Application of magnetic carboxylated covalent organic framework material as magnetic solid-phase extraction adsorbent

A technology of covalent organic framework and carboxylation, applied in the direction of selective adsorption, inorganic chemistry, alkali metal compounds, etc., can solve the problems of simultaneous enrichment and separation of multiple hazards, single extraction force mode of solid phase extractant, etc., to achieve Moderate pore size, improved qualitative and quantitative analysis, time-consuming effect

Active Publication Date: 2022-03-04
SOUTH CHINA UNIV OF TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because these multi-hazards have great differences in physical and chemical properties such as molecular weight, molecular polarity, stability, and solubility, and the extraction force mode of traditional solid-phase extraction agents is relatively single, this often leads to simultaneous enrichment of multi-hazards. Difficulty in separation

Method used

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  • Application of magnetic carboxylated covalent organic framework material as magnetic solid-phase extraction adsorbent
  • Application of magnetic carboxylated covalent organic framework material as magnetic solid-phase extraction adsorbent
  • Application of magnetic carboxylated covalent organic framework material as magnetic solid-phase extraction adsorbent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1 Synthesis and Adsorption Selectivity of Magnetic Carboxylated Covalent Organic Framework Materials

[0048] 1.2g FeCl 3 ·6H 2 O and 0.73 g FeCl 2 4H 2 O was dissolved in 20 mL of ultrapure water, then 2.8 mL of ammonia water was added, and stirred at 250 rpm for 5 min at room temperature. Then add 1.6 mL of dopamine hydrochloride solution, stir at room temperature for 1 h, collect the aminated magnetic iron oxide particles with a magnet, and wash with ultrapure water until the washing liquid is neutral. Subsequently, the aminated magnetic iron oxide particles were dispersed into 5 mL of ultrapure water at a concentration of 50 mg / mL, and then 25 mL of dioxane, 10 mg of trialdehyde phloroglucinol and 0.38 mL of glacial acetic acid were added, and reacted at 120 ° C for 1 h. The activated surface-aminated magnetic iron oxide particles were separated with a magnet and washed three times with THF and dioxane, respectively, and then redispersed in 5 mL of dioxa...

Embodiment 2

[0052] Example 2 The adsorption efficiency of carboxylated covalent organic framework materials to heterocyclic amines in chicken cakes

[0053] Mash and mix the commercially available Chaoshan Chicken Cake, accurately weigh 3g and disperse them into 4mL of acetonitrile and acetonitrile-heterocyclic amine spiked solution and stir evenly, then add 8mL of 1M sodium hydroxide solution, homogenize for 5min, and 100W ultrasonic Extract for 30min and centrifuge at 4000rpm for 15min. After homogenization was repeated twice, the supernatants were pooled. Subsequently, 5 mL of n-hexane was added to the supernatant for extraction to remove fat, and the lower layer of the liquid was removed by rotary evaporation to remove acetonitrile, and the remaining solution was added to distilled water to make up to 10 mL, then 5 mg of the material was weighed and dispersed into the above solution, and the Magnetic stirring was performed at a speed of 300 rpm for 1, 5, 10, 20, 30, 60, 90 and 120 mi...

Embodiment 3

[0054] Example 3 Adsorption efficiency of carboxylated covalent organic framework materials on heterocyclic amines in wife cakes

[0055] Mash and mix the commercially available wife cake, accurately weigh 3g and disperse them into 6mL of acetonitrile and acetonitrile-heterocyclic amine spiked solution and stir evenly, then add 7mL of 1M sodium hydroxide solution, homogenize for 5min, and extract with 100W ultrasonic for 30min , centrifuged at 4000rpm for 15min. After homogenization was repeated twice, the supernatants were pooled. Subsequently, 5 mL of cyclohexane was added to the supernatant for extraction to remove fat, and the lower layer of the supernatant was removed by rotary evaporation to remove acetonitrile, and the remaining solution was added to distilled water to make up to 10 mL, and then 5 mg of the material was weighed and dispersed into the above solution. Magnetic stirring was performed at room temperature at a speed of 300 rpm for 1, 5, 10, 20, 30, 60, 90 and...

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Abstract

The invention discloses application of a magnetic carboxylated covalent organic framework material as a magnetic solid-phase extraction adsorbent, and a preparation method of the material comprises the following steps: (1) firstly, by taking dopamine hydrochloride as a coordination stabilizer, synthesizing surface aminated magnetic iron oxide particles from ferric chloride and ferrous chloride through a coprecipitation method; and (2) activating the surface-aminated magnetic iron oxide particles, and carrying out covalent crosslinking on the surfaces of the aminated magnetic iron oxide particles through a solvothermal method under the reversible catalytic action of acetic acid by taking trialdehyde phloroglucinol and 4, 4-diaminobiphenyl-2, 2-dicarboxylic acid as construction units, so as to prepare the magnetic carboxylated covalent organic framework material. The carboxylated covalent organic framework material prepared by the method has a relatively large specific surface area and a good mesoporous structure, is stable in structure, large in adsorption capacity and short in equilibrium time and has multiple adsorption acting forces, so that the steps of sample pretreatment are greatly simplified, and the sample treatment time is shortened.

Description

technical field [0001] The invention relates to a magnetic carboxylated covalent organic framework material and its preparation method and its application in the analysis and detection of heterocyclic amine compounds in food, belonging to the technical field of porous framework material synthesis and analysis and detection. Background technique [0002] Food thermal processing pollutants are hazardous substances spontaneously produced during the processing of food raw materials. For a long time, due to the lack of understanding of the formation and transformation rules of chemical hazards in the processing process, safety problems caused by processing have emerged in endlessly, and serious situations have led to The types of foods that need to be monitored and analyzed are increasing, and the sample matrices are becoming more and more complex. Among them, heterocyclic amines are a class of chemical substances with mutagenic and carcinogenic effects produced during high-tempe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/28B01J20/22B01J20/30B01D15/08
CPCB01J20/28009B01J20/226B01J20/28011B01D15/08B01J2220/46Y02P10/20
Inventor 李晓玺王天星刘伟陈玲李冰
Owner SOUTH CHINA UNIV OF TECH
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