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Preparation of terbium-based rare earth crystalline material and its application in fluorescence detection of antibiotics in water

A fluorescence detection, rare earth technology, applied in luminescent materials, analytical materials, fluorescence/phosphorescence, etc., can solve the problems of cumbersome, time-consuming operation and high cost

Active Publication Date: 2022-03-08
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, antibiotic detection mainly adopts ultra-high performance liquid chromatography-tandem mass spectrometry technology with high precision but high cost; magnetic solid-phase extraction technology with simple and fast operation but cumbersome preparation of magnetic polymers and magnetic molecular imprinted materials, and high sensitivity Molecularly imprinted enzyme-linked immunoassay with good operability but high detection cost and time-consuming operation

Method used

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  • Preparation of terbium-based rare earth crystalline material and its application in fluorescence detection of antibiotics in water
  • Preparation of terbium-based rare earth crystalline material and its application in fluorescence detection of antibiotics in water
  • Preparation of terbium-based rare earth crystalline material and its application in fluorescence detection of antibiotics in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh 0.0167g of organic ligand, 0.0271g of terbium nitrate hexahydrate, 1mL of N,N-dimethylformamide, 1mL of polyethylene glycol-400 and 3mL of deionized water, adjust the pH of the solution to 2.0 with 6M nitric acid, add In a Teflon-lined stainless steel reactor, react at a constant temperature of 100°C for 24 hours, and cool down to room temperature to obtain a colorless and transparent terbium rare earth crystal material.

[0036] The single crystal of the terbium rare earth crystalline material synthesized by the present invention uses the small molecule type X-ray single crystal diffractometer of Japan Rigaku Company to carry out structure determination on the crystal, and utilizes the Mo Kα ray monochromated by the graphite monochromator, under 173K The data such as diffraction intensity and unit cell parameters were measured, and the collected data were corrected by empirical absorption using scanning technology. The results obtained were analyzed by the direct me...

Embodiment 2

[0042] Configure 11 antibiotics into 2×10 -4 M solution, 11 antibiotics including penicillin (PCL), florfenicol (FFC), chloramphenicol (CAP), sulfamethazine (SMZ), sulfadiazine (SDZ), ornidazole (ODZ), Dimetridazole (DTZ), metronidazole (MDZ), ronidazole (RDZ), nitrofurantoin (NFT), nitrofurazone (NZF). 5mg of the terbium rare earth crystalline material obtained in Example 1 were added to 10mL 2×10 -4 M antibiotic solution, ultrasonically dispersed at room temperature for 20 minutes, got 3mL suspension and moved it into a cuvette and tested the fluorescence spectrum of the suspension, and focused on comparing the 548nm before and after adding different antibiotics ( 5 D. 4 → 7 f 5 ) changes in fluorescence intensity at the emission peak. The above-mentioned fluorescence tests are all carried out at room temperature and under the conditions of an optimal excitation wavelength of 230nm.

[0043] Figure 5 It is the solid fluorescence emission diagram of the terbium-based ...

Embodiment 3

[0047] 5 mg of the terbium rare earth crystalline material in Example 1 were added to 10 mL of SMZ aqueous solutions containing different concentrations, ultrasonically dispersed at room temperature for 20 minutes, and 3 mL of the suspension was transferred into a cuvette and tested at the optimal excitation wavelength of 230 nm. Fluorescence spectra, such as Figure 8 The fluorescence quenching of the material to different concentrations of SMZ antibiotics and the 5 D. 4 → 7 f 5 Fluorescent emission conditions. Figure 8 (a) is the fluorescence intensity variation diagram (in the figure, from top to bottom is H 2 O, 2×10 -6 M, 4×10 -6 M, 5×10 -6 M, 1×10 -5 M, 3×10 -5 M, 5×10 -5 M, 8×10 -5 M, 1×10 -4 M, 1.5×10 -4 M, 2×10 -4 M); (b) is when different concentrations of antibiotic sulfamethazine (SMZ) are added to the aqueous solution of terbium-based rare earth crystalline materials 5 D. 4 → 7 f 5 Fluorescence emission intensity change graph. With the increase...

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Abstract

The chemical molecular formula of the terbium-based rare earth crystalline material of the present invention is [Tb(TZBT)(H 2 O) 2 ] n ; Wherein, n represents positive infinity, TZBT represents 1-(1,3,4-triazolyl)-2,4,6-tricarboxylate, and its valence is negative trivalent. The invention has strong fluorescence emission, can be used for the detection of antibiotics in water, and belongs to the field of crystalline materials and fluorescence detection materials. The preparation method of the material is as follows: under closed conditions, the organic ligand 1-(1,3,4-triazolyl)-2,4,6-trimesic acid and terbium nitrate hexahydrate in N,N-di In the mixed solution of methylformamide and water, the surfactant polyethylene glycol 400 is used to adjust, and the terbium-based rare earth crystalline material is obtained through solvothermal reaction. The advantages of the present invention are: the synthesis process of the terbium-based rare earth crystalline material is simple, the crystallization purity is high, the yield is high, and the reproducibility is good; it has high stability in aqueous solution; and antibiotics can be detected with high selectivity in various antibiotic aqueous solutions Sulfamethazine (SMZ).

Description

technical field [0001] The invention belongs to the field of crystal materials and fluorescent detection materials, and the technology relates to 1-(1,3,4-triazolyl)-2,4,6-tribenzenetricarboxylic acid as a ligand and rare earth terbium ions as a metal center. The preparation of terbium-based rare earth crystalline materials, and the application of this material to the efficient and selective detection of the antibiotic sulfamethazine in aqueous solution at room temperature. Background technique [0002] Rare earth crystalline materials are a kind of inorganic-organic hybrid materials prepared by self-assembly of rare earth ions or clusters and organic ligands. Such materials not only have the inherent physical and chemical properties of inorganic and organic units, but also have the hybrid properties of inorganic-organic hybrids. As the metal center of rare earth crystalline materials, lanthanide ions have advantages such as narrow-spectrum luminescence, good color purity, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00C09K11/06G01N21/64
CPCC09K11/06C08G83/008G01N21/643C09K2211/182C09K2211/1466C09K2211/1425G01N2021/6432
Inventor 董文文于晓燕鲍伟方义铭赵君李东升
Owner CHINA THREE GORGES UNIV
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