Covalent organic framework material, solid-phase micro-extraction probe and preparation method and application of solid-phase micro-extraction probe

A technology of covalent organic framework and probe, applied in the field of chemistry

Pending Publication Date: 2021-02-05
GUANGDONG INST OF ANALYSIS CHINA NAT ANALYTICAL CENT GUANGZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are few reports on the use of COFs to make SPME probes and combine them with atmospheric pressure open ionization mass spectrometry to achieve rapid and highly sensitive analysis of trace pollutants in complex matrices.

Method used

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  • Covalent organic framework material, solid-phase micro-extraction probe and preparation method and application of solid-phase micro-extraction probe
  • Covalent organic framework material, solid-phase micro-extraction probe and preparation method and application of solid-phase micro-extraction probe
  • Covalent organic framework material, solid-phase micro-extraction probe and preparation method and application of solid-phase micro-extraction probe

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1: Preparation of a covalent organic framework material for highly selective adsorption of perfluorinated and polyfluoroalkyl compounds

[0037] Preparation of a covalent organic framework material for highly selective adsorption of perfluorinated and polyfluoroalkyl compounds (see figure 1 ), the process involves the mixing of reaction raw materials and solvents, the addition of catalysts, the formation of imine products under certain conditions and the post-treatment of products. details as follows:

[0038]First, mix 2,3,5,6-tetrafluoro-p-benzaldehyde and 2,4,6-(4-aminophenyl)-1,3,5-triazine monomers in a stoichiometric ratio of 3:2 , wherein the dosage of 2,3,5,6-tetrafluoro-p-benzaldehyde is 61.8mg, and the dosage of 2,4,6-(4-aminophenyl)-1,3,5-triazine is 70.9mg; Then add 3.5mL of N,N-dimethylformamide, sonicate until the reactant is completely dissolved, then add 15mL of acetonitrile and 35mL of o-dichlorobenzo and sonicate until mixed; then add 2mL of ...

Embodiment 2

[0039] Example 2: Preparation of a biocompatible solid-phase microextraction probe based on highly selective adsorption of covalent organic framework materials by perfluorinated and polyfluoroalkyl compounds

[0040] Preparation of a biocompatible solid-phase microextraction probe based on perfluorinated and polyfluoroalkyl compounds with high selective adsorption of covalent organic framework materials, using a direct coating method (see Figure 4 ), the process includes etching the probe carrier, coating the adhesive on the etched carrier, adhering the above-mentioned covalent organic framework material powder with the probe carrier coated with the adhesive, curing the adhesive, biocompatible Coating modification and probe post-processing.

[0041] First, take a 304 stainless steel needle (diameter 0.5 mm, length 3 cm), and ultrasonically clean it in acetone, ultrapure water and methanol for 30 minutes to remove surface impurities; then, immerse the stainless steel needle in...

Embodiment 3

[0042] Example 3: Study on the adsorption capacity of COFs-SPME

[0043] Under optimized experimental conditions, COFs-SPME and open nano-electrospray mass spectrometry were used to analyze a series of concentrations of perfluorooctane sulfonic acid (PFOS) in pure water spiked solutions to study the adsorption capacity of COFs-SPME probes .

[0044] It was observed that the adsorption saturation concentration of COFs-SPME probe to PFOS was 50ng / μL (see Figure 5 ). Then, under the same experimental conditions, the standard solution of PFOS in methanol solution was analyzed by nano-electrospray mass spectrometry, and it was found that the concentration that produced the same signal intensity as saturated extraction was 1.2 μg / μL. Since 2 μL of methanol was used for desorption during the analysis, the adsorption capacity of the COFs-SPME probe was calculated to be 2.4 μg of PFOS.

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Abstract

The invention discloses a covalent organic framework material, a solid-phase microextraction probe and a preparation method and application thereof. The covalent organic framework material comprises 2, 3, 5, 6-tetrafluoro-p-dibenzaldehyde and a 2, 4, 6-tri(4-aminophenyl)1, 3, 5-triazine repetitive structure unit which take an imine bond as a connection mode. The solid-phase micro-extraction probeprepared from the material has high selectivity and high enrichment capacity on perfluoro and polyfluoroalkyl compounds, can be directly combined with a nanoliter electrospray ion source for mass spectrometry after sampling extraction, and has extremely high sensitivity, the method can be used for rapid, accurate and sensitive analysis of trace perfluoroalkyl and polyfluoroalkyl compounds in complex environments and biological samples.

Description

technical field [0001] The invention belongs to the field of chemistry, and in particular relates to a covalent organic framework material, a solid-phase microextraction probe and a preparation method and application thereof. Background technique [0002] Per- and polyfluoroalkyl substances (PFASs) are a class of persistent organic pollutants (POPs) widely present in the environment and organisms. Multiple studies have shown that PFASs have liver, reproductive development, and immunotoxicity, as well as potential carcinogenic effects. Perfluorooctanesulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) are the two most widely used PFASs, which were listed in the Stockholm Convention in 2009 and 2015. In order to clearly understand the environmental behavior and biological toxicity of PFASs, it is necessary to monitor the content and composition of PFASs in the environment and in vivo. [0003] Mass spectrometry is the method of choice for the analysis of PFASs in complex ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/30G01N27/62
CPCB01J20/285G01N27/62
Inventor 侯雅君杨运云何凯丽
Owner GUANGDONG INST OF ANALYSIS CHINA NAT ANALYTICAL CENT GUANGZHOU
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