Metal organic frame fluorescent probe and application thereof in hydrogen sulfide detection

A metal-organic framework, fluorescent probe technology, applied in 3/13 groups of organic compounds without C-metal bonds, organic chemistry, fluorescence/phosphorescence, etc., can solve the problem of poor selectivity, complex working environment of small molecule fluorescent probes, The synthesis is cumbersome and complicated, and the effects of high selectivity, high yield and simple synthesis route are achieved.

Active Publication Date: 2016-09-28
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are many small-molecule fluorescent probes currently used to detect common metal ions and chemical substances in the environment and organisms, the working environment of small-molecule fluore

Method used

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  • Metal organic frame fluorescent probe and application thereof in hydrogen sulfide detection
  • Metal organic frame fluorescent probe and application thereof in hydrogen sulfide detection
  • Metal organic frame fluorescent probe and application thereof in hydrogen sulfide detection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Add ZrCl to the round bottom flask 4 (2.43 g, 10.4 mmol), pyromellitic acid (2.54 g, 10 mmol), deionized water (60 mL) and glacial acetic acid (40 mL), stirred at room temperature for 30 min, and placed in an oil bath at 100 °C Condensation and reflux reaction for 24 h;

[0028] After cooling to room temperature, centrifuge, disperse the precipitate in deionized water, repeat centrifugal washing 3 times, after centrifugation, the obtained precipitate is UiO-66-(COOH) containing uncoordinated carboxyl group 2 ;

[0029] (2) Take the UiO-66-(COOH) synthesized above 2 (0.1 g) was uniformly dispersed in deionized water (10 mL), and Eu(NO 3 ) 3 ·6H 2 O (0.446 g, 1 mmol) and Cu(NO 3 ) 2 2.5H 2 O (0.465 g, 1 mmol), condensed and refluxed at 60°C for 24 h; cooled to room temperature and centrifuged, dispersed the precipitate in deionized water, centrifuged and washed 3 times repeatedly, after centrifuged, exchanged with acetone for 3 days, and replaced every day ...

Embodiment 2

[0033] (1) Add Zr(NO 3 ) 4 ·5H 2 O (4.46 g, 10.4 mmol), pyromellitic acid (2.10 g, 10 mmol), deionized water (60 mL) and glacial acetic acid (40 mL), stirred at room temperature for 30 min, and placed in an oil bath at 100 °C Condensation and reflux reaction in middle temperature for 24 h; after cooling to room temperature and centrifugation, the precipitate was dispersed in deionized water, and centrifuged and washed 3 times repeatedly. After centrifugation, the obtained precipitate was UiO-66-(COOH) containing uncoordinated carboxyl groups. 2 ;

[0034] (2) Take the UiO-66-(COOH) synthesized above 2 (0.1 g) was uniformly dispersed in deionized water (10 mL), and EuCl 3 ·6H 2 O (0.366 g, 1 mmol) and Cu(NO 3 ) 2 2.5H 2 O (0.465 g, 1 mmol), stirred and condensed at 90°C for reflux for 12 hours; cooled to room temperature and centrifuged, dispersed the precipitate in deionized water, repeated centrifuged and washed 3 times, after centrifuged, exchanged with acetone for ...

Embodiment 3

[0036] Example 3 Selectivity, response time and sensitivity of metal-organic framework fluorescent probes for hydrogen sulfide detection

[0037] (1) Take 1 mL of 5 mM containing F - , Cl - , Br - , I - , HS - , HCOO - , CH 3 COO - , NO 2 - , SiO 3 2- , NO 3 - , HPO 4 2- , PO 4 3- , P 3 o 9 3- , S 2 o 3 2- , SO 4 2- , HCO 3 - , and N 3 - The sodium salt solution of the anion is placed in a cuvette, and 1 mg of fluorescent probe Eu is added to each cuvette 3+ / Cu 2+ @UiO-66-(COOH) 2 , shake well, and measure its fluorescence emission spectrum at an excitation wavelength of 305 nm after 30 seconds (such as image 3 shown), the results show that adding these anions: F - , Cl - , Br - , I - , HCOO - , CH 3 COO - , NO 2 - , SiO 3 2- , NO 3 - , HPO 4 2- , PO 4 3- , P 3 o 9 3- , S 2 o 3 2- , SO 4 2- , HCO 3 - , and N 3 - The sodium salt solution of the fluorescent probe Eu 3+ / Cu 2+ @UiO-66-(COOH) 2 The fluorescence inten...

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Abstract

The invention discloses a metal organic frame fluorescent probe and application thereof in hydrogen sulfide detection. A preparation method of the metal organic frame fluorescent probe comprises the steps that 1, UiO-66-(COOH)2 containing non-coordinate carboxyl is prepared and synthesized; 2, stirring and heating are utilized, metal ions Eu3+ and Cu2+ are successfully coordinate with the non-coordinate carboxyl of UiO-66-(COOH)2, and the fluorescent probe Eu3+/Cu2+@UiO-66-(COOH)2 is obtained. The metal organic frame fluorescent probe is good in stability, and the probe can be used for rapid recognition and quantitative detection of hydrogen sulfide, and has the high selectivity and good anti-jamming capability; ratio fluorescent analysis can be achieved, influences of detection condition differences on results are greatly eliminated, and the detection sensitivity is improved. The metal organic frame fluorescent probe can be used for detecting hydrogen sulfide in environmental, biological, chemical and other samples.

Description

technical field [0001] The invention relates to a metal organic framework fluorescent probe and its application, especially the application in hydrogen sulfide detection. Background technique [0002] For centuries, hydrogen sulfide (H 2 S) Toxic pollution to the environment has been intensively studied. However, recent studies on physiological endogenous H 2 Research work on S has been devoted to its regulation of several physiological functions. h 2 S, a gas with a special odor, was confirmed to be the third endogenous gas signal molecule after nitric oxide and carbon monoxide. At physiological concentrations, H 2 S is involved in a series of physiological regulation processes, such as regulation of vascular tone, myocardial contraction, nerve conduction and insulin secretion, etc. Once a cell is unable to maintain its normal H 2 S concentration, it will cause diseases such as arterial and pulmonary hypertension, Alzheimer's disease, gastric mucosal injury and liver...

Claims

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Application Information

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IPC IPC(8): C07F19/00C09K11/06G01N21/64
CPCC07F5/003C09K11/06C09K2211/188G01N21/6428G01N21/643G01N21/6486
Inventor 杨雨张新崔元靖钱国栋
Owner ZHEJIANG UNIV
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