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Manufacturing method of beta-cyclodextrin matrix solid-phase micro-extraction head

A technology of matrix solid phase and cyclodextrin, applied in chemical instruments and methods, material separation, instruments, etc., can solve the problems of narrow application range and few types of extraction heads, and achieve the effect of increasing adsorption capacity and expanding the selection range

Inactive Publication Date: 2011-04-13
TIANJIN CHUNFA BIO TECH GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention overcomes the problems in the prior art that there are few types of solid-phase microextraction coatings and the application range of the prepared extraction head is narrow, and provides a preparation of a β-cyclodextrin matrix solid-phase microextraction head (hereinafter referred to as the extraction head) The method uses β-cyclodextrin combined with polydimethylsiloxane as solid-phase microextraction coating material to prepare extraction head, and the prepared extraction head expands the selection range of the coating for the polarity of the adsorbed substance, especially It is suitable for the detection of aroma components, organic substances such as phenols in environmental water samples, and pesticide residues in fruits and vegetables

Method used

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  • Manufacturing method of beta-cyclodextrin matrix solid-phase micro-extraction head
  • Manufacturing method of beta-cyclodextrin matrix solid-phase micro-extraction head
  • Manufacturing method of beta-cyclodextrin matrix solid-phase micro-extraction head

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Embodiment 1

[0034] The preparation method of embodiment 1β-cyclodextrin matrix solid-phase microextraction extraction tip:

[0035] (1) Selection and pretreatment of quartz fibers:

[0036] Select a quartz fiber with a length of 20mm and a diameter of 0.1mm, soak it in dichloromethane solution to remove the polyamide protective layer, etch it with hydrogen fluoride for 10min, and finally wash it with deionized water until it is neutral. drying;

[0037] (2), production of solid-phase microextraction head:

[0038] Take 400 mg of hydroxyl-terminated polydimethylsiloxane, dilute it with 600 μl of dichloromethane, add 130 mg of β-cyclodextrin, 100 mg of hydrogen-containing silicone oil, 100 μl of methyltrimethoxysilane and 100 μl of trifluoroacetic acid, stir well, Prepare the sol, place the quartz fiber treated in step (1) in the sol for 30 minutes, take it out, form a gel at room temperature for 12 hours, and carry out temperature-programmed aging under the protection of nitrogen, keep a...

Embodiment 2

[0039] Example 2 The preparation method of β-cyclodextrin matrix solid-phase microextraction head:

[0040] (1) Selection and pretreatment of quartz fibers:

[0041] Select a quartz fiber with a length of 20mm and a diameter of 0.1mm, soak it in dichloromethane solution to remove the polyamide protective layer, then etch it with hydrogen fluoride for 10min, and finally rinse it with deionized water until it is neutral, and bake it under a nitrogen flow at 120°C Dry;

[0042] (2) Production of solid-phase microextraction head: Take 400 mg of hydroxyl-terminated polydimethylsiloxane, dilute it with 600 μl of dichloromethane, add 130 mg of β-cyclodextrin, 100 mg of hydrogen-containing silicone oil, and 50 μl of glycidyl oxide Propyltrimethylsilane, 50 μl of tetraethoxysilane and 100 μl of trifluoroacetic acid were fully stirred to obtain a sol, and the quartz fiber treated in step (1) was placed in the sol for 30 minutes, then taken out, and placed at room temperature The gel w...

Embodiment 3

[0043] Example 3 The preparation method of β-cyclodextrin matrix solid-phase microextraction head:

[0044](1) Selection and pretreatment of quartz fibers: select quartz fibers with a length of 20 mm and a diameter of 0.1 mm, soak them in dichloromethane solution to remove the polyamide protective layer, etch them with hydrogen fluoride for 10 minutes, and finally use deionized Rinse with water until neutral, and dry under nitrogen flow at 135°C;

[0045] (2) Production of solid-phase microextraction head: Take 400 mg of hydroxyl-terminated polydimethylsiloxane, dilute it with 600 μl of dichloromethane, add 170 mg of β-cyclodextrin, 120 mg of hydrogen-containing silicone oil, and 90 μl of methyltrimethoxy base silane and 110 μl trifluoroacetic acid, stir well to obtain a sol, place the quartz fiber treated in step (1) in the sol for 40 minutes, take it out, form a gel at room temperature for 12 hours, and carry out a temperature program under the protection of nitrogen Aging,...

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Abstract

The invention relates to a manufacturing method of a beta-cyclodextrin matrix solid-phase micro-extraction head, belonging to the trace analysis field of volatile and semi-volatile organic matter in foods, environment and biological samples. The manufacturing method comprises the following steps of: (1) selecting and pretreating quartz fiber; (2) manufacturing the solid-phase micro-extraction head: preparing a sol from a coating material containing polydimethylsiloxane and beta-cyclodextrin, placing the quartz fiber treated in the step (1) in the sol, taking out, gelling at room temperature, aging by heating and refluxing the aged gel by using dichloromethane to manufacture the solid-phase micro-extraction head. In the invention, the beta-cyclodextrin and the polydimethylsiloxane are combined and used as the solid-phase micro-extraction coating material to manufacture the extraction head, and the extraction head enlarges the selection range of a coating on the polarity of an absorbed substance and is especially applicable to the detection of organic matter such as phenols and the like in perfume compositions and environment water samples and the detection of residual pesticides in fruits and vegetables.

Description

technical field [0001] The invention belongs to the field of trace analysis of volatile and semi-volatile organic substances, in particular to a method for trace analysis of volatile and semi-volatile organic substances in food, environment, and biological samples. Specifically, the present invention relates to a β-cyclic A preparation method of a dextrin matrix solid-phase microextraction tip. Background technique [0002] Solid phase microextraction (SPME) is a novel sample pretreatment and enrichment technology that emerged in the 1990s. It was first developed and studied by the research group of Professor Pawliszyn at the University of Waterloo in Canada in 1989. Solvent-based selective extraction. [0003] Solid-phase microextraction technology can be used for the analysis of almost all kinds of volatile or semi-volatile substances in gas, liquid, biological, solid and other samples. The biggest feature of SPME is that it integrates sampling, extraction, enrichment, a...

Claims

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Application Information

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IPC IPC(8): B01J20/24B01J20/32G01N30/00
Inventor 邓莉郝学财邢海鹏盛家川
Owner TIANJIN CHUNFA BIO TECH GRP
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