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A curd-shaped covalent organic framework material and its preparation and application

A covalent organic framework and curd-shaped technology, applied in the field of covalent organic framework materials and analysis and detection, can solve the problems of universal applicability to be explored, achieve high sensitivity and reproducibility, good linear relationship, and reduce costs

Active Publication Date: 2022-07-19
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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  • A curd-shaped covalent organic framework material and its preparation and application
  • A curd-shaped covalent organic framework material and its preparation and application
  • A curd-shaped covalent organic framework material and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1. the preparation of curd-shaped covalent organic framework material:

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

Embodiment 2

[0044] Embodiment 2. Inter-column and intra-column repeatability of flower-shaped covalent organic framework solid-phase extraction column:

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

Embodiment 3

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

[0048] After the tap water sample was filtered through a 0.45 microporous membrane, 500 mL of tap water was accurately measured, and the concentration of sodium chloride was adjusted to 0.1 mol·L -1 . Drive tap water and spiked tap water with a vacuum pump through a pre-activated flower ball-shaped covalent organic framework (using the method of Example 1) solid phase extraction column, eluted with 5% ammonia water-methanol, and blow the eluent nitrogen to dryness, Reconstituted, passed through a 0.22 μm filter membrane, and detected by high performance liquid chromatography tandem mass spectrometry. Quinolone antibiotics were not detected in tap water. The accuracy of the method was checked by the method of spike recovery. As shown in Table 3, the recovery rate of quinolone antibiotics in spiked water samples was between 85.2% and 103.5%, indicating that the...

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Abstract

The invention relates to a curd-shaped covalent organic framework material and its preparation and application. The present invention uses tris(4-aminophenyl)amine and 1,3,5-tris(4-formylphenyl)benzene as monomers, and reacts at room temperature to prepare curd-shaped balls with good crystallinity and stacking of nano-sheets Structure of covalent organic framework materials. Using the curd-shaped covalent organic framework material as a solid-phase extraction adsorbent, the separation and enrichment of quinolone antibiotics can be realized, and the recycling performance is good, which greatly reduces the use cost. Combined with high performance liquid chromatography tandem mass spectrometer, a method for the detection of trace quinolone antibiotics in complex samples such as environmental water and food was constructed, which has the advantages of high accuracy, good reproducibility and low detection limit.

Description

technical field [0001] The invention belongs to the field of covalent organic framework materials and analysis and detection, in particular to a curd-shaped covalent organic framework material and applications thereof. Background technique [0002] The disclosure of information in this Background section is only for enhancement of understanding of the general background of the invention and should not necessarily be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art. [0003] Quinolone antibiotics are widely used in medical treatment, livestock and aquatic animal breeding as drugs for the prevention and treatment of infectious diseases and antibacterial growth promoters. However, improper or excessive use of these drugs leads to excessive residues in environmental water bodies and food, which pose a serious threat to ecosystems and human health. How to efficiently detect quin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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