments: the molar ratio of 2,5-diaminopyridine to compound I in the first step reaction is 1:1 to 1:3, and the temperature of the first step reaction needs to reach 100 to 120°C under the protection of nitrogen. The one-step reaction time is 8-24h.

[0039] Step 2: Under the condition of N,N-dimethylacetamide (DMAc) as the solvent, the intermediate product II and trimethylamine (NMe 3 ) Reaction to obtain polymer P.

[0040] In some embodiments: the second step reaction needs to be carried out under seale...

Embodiment 1

[0043] Preparation and characterization of iodide ion recognition probe P:

[0044] Take 0.02667g of 9,9-bis(6-bromohexyl)-2,7-difluorenaldehyde as raw material, and a 3-fold excess of 0.0159g (0.15mmoL) 2,5-diaminopyridine, and measure 25mL DMF( Dewatering) was added to the reaction eggplant bottle, 0.5g (0.0118moL) catalyst anhydrous LiCl was added, and it was placed in an oil bath under the protection of nitrogen and heated to 110°C for 12 hours. After the reaction, the reactant was slowly added dropwise to 500 mL of ice-water mixture to allow it to settle, and then the precipitate was centrifuged, washed with deionized water until the supernatant was clear, and freeze-dried. The intermediate product II obtained as a brown powder was 0.0204 g, and the yield was 48%.

[0045] Separately take 0.02g (32.2μmoL) of the above-mentioned intermediate product II in a 100mL eggplant-shaped bottle, and then measure 15mL DMAc, then add 15mL 30% trimethylamine aqueous solution, seal the dev...

Embodiment 2

[0051] Fluorescence recognition and detection of iodide ion by probe P:

[0052] Such as figure 1 As shown, to the PBS (pH=7) buffer solution system of 10μmol / L probe molecule P, add anion solution (SO 4 2- , ClO 4 - , HCO 3 - , OH - , F - , Cl - , Br - , I - ) Make the concentration reach 100mmol / L, and the fluorescence experiment is measured on the LS55 fluorescence spectrophotometer produced by PE company in the United States. From the figure, we can find that different anions can quench the fluorescence of probe P to different degrees, and iodide ion is the most significant. This phenomenon indicates that the probe molecule P has a unique response to iodide ions.

[0053] Such as figure 2 As shown, the fluorescence quenching efficiency is calculated when the anion concentration is 100mmol / L. It can be seen from the figure that different anions can quench the fluorescence of the probe molecule P to different degrees, but I - The fluorescence quenching effect in the sample is re...

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Abstract

The invention provides an iodide ion recognition probe and a preparation method thereof. The preparation method comprises the following steps: reacting 9,9-bis(6-bromohexyl)-fluorene-2,7-dicarbaldehyde serving as a raw material with 2,5-diaminopyridine under the condition of anhydrous LiCl serving as a catalyst to obtain an intermediate product; and under the condition that N,N-dimethylacetamide is taken as a solvent, reacting the intermediate product with trimethylamine to obtain a pyridine fluorenyl fluorescent conjugated polymer. The synthesis method is simple, industrial production is easy, iodine ions can be rapidly, sensitively, accurately and economically detected, the efficiency is high in an actual application process, and the probe and method are particularly suitable for detection of micro and trace iodine ions. The fluorescence probe disclosed by the invention is high in iodine ion detection selectivity, the lowest detection limit is 4.68*10<-7> mol / L, a good linear quantitative relation is shown in a range of 0-25 [mu]mol / L, and the fluorescence probe is suitable for trace detection.

Description

Technical field [0001] The invention relates to a recognition probe and a preparation method thereof, in particular to an iodide ion recognition probe and a preparation method thereof, belonging to the field of analysis and detection. Background technique [0002] Iodine is one of the important essential trace elements in the human body. Too much or too little iodine intake can induce various thyroid-related diseases. The detection of iodine content in the human body not only has very important clinical significance in medicine, but also timely evaluates the iodine nutritional status of the population in the area, promptly guides the correct adjustment of the iodine intake in the diet, and thereby reduces the iodine deficiency caused by The incidence of disease is of great significance to improving the quality of the entire nation’s population. In addition, my country has abundant brine resources, and the determination of iodine content in brine plays an important role in iodine...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C08G73/06G01N21/64
CPCC09K11/06G01N21/6428C08G73/0627G01N2021/6432C09K2211/1416C09K2211/1466
Inventor 宫琳丹杜松辉范路安张博郑文岐
Owner HARBIN ENG UNIV
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