Solid-phase microextraction head for enriching perfluorinated compounds and preparation method thereof

A solid-phase micro-extraction head and perfluorinated compound technology, applied in the field of food analysis, can solve the problems of lack of special extraction head for perfluorinated compounds, etc., and achieve the effects of high mechanical strength, solving difficult enrichment, and enhancing stability and firmness

Active Publication Date: 2021-12-14
GUANGZHOU QUALITY SUPERVISION & TESTING INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Based on this, it is necessary to address the problem that most of the solid-phase microextraction heads on the market are broad-spectrum and lack a special extraction head for efficiently enriching perfluorinated compounds in food, and provide a method for enriching perfluorinated compounds. Solid phase microextraction head

Method used

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  • Solid-phase microextraction head for enriching perfluorinated compounds and preparation method thereof
  • Solid-phase microextraction head for enriching perfluorinated compounds and preparation method thereof
  • Solid-phase microextraction head for enriching perfluorinated compounds and preparation method thereof

Examples

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Effect test

Embodiment 1

[0031] A solid-phase microextraction head for enriching perfluorinated compounds, the preparation method of which is as follows:

[0032] 1) Take an iron wire with a diameter of 0.3mm, roughen its surface with fine sandpaper, and place it with a permanent magnet for several days until it becomes magnetic, then use 0.1M sodium hydroxide, 0.1M hydrochloric acid, methanol , acetone and ultrapure water for 10 minutes to remove surface oxides and impurities, and then dry in a vacuum oven.

[0033] 2) Preparation of fluorinated graphene (F-G):

[0034] Weigh 100 mg of graphene oxide into a 200 mL beaker, add 100 mL of ultrapure water, and sonicate for 30 minutes to obtain a uniform graphene oxide dispersion. Add the dispersion into a polytetrafluoroethylene-lined hydrothermal kettle, and add 60mL of hydrofluoric acid, tighten the hydrothermal kettle to make it airtight, then place it in an oven and keep it warm at 180°C 24h. After the reaction was completed, it was allowed to coo...

Embodiment 2

[0040] The metal carrier used in the experiment of this example is nickel wire, the diameter of which is 0.4mm. The surface of the nickel wire is polished with fine sandpaper to roughen it, and then it is placed together with a permanent magnet for several days until it becomes magnetic. Wash with ultrapure water for 10 minutes to remove surface impurities. The cleaned magnetized nickel wire was vertically immersed in the dispersion for 5 minutes, then lifted vertically at a constant speed, and the pulling process was repeated until the coating thickness reached about 20 μm. The metal wire was subjected to aging treatment at 150°C for 1 h in a high-purity nitrogen atmosphere.

[0041] Other steps and preparation conditions are all identical with embodiment 1.

Embodiment 3

[0043]The iron wire of the metal carrier in the experiment of this embodiment, the diameter of the iron wire is 0.2mm, and its surface is roughened with fine sandpaper, and then placed together with a permanent magnet for several days until it is magnetic, and then washed with 0.1M sodium hydroxide , 0.1M hydrochloric acid, methanol, acetone and ultra-pure water for 10 minutes to remove surface oxides and impurities, immerse the cleaned magnetized iron wire vertically in the dispersion for 5 minutes, then lift it vertically at a constant speed, and repeat the pulling process until The coating thickness reaches about 100 μm. The metal wire was subjected to aging treatment at 200°C for 1.5h in a high-purity nitrogen atmosphere.

[0044] Other steps and preparation conditions are all identical with embodiment 1.

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Abstract

The invention relates to a solid-phase microextraction head for enriching perfluorinated compounds, which is composed of a metal carrier and a coating material coated on the surface of the metal carrier, and the coating material is ferromagnetic fluorinated graphene. The invention uses ferromagnetic fluorinated graphene as the adsorption coating, which can effectively enrich perfluorinated compounds, has good thermal stability, and is very stable in organic solvents, and solves the problem that most of the solid-phase microextraction heads on the market are broad-spectrum However, there is a lack of dedicated extraction heads for the efficient enrichment of perfluorinated compounds in food. In addition, the present invention uses magnetized metal wire as the metal carrier, which has high mechanical strength and is not easy to break. The coating is fixed on the metal carrier by magnetic force, which greatly enhances the stability and firmness of the extraction coating.

Description

technical field [0001] The invention relates to the technical field of food analysis, in particular to a solid-phase microextraction head for enriching perfluorinated compounds and a preparation method thereof. Background technique [0002] Solid phase microextraction (Solid Phase Microextraction, SPME) is a kind of sample pretreatment technology that integrates sampling, enrichment and sample injection, invented in the early 1990s. This technology uniformly coats a small amount of extraction phase on the On the surface of the fiber carrier, the analyte enriched on the coating is quickly desorbed to the analytical instrument (such as gas chromatography, liquid chromatography) through thermal desorption or solvent elution for analysis and determination, which greatly simplifies the conventional pretreatment The operation process is simple, easy to carry, and low in cost. It can be used in conjunction with gas chromatography, high performance liquid chromatography, electrophor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/32B01D15/20
CPCB01D15/20B01J20/286B01J20/324
Inventor 梁明陈立伟王莉王斌陈杰锋侯向昶吴玉銮郭新东冼燕萍
Owner GUANGZHOU QUALITY SUPERVISION & TESTING INST
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