Sol-gel ionic liquid solid phase microextraction extraction fiber and preparation method thereof

A technology of ionic liquid and extraction head, which is applied in the field of solid-phase microextraction extraction head and its preparation, can solve the problems of weak anti-solvent washing ability, limited application range, and few types of coatings, etc., and achieve high thermal and chemical stability , Expand the application range, and the effect of a wide linear range

Inactive Publication Date: 2010-12-22
HUAZHONG AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

First of all, the vast majority of commercial extraction heads are prepared by physical coating and partial cross-linking methods, with low operating temperature, weak resistance to solve...

Method used

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  • Sol-gel ionic liquid solid phase microextraction extraction fiber and preparation method thereof
  • Sol-gel ionic liquid solid phase microextraction extraction fiber and preparation method thereof
  • Sol-gel ionic liquid solid phase microextraction extraction fiber and preparation method thereof

Examples

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Embodiment 1

[0027]The method for preparing 1-allyl-3-methylimidazolium hexafluorophosphate ionic liquid solid-phase microextraction extraction head: take 10 mg of ionic liquid containing allyl active groups, dissolve it in 300 μL of dichloromethane, add 30 mg of hydroxyl silicone oil, Add 50 μL of tetraethoxysilane, add 30 μL of γ-methacryloxypropyl trimethoxysilane, add 5 μL of hydrogen-containing silicone oil, add 6 mg of benzophenone, ultrasonically oscillate for 5 minutes, and then add 60 μL of 5% (volume ratio) trifluoroacetic acid in water, continue ultrasonic oscillation for 8 minutes, centrifuge at 12000r / min for 8 minutes, take out the supernatant for later use. Insert one end of the dry quartz fiber whose protective layer has been removed into the sol clear solution, and place it for 5 hours, pull out the fiber vertically from the solution, repeat the operation several times to obtain a coating with a thickness of 65 μm, and place it in a desiccator for 24 hours after taking it...

Embodiment 2

[0029] The method for preparing 1-allyl-3-methylimidazolium hexafluorophosphate ionic liquid solid-phase microextraction head: take 30 mg of ionic liquid containing allyl active groups, dissolve it in 700 μL of dichloromethane, add 60 mg of hydroxyl silicone oil, Add 100 μL tetraethoxysilane, add 50 μL γ-methacryloxypropyltrimethoxysilane, add 8 μL hydrogen-containing silicone oil, add 7 mg benzophenone, ultrasonically oscillate for 5 minutes, and then add 70 μL containing 5% (Volume ratio) trifluoroacetic acid in water, continue ultrasonic oscillation for 7 minutes, centrifuge at 10000r / min for 7 minutes, take out the supernatant for later use. Insert one end of the dry quartz fiber whose protective layer has been removed into the sol clear solution, place it for 3.5 hours, pull out the fiber vertically from the solution, repeat the operation several times to obtain a coating with a thickness of 80 μm, and place it in a desiccator for 12 hours after taking it out , and then...

Embodiment 3

[0031] The method for preparing 1-allyl-3-methylimidazolium hexafluorophosphate ionic liquid solid-phase microextraction head: take 50 mg of ionic liquid containing allyl active groups, dissolve it in 1000 μL of dichloromethane, add 90 mg of hydroxyl silicone oil, Add 150 μL tetraethoxysilane, add 80 μL γ-methacryloxypropyltrimethoxysilane, add 15 μL hydrogen-containing silicone oil, add 8 mg benzophenone, ultrasonically oscillate for 5 minutes, and then add 80 μL containing 5% (volume ratio) trifluoroacetic acid in water, continue ultrasonic oscillation for 10 minutes, centrifuge at 16000r / min for 6 minutes, and take out the supernatant for later use. Insert one end of the dried quartz fiber whose protective layer has been removed into the sol clear solution, place it for 4 hours, pull out the fiber vertically from the solution, repeat the operation several times to obtain a coating with a thickness of 100 μm, and place it in a desiccator for 10 hours after taking it out , ...

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Abstract

The invention belongs to the technical field of chemical analysis and test instruments, relates to the fields of polymer chemistry and analytical chemistry, and relates to a sol-gel ionic liquid solid phase microextraction extraction fiber and a preparation method thereof. In the preparation method, 1-allyl-3-methylimidazolium hexafluorophosphate or 1-allyl-3-methylimidazolium bis [(trifluoromethyl)sulfonyl] imide ionic liquid is taken as a coating material; and a layer of ionic liquid and hydroxy silicone oil composite coating is chemically bonded on the surface of a quartz fiber by a method for combining the sol-gel with free radical initiated crosslinking. The sol-gel ionic liquid solid phase microextraction extraction fiber prepared by the technical scheme can be directly combined with gas chromatogram, and has the advantages of porous surface structure, high thermal stability, high solvent washing resistance, wide pH application range, high repeatability, good extraction effect on strongly polar phenol environmental estrogen, arylamine and non-polar polycyclic aromatic hydrocarbon, and good application prospects in the fields of environmental monitoring, food sanitation, inspection and quarantine, and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis testing instruments, and is related to the fields of polymer chemistry and analytical chemistry. The invention relates to a solid-phase microextraction (SPME) extraction head and a preparation method thereof. Background technique [0002] Solid-phase microextraction is a new solvent-free sample pretreatment technology developed on the basis of solid-phase extraction. Its core is a solid-phase coating coated on the surface of the extraction head. Although solid-phase microextraction technology has developed rapidly in recent years, there are still some problems that need to be solved urgently. First of all, the vast majority of commercial extraction heads are prepared by physical coating and partial cross-linking methods, which have low operating temperature, weak resistance to solvent washing, and narrow polarity range. Secondly, the existing solid-phase microextraction head has few ty...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/285B01J20/30B01D15/08
Inventor 刘名茗周欣陈颖漪冯雄汉刘凡
Owner HUAZHONG AGRI UNIV
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