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A kind of solid-phase microextraction probe and its preparation method and application

An extraction and probe technology, applied in chemical instruments and methods, other chemical processes, instruments, etc., can solve the problems that limit the further development and development of solid-phase microextraction technology, the limited types of extraction coatings, and the easy breakage of extraction heads. Simple and fast preparation steps, uniform and controllable coating thickness, and strong resistance to matrix interference

Active Publication Date: 2021-09-07
HUAZHONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, commercial solid-phase microextraction probes mostly use quartz fiber as a carrier, and the extraction head is easily broken during operation, and there are still the following problems: commercialized extraction coatings are limited and expensive (800-900 yuan / piece) , low extraction efficiency, poor extraction selectivity, etc.
These unfavorable factors limit the further development of solid phase microextraction technology, so it is urgent to develop and research more new solid phase microextraction coatings.

Method used

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  • A kind of solid-phase microextraction probe and its preparation method and application
  • A kind of solid-phase microextraction probe and its preparation method and application
  • A kind of solid-phase microextraction probe and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Example 1 Preparation of MWCNTs / PANI-PPy@PDMS composite solid-phase microextraction probe

[0040] The present invention prepares the MWCNTs / PANI-PPy composite material coating by in-situ electrodeposition, and then prepares the solid-phase microextraction probe by the direct adhesion method, and the preparation process is as follows figure 1 , including the following steps:

[0041](1) prepare MWCNTs / PANI-PPy composite material coating according to the method for comparative example 1;

[0042] (2) Prepare polydimethylsiloxane diluent according to the method of comparative example 2;

[0043] (3) Insert the MWCNTs / PANI-PPy composite fiber head described in step (1) into the polydimethylsiloxane diluent with a depth of 1.5cm, take it out after standing for 5s, and dry the surface of the fiber head with filter paper Visible droplets were cured at 100°C for 9 hours, and a PDMS protective layer with a thickness of 4.1 μm was formed on the coating surface, and the MWCNTs / ...

Embodiment 2

[0047] Example 2 The Enrichment Ability of Solid-Phase Microextraction Probes to Organochlorine Pesticides and Heterocyclic Pesticides

[0048] Determination of the MWCNTs / PANI-PPy@PDMS composite solid-phase microextraction probe prepared in Example 1 of the present invention and four kinds of commercial extraction probes are effective against organochlorine pesticides (hexachlorobenzene, chlorothalonil), heterocyclic insecticides agent (fipronil, chlorfenapyr) enrichment capacity.

[0049] The four commercial probes were purchased from SUPELCO, specifically including: polydimethylsiloxane (PDMS), thickness 100 μm, non-polar probe, model 57300-U; polydimethylsiloxane / dimethicone Vinylbenzene (PDMS / DVB), 65 μm thick, bipolar, model 57310-U; carbon molecular sieve / polydimethylsiloxane (CAR / PDMS), 85 μm, bipolar, model 57334-U; polyacrylic acid Ester (PA), thickness 85μm, type 57304, polar.

[0050] The probe prepared in Example 1 of the present invention and four commercial ex...

Embodiment 3

[0051] Example 3 Comparison of the extraction capabilities of MWCNTs / PANI-PPy@PDMS probes and other two self-made probes for organochlorine pesticides and heterocyclic pesticides

[0052] Measure the MWCNTs / PANI-PPy@PDMS composite solid-phase microextraction probe that the embodiment of the present invention makes, the MWCNTs / PANI-PPy probe that comparative example 1 makes and the PDMS probe that comparative example 2 make have to organic The enrichment capacity of chlorinated pesticides (hexachlorobenzene, chlorothalonil) and heterocyclic insecticides (fipronil, chlorfenapyr).

[0053] The probe prepared in Example 1 of the present invention, the MWCNTs / PANI-PPy probe and the self-made PDMS probe were respectively extracted with mixed standard aqueous solutions of hexachlorobenzene, chlorothalonil, fipronil and chlorfenapyr. Then insert the extracted probe into the GC-MS inlet for thermal desorption, analyze and compare the peak areas of each substance, so as to compare the e...

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Abstract

The invention belongs to the field of solid-phase microextraction, and in particular relates to a novel solid-phase microextraction probe, its preparation method and application. The solid-phase microextraction probe includes stainless steel fibers and a surface coating coated on the stainless steel fibers, and the surface coating is a composite coating of multi-walled carbon nanotubes / polyaniline-polypyrrole@polydimethylsiloxane Floor. The solid-phase microextraction probe of the present invention has better biocompatibility, stronger anti-matrix interference ability, is more suitable for the pretreatment of organic matter in complex matrices, and can directly expose the probe of the present invention to living organisms Tissue extraction and enrichment for target analytes. Utilizing the probe of the present invention for analysis and detection not only has low detection limit and good reproducibility, but also has higher extraction efficiency compared with existing commercialized fibers; meanwhile, the solid-phase microextraction probe of the present invention The needle preparation steps are simple and quick, the preparation cost is low, the thickness of the prepared coating is uniform and controllable, the mechanical properties are good, and the reproducibility is excellent.

Description

technical field [0001] The invention belongs to the field of solid-phase microextraction, and in particular relates to a novel solid-phase microextraction probe and its preparation method and application. Background technique [0002] Solid phase microextraction (SPME) is a sample preparation technique based on the equilibrium distribution of target analytes between the sample matrix and the extraction phase. This technology integrates sampling, extraction, concentration, and sample injection, does not consume solvents, and can process specific trace substances in different complex matrix samples in a green, efficient, and fast manner, and can be used online with instruments. Therefore, SPME is widely used in environmental protection, food monitoring, biomedicine and other fields. [0003] The core of solid phase microextraction technology lies in the selection and immobilization of the solid phase microextraction coating on the probe. The development and preparation of the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/281B01J20/32B01D15/08C02F1/28G01N30/02G01N30/06
CPCB01D15/08B01J20/281B01J20/3231C02F1/288G01N30/02G01N30/06G01N2030/062
Inventor 徐晖陈天天
Owner HUAZHONG NORMAL UNIV
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