Preparation of solid-phase microextraction (SPME) fiber and extraction device assembled by same

A technology for extracting fibers and extraction devices, applied in the field of solid-phase microextraction, to achieve the effects of overcoming poor mechanical strength, novel structure, and unique design

Inactive Publication Date: 2013-03-27
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there has been no report on the use of chemical bonds and

Method used

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  • Preparation of solid-phase microextraction (SPME) fiber and extraction device assembled by same

Examples

Experimental program
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Effect test

Embodiment 1

[0025] A preparation of solid-phase microextraction fiber coating, using covalent bond and method to prepare metal organic framework (MOFs) material ZIF-90 as the extraction fiber coating, the steps are as follows:

[0026] 1) Pretreatment of hollow quartz fiber:

[0027] Burn a hollow quartz fiber with an inner diameter of 250 μm and a length of 3 cm with an alcohol lamp to burn off the outer polyimide protective layer, put it in a sodium hydroxide solution with a concentration of 1M for activation, and expose a large amount of silicon hydroxyl groups on the surface, and then Wash with water until neutral, dry for later use;

[0028] 2) APTES functionalization of hollow silica fibers:

[0029] Put the hollow quartz fiber treated in the first step in the solution of APTES for reaction, react at room temperature for 12 hours, take it out and put it in a 120-degree oven for 30 minutes, repeat this process twice, finally wash with toluene and ethanol, and dry it for later use; ...

Embodiment 2

[0033] A preparation of solid-phase microextraction fiber coating, using covalent bond and method to prepare metal organic framework (MOFs) material ZIF-8 as the extraction fiber coating, the steps are as follows:

[0034] 1) Same as embodiment 1;

[0035] 2) Same as embodiment 1;

[0036] 3) Preparation of silica fiber surface bonds and metal-organic framework materials:

[0037] Dissolve 0.12g of zinc nitrate tetrahydrate and 0.03g of 2-methyl-imidazole in 9mL of N,N-dimethylformamide, ultrasonically dissolve for 10min, and place the mixture in a 25mL polytetrafluoroethylene reactor; the second step Put the treated quartz fiber vertically into the reaction mixture, react at 140°C for 24 hours, wait for the reactor to cool down, take out the quartz fiber with surface bonds and metal-organic framework materials, and use N,N-dimethylformamide solvent After washing, the extracted fiber of solid phase microextraction is obtained.

Embodiment 3

[0039] A preparation of solid-phase microextraction fiber coating, using covalent bond and method to prepare metal organic framework (MOFs) material ZIF-7 as the extraction fiber coating, the steps are as follows:

[0040] 1) Same as embodiment 1;

[0041] 2) Same as embodiment 1;

[0042] 3) Preparation of silica fiber surface bonds and metal-organic framework materials:

[0043] Dissolve 0.28g of zinc nitrate tetrahydrate and 0.16g of benzimidazole in 15mL of N,N-dimethylformamide, ultrasonically dissolve for 10min, and place the mixture in a 25mL polytetrafluoroethylene reactor; process the second step Put the quartz fiber vertically into the reaction mixture, react at 130°C for 48 hours, wait for the reactor to cool down, take out the quartz fiber with surface bonds and metal-organic framework materials, wash with N,N-dimethylformamide solvent, That is the extraction fiber of solid phase microextraction.

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Abstract

Disclosed is a preparation of an SPME fiber. A covalent bond method is adopted to prepare metal-organic frameworks (MOFs) as a coating for the extraction fiber. The fiber preparing method includes performing APTES amino-functionalization on a quartz fiber, namely, placing the fiber with amino on the surface into an MOF solution for reaction. An extraction device assembled by the prepared SPME coating comprises a device body, a microsyringe outer tube, a microsyringe needle, a push-pull rod and the extraction fiber with the coating, wherein the push-pull rod is arranged in the microsyringe outer tube and forms a sliding matching with the inner wall of the tube, the lower end of the push-pull rod is corroded by an aqua regia solution to obtain a corrosion end which is inserted into the extraction fiber with the coating, and a handle is arranged at the upper end of the push-pull rod. The preparation and the device have the advantages that an organic ligand of the extraction fiber coating and the MOFs is highly ordered and controllable, the extraction device has a novel structure, the coating fiber fixation is firm, and the stability and service life of the extraction fiber coating are improved.

Description

technical field [0001] The invention relates to solid-phase micro-extraction technology, in particular to the preparation of a solid-phase micro-extraction fiber and an extraction device assembled with it. Background technique [0002] Solid phase microextraction (SPME) is a solvent-free sample pretreatment technique proposed by Professor Pawliszyn of Canada in 1990. Compared with traditional techniques, solid-phase microextraction integrates sampling, extraction, enrichment and sample injection, which is simple to operate and easy to realize automation; it can be used in combination with gas chromatography, high performance liquid chromatography and other instruments to analyze samples quickly and effectively Medium trace organic matter. Therefore, SPME is widely used in various fields such as the environment, food, and biology. The core component of this technology is the extraction fiber coated with adsorbent material on the surface. The target object is extracted from ...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30G01N30/06
Inventor 严秀平于丽青杨成雄
Owner NANKAI UNIV
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