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Solid phase microextraction head and preparation method and application thereof

A solid-phase microextraction head and extraction technology, which is applied in chemical instruments and methods, other chemical processes, alkali metal oxides/hydroxides, etc., can solve the problems of sensitivity improvement and achieve the effect of improving sensitivity

Active Publication Date: 2020-01-17
HONGHE COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its core technology is the preparation of the extraction head. The sensitivity of the SPME head in the prior art needs to be improved when detecting organic phosphorus.

Method used

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  • Solid phase microextraction head and preparation method and application thereof
  • Solid phase microextraction head and preparation method and application thereof
  • Solid phase microextraction head and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1: the preparation (PPY) of solid-phase microextraction head

[0045] Such as figure 1As shown, the platinum wire as the counter electrode, the saturated calomel electrode as the reference electrode and the stainless steel wire as the working electrode were assembled into a three-electrode electrochemical working system. In the range of 0-1.5V cyclic voltammetry, scan 100 cycles at a speed of 0.05mV / s, then take out the prepared SPME head, rinse with ethanol and deionized water to remove impurities on the surface, and dry it for later use. Afterwards, the extraction head was bonded to the handle of the self-made injector in this experiment with a mixed resin of epoxy resin and polyamide resin at a ratio of 1:1, and dried in the air. Extraction injector. Next, insert the SPME head into the GC inlet through the injection handle, and age the extraction head for 5 minutes at a temperature of 250°C in the inlet.

Embodiment 2

[0046] Embodiment 2: the preparation of solid phase microextraction head (PPY-IL)

[0047] Such as figure 1 As shown, the platinum wire as the counter electrode, the saturated calomel electrode as the reference electrode and the stainless steel wire as the working electrode were assembled into a three-electrode electrochemical working system, and the three electrodes were immersed in a solution containing 40.0 μL / mL pyrrole and 2.0 mg / mL In the mixed solution of 1-butyl-3-methylimidazolium hexafluorophosphate (IL) liquid, in the voltage range of 0-1.5V cyclic voltammetry, scan 100 cycles at a speed of 0.05mV / s, and then take out The prepared SPME head was rinsed with ethanol and deionized water to remove impurities on the surface, and dried for later use. Afterwards, the extraction head was bonded to the handle of the self-made injector in this experiment with a mixed resin of epoxy resin and polyamide resin at a ratio of 1:1, and dried in the air. Headspace solid phase micr...

Embodiment 3

[0048] Embodiment 3: Preparation of solid phase microextraction head (PPY-IL-N-MWCNT)

[0049] Such as figure 1 As shown, the platinum wire as the counter electrode, the saturated calomel electrode as the reference electrode and the stainless steel wire as the working electrode were assembled into a three-electrode electrochemical working system. In the mixed solution of mL carbon nanotube (N-MWCNT) and 2.0mg / mL 1-butyl-3-methylimidazolium hexafluorophosphate (IL) liquid, in the voltage range of 0-1.5V cyclic voltammetry, with Scan at a speed of 0.05mV / s for 100 cycles, then take out the prepared SPME head, rinse with ethanol and deionized water to remove surface impurities, and dry it for later use. Afterwards, the extraction head was bonded to the handle of the self-made sample injector in this experiment with a mixed resin of epoxy resin and polyamide resin at a ratio of 1:1, dried in the air, and the extraction head containing (PPY+IL+N- MWCNT) manual headspace solid-pha...

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Abstract

The invention discloses a solid phase microextraction head and a preparation method thereof. A polypyrrole-ionic liquid-nitrogen doped multi-walled carbon nanotube extraction head is prepared by cyclic voltammetry by taking pyrrole as a functional monomer, and ionic liquid and nitrogen doped multi-walled carbon nanotubes as dopants. By combining the extraction with gas chromatography-mass spectrometry, an analytical method for the analysis and detection of methyl parathion, malathion and fenitrothion in food is established. Due to the large adsorption capacity and stability of IL and N-MWCNT,the sensitivity of the analysis method is improved and the analysis of the methyl parathion, malathion and fenitrothion in the food is further expanded. In addition, the PPY-IL-N-MWCNT extraction headcan also be used to detect other volatile pesticide residues.

Description

technical field [0001] The present application relates to the technical field of food analysis and detection, in particular to a solid-phase microextraction head used in the detection of food organic phosphorus and its preparation method and application. Background technique [0002] In recent years, due to the illegal use of chemical fertilizers, pesticides, and veterinary drugs, food safety incidents such as red duck eggs, bleached vermicelli, clenbuterol, and melamine have been banned repeatedly, which is extremely harmful to human health. The frequent occurrence of these incidents is due to the incompleteness and incompleteness of relevant laws and regulations on the one hand; on the other hand, the limitation of food-related inspection and testing methods and the single detection object. Traditional food testing methods have complex sample pretreatment process, cumbersome operation, organic reagent contamination, high cost support and high requirements for practitioners...

Claims

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Application Information

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IPC IPC(8): B01J20/282B01J20/28B01D15/08G01N30/06B01J20/30
CPCB01J20/282B01J20/28023B01D15/08G01N30/06G01N2030/062
Inventor 杨光明曾斯丽陈昕娜廖文椿韦堂娟杨红萍
Owner HONGHE COLLEGE
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