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A kind of 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, complicated procedures, and many steps, and achieve the effects of strong anti-interference ability, high detection selectivity and simple synthesis method.

Active Publication Date: 2022-01-14
HARBIN ENG UNIV
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  • Abstract
  • Description
  • Claims
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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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  • A kind of iodide ion recognition probe and preparation method thereof
  • A kind of iodide ion recognition probe and preparation method thereof
  • A kind of iodide ion recognition probe and preparation method thereof

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preparation example Construction

[0031] A kind of preparation method of the probe of above-mentioned recognition iodide ion, its synthesis technical route is as follows:

[0032] first step:

[0033]

[0034] Step two:

[0035]

[0036] The specific method is as follows:

[0037] The first step: the 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 1:1~1:3, the temperature of the first step reaction needs to reach 100~120°C under nitrogen protection, the second step The one-step reaction time is 8 to 24 hours.

[0039] The second step: under the condition of N,N-dimethylacetamide (DMAc) as solvent, intermediate product II and trimethylamine (NMe 3 ) reaction to obtain polymer P.

[0040] In some embodiments: the second step reaction...

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 0.0159g (0.15mmoL) 2,5-diaminopyridine in excess of 3 times, measure 25mL of DMF ( Remove water) into the reaction eggplant bottle, add 0.5g (0.0118moL) catalyst anhydrous LiCl, place in an oil bath under the protection of nitrogen and heat to 110 ° C for 12 hours. After the reaction was completed, the reactant was slowly added dropwise to 500 mL of ice-water mixture to make it settle, and then the precipitate was centrifuged, washed with deionized water until the supernatant was clear, and freeze-dried. 0.0204 g of the intermediate product II was obtained as a brown powder, and the yield was 48%.

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

Embodiment 2

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

[0052] Such as figure 1 As shown, in the PBS (pH=7) buffer solution system of 10 μmol / L probe molecule P, add anion solution (SO 4 2- , ClO 4 - 、HCO 3 - , OH - , F - , Cl - 、Br - , I - ) to make its concentration reach 100mmol / L, and the fluorescence experiment was measured on a fluorescence spectrophotometer of model LS55 produced by PE Company in the United States. From the figure, we can find that different anions can cause different degrees of fluorescence quenching of probe P, among which 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 cause the fluorescence of the probe molecule P to be quenched to varying degrees, but addi...

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Abstract

The invention provides an iodide ion recognition probe and a preparation method thereof, comprising the following steps: using (9,9-bis(6-bromohexyl)-2,7-difluorenal) as a raw material, using anhydrous LiCl as a catalyst Reaction with 2,5-diaminopyridine under certain conditions to obtain an intermediate product: under the condition of N,N-dimethylacetamide as a solvent, the intermediate product is reacted with trimethylamine to obtain a pyridine fluorenyl fluorescent conjugated polymer. The synthesis method of the invention is simple and easy for industrialized production. The invention can realize rapid, sensitive, accurate and economical detection of iodide ions, has high efficiency in practical application, and is especially suitable for detection of trace and trace iodide ions. The fluorescent probe of the present invention has high selectivity for iodide ion detection, and the minimum detection limit is 4.688×10 ‑7 mol / L, and shows a good linear quantitative relationship in the range of 0-25μmol / L, 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 for the human body. Too much or too little iodine intake can induce the occurrence of various thyroid-related diseases. The detection of iodine content in the human body not only has very important clinical significance in medicine, but also can timely evaluate the iodine nutritional status of the population in the area, timely guide the correct adjustment of iodine intake in the diet, and then reduce the iodine deficiency caused by iodine deficiency. It is of great significance to improve the quality of the whole nation's population. In addition, my country has abundant brine resources, and the determination of iodine content in brine plays an important role...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06
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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