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A method for the enrichment and detection of sulfonamide antibiotics based on porous covalent organic nitrogen framework materials

A technology of covalent organic, framework materials, applied in the field of analysis and detection, can solve problems such as residues, ecosystem and human health threats

Active Publication Date: 2021-04-09
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in recent years, improper or excessive use of such drugs has resulted in excessive residues in environmental water bodies and animal-derived foods, posing a serious threat to ecosystems and human health (Environmental Pollution, 2009, 157, 2893-2902)

Method used

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  • A method for the enrichment and detection of sulfonamide antibiotics based on porous covalent organic nitrogen framework materials
  • A method for the enrichment and detection of sulfonamide antibiotics based on porous covalent organic nitrogen framework materials
  • A method for the enrichment and detection of sulfonamide antibiotics based on porous covalent organic nitrogen framework materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1. Preparation of porous covalent organic nitrogen framework material solid-phase extraction column and extraction analysis water sample:

[0038] Weigh 3mmol of 3,3'-diaminobenzidine and 1mmol of phosphazene trichloride into a three-neck flask, add 30mL of dimethyl sulfoxide, stir at room temperature for 30min under nitrogen atmosphere, heat up to 125°C, stir for 30min, and cool to The porous covalent organic nitrogen framework material was obtained by centrifugal washing and drying at room temperature. Such as figure 1 As shown, nearly spherical particles with a diameter of about 200 nanometers growing together were obtained. Weigh 100mg of porous covalent organic nitrogen framework material, transfer it into a 6mL empty column tube, and compact it with a 1.2mm thick sieve plate to obtain a solid phase extraction column. The obtained solid-phase extraction cartridge was activated with equal volumes of methanol and water sequentially before use.

[0039]...

Embodiment 2

[0043] Example 2. Preparation and Extraction Analysis of Porous Covalent Organic Nitrogen Framework Material Solid Phase Extraction Column Milk Sample:

[0044] Weigh 3mmol of 3,3'-diaminobenzidine and 1mmol of phosphazene trichloride into a three-neck flask, add 15mL of dimethyl sulfoxide, stir at room temperature for 30min under nitrogen atmosphere, heat up to 125°C, stir for 30min, and cool to The porous covalent organic nitrogen framework material was obtained by centrifugal washing and drying at room temperature. Use a 3mL empty column tube to fill 60mg of porous covalent organic nitrogen framework material, and compact it with a 1.6mm thick sieve plate to obtain a solid phase extraction column, which is activated with equal volumes of methanol and water in sequence before use.

[0045] First, remove the protein and fat in the milk sample, weigh 10g of milk, add 30mL of acetonitrile and sonicate for 10min, and centrifuge to collect the supernatant; add 30mL of n-hexane to...

Embodiment 3

[0049] Example 3. Preparation of porous covalent organic nitrogen framework material solid-phase extraction column and extraction and analysis of honey samples:

[0050] Weigh 3mmol of 3,3'-diaminobenzidine and 1mmol of phosphazene trichloride into a three-necked flask, add 6mL of dimethyl sulfoxide, stir at room temperature for 30min under nitrogen atmosphere, heat up to 125°C, stir for 30min, and cool to The porous covalent organic nitrogen framework material was obtained by centrifugal washing and drying at room temperature. A 12mL empty column tube was used to fill 150mg of porous covalent organic nitrogen framework material, and was compacted with a 2.5mm thick sieve plate to obtain a solid phase extraction column, which was activated with equal volumes of methanol and water in sequence before use.

[0051] Weigh 10g honey into a 50mL centrifuge tube, add 5mL ultrapure water and vortex mix, add 5mL methanol, vortex mix for 1min, shake for 10min, centrifuge at 4000r / min fo...

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Abstract

The invention relates to a method for enriching and detecting sulfonamide antibiotics based on a porous covalent organic nitrogen framework material, and belongs to the field of detection of sulfonamide antibiotics. Aiming at the technical problems such as low sensitivity of the sulfonamide detection method in the prior art and relatively complex detection matrix, the present invention provides a method that uses a porous organic nitrogen framework material as a solid phase extraction column filler, and enriches the sample to be tested through the solid phase extraction column. A method for detecting trace amounts of sulfonamide antibiotics in samples combined with liquid chromatography-tandem mass spectrometry. This method can better separate the target substance from the coexisting matrix interference substance, and achieve better enrichment and purification. It has the advantages of high detection sensitivity, good reproducibility, simple and fast, and low detection cost. It can be used for food and Environmental water safety supervision and law enforcement provide strong technical support.

Description

technical field [0001] The invention belongs to the field of analysis and detection, and in particular relates to a method for detecting sulfonamide antibiotics with a porous covalent organic nitrogen frame material used as solid-phase extraction column packing combined with liquid mass spectrometry technology. Background technique [0002] Sulfonamide antibiotics are widely used in medical treatment, poultry and aquatic animal breeding as drugs for preventing and treating infectious diseases and antibacterial growth promoters. However, in recent years, improper or excessive use of such drugs has resulted in excessive residues in environmental water bodies and animal-derived foods, posing serious threats to ecosystems and human health (Environmental Pollution, 2009, 157, 2893-2902). In order to protect the environment and ensure the quality and safety of animal-derived food, the residue analysis of sulfonamide antibiotics has increasingly become a key research object. [00...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/60
CPCG01N30/02G01N30/06G01N30/08G01N30/60G01N30/6052G01N2030/027G01N2030/062
Inventor 徐桂菊赵汝松张贝贝王晓利李娜
Owner SHANDONG ANALYSIS & TEST CENT
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