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Flower-ball-shaped covalent organic framework material as well as preparation and application thereof

A covalent organic framework and curd-shaped technology, which is applied in the field of covalent organic framework materials and analysis and detection, can solve problems such as universal applicability to be explored, and achieve the effects of high sensitivity and reproducibility, simple preparation method and cost reduction.

Active Publication Date: 2020-06-19
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of the room temperature method is that it breaks through the bottleneck of high-temperature solvothermal synthesis, and has great potential for large-scale and industrial production. However, its general applicability to monomers remains to be explored

Method used

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  • Flower-ball-shaped covalent organic framework material as well as preparation and application thereof
  • Flower-ball-shaped covalent organic framework material as well as preparation and application thereof
  • Flower-ball-shaped covalent organic framework material as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1. The preparation of flower spherical covalent organic framework material:

[0043] Weigh 0.6mmol of tris(4-aminophenyl)amine and 0.6mmol of 1,3,5-tris(4-formylphenyl)benzene into a three-necked flask, add 6mL of mesitylene and 6mL of 1,4-dioxo Hexacyclic, after ultrasonication for 5min, add 1.2mL6mol·L -1 Acetic acid, reacted at 25°C for 72 hours, centrifuged, washed and dried to obtain flower-shaped covalent organic framework materials. Its scanning electron microscope picture, X-ray diffraction picture and Fourier transform infrared spectrum picture are as follows respectively figure 1 , figure 2 and image 3 shown.

Embodiment 2

[0044] Example 2. Intercolumn and intracolumn repeatability of curd covalent organic framework solid phase extraction column:

[0045] The curd-shaped covalent organic framework materials (using the method in Example 1) prepared in different batches were weighed and filled into 6 mL empty column tubes, and the sieve plate was compacted to obtain six curd-shaped covalent organic framework solid-phase extraction columns. Adjust the concentration of sodium chloride in ultrapure water to 0.1mol L -1 , add 1mL 25μg·L -1 The mixed standard of quinolone antibiotics, after mixing evenly, was loaded onto a pre-activated solid phase extraction column, eluted with 5% ammonia water-methanol, and the eluent was blown to dryness with nitrogen, after reconstitution, passed through a 0.22 μm filter membrane, Detection by high performance liquid chromatography tandem mass spectrometry. The relative standard deviations ranged from 2.7% to 9.8%, indicating that the curd-shaped covalent organic...

Embodiment 3

[0047] Embodiment 3. Spherical covalent organic framework solid-phase extraction column analyzes tap water sample:

[0048] After the tap water sample is filtered through a 0.45 microporous membrane, accurately measure 500mL of tap water and adjust the concentration of sodium chloride to 0.1mol L -1 . Tap water driven by a vacuum pump and spiked tap water pass through a pre-activated curd-shaped covalent organic framework (using the method of Example 1) solid-phase extraction column, eluted by 5% ammonia water-methanol, and the eluent is blown to dryness with liquid nitrogen. Reconstituted, passed through a 0.22 μm filter membrane, and detected by high performance liquid chromatography tandem mass spectrometry. No quinolone antibiotics were detected in tap water. The accuracy of the method was examined by the method of standard recovery. As shown in Table 3, the recoveries of quinolone antibiotics in spiked tap water samples ranged from 85.2% to 103.5%, indicating that the ...

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PUM

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Abstract

The invention relates to a flower-ball-shaped covalent organic framework material as well as preparation and application thereof. Tris (4-aminophenyl) amine and 1, 3, 5-tris (4-formylphenyl) benzene are used as monomers, and the covalent organic framework material with high crystallinity and a flower-ball-shaped structure formed by stacking nanosheets is prepared through a reaction at room temperature. When the flower-ball-shaped covalent organic framework material is used as a solid-phase extraction adsorbent, separation and enrichment of quinolone antibiotics can be realized, the recycling performance is good, and the use cost is greatly reduced. By combining a high performance liquid chromatography tandem mass spectrometer, a detection method for trace quinolone antibiotics in complex samples such as environmental water and food is formed, and the accuracy and reproducibility are high, and the detection limit is low.

Description

technical field [0001] The invention belongs to the field of covalent organic framework materials and analysis and detection, and in particular relates to a flower-shaped covalent organic framework material and applications thereof. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Quinolones antibiotics, as anti-infectious disease drugs and antibacterial growth promoters, are widely used in medical treatment, poultry and aquatic animal breeding. However, improper or excessive use of these drugs leads to excessive residues in environmental water and food, posing a serious threat to ecosystems and human health. How to effectively detect quinolone antibiotics in complex samp...

Claims

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Application Information

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IPC IPC(8): G01N30/02B01J20/26B01J20/28B01J20/30B01D15/10C02F1/28C02F101/36C02F101/30
CPCC08G83/008G01N30/02B01J20/264B01J20/28019B01D15/08C02F1/285C02F2101/36C02F2101/30
Inventor 徐桂菊赵汝松候龙飞刘璐王晓利
Owner SHANDONG ANALYSIS & TEST CENT
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