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Solid-phase micro-extraction fiber and preparation method thereof

A technology for extracting fibers and capillaries, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of poor stability and non-universality of solid-phase microextraction materials, and achieve easy control, reduced production costs, and uniform pores Effect

Inactive Publication Date: 2014-11-26
FOOD INSPECTION CENT OF CIQ SHENZHEN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the above-mentioned deficiencies of the prior art, to provide a solid-phase microextraction fiber and its preparation method, to solve the technical problems of poor stability and no universal applicability in the existing solid-phase microextraction materials

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  • Solid-phase micro-extraction fiber and preparation method thereof
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  • Solid-phase micro-extraction fiber and preparation method thereof

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preparation example Construction

[0018] The embodiment of the present invention provides a method for preparing solid-phase microextraction fibers. The method comprises the steps of:

[0019] S01. Prepare a mixed organic solution containing α-methacrylic acid, styrene, organic crosslinking agent, organic porogen, and azo initiator: mix α-methacrylic acid, styrene, organic crosslinking agent, and organic porogen , the azo initiator is mixed and processed to obtain a mixed organic solution;

[0020] S02: After placing the mixed organic solution in an oxygen-free environment, inject a capillary into the mixed organic solution prepared in step S01, and fill the mixed organic solution into the cavity of the capillary;

[0021] S03: Continue to heat the mixed organic solution with the capillary to 50-70°C in an oxygen-free environment to carry out the polymerization reaction, wash and remove the capillary after the polymerization reaction to obtain a solid Phase microextraction fibers.

[0022] Specifically, in ...

Embodiment 1

[0046] A solid-phase microextraction fiber and a preparation method thereof. The preparation method of this solid-phase microextraction fiber comprises the steps:

[0047] S11: Accurately measure 672 μL of α-methacrylic acid, 168 μL of styrene, 2016 μL of ethylene glycol dimethacrylate, 1008 μL of toluene, and 45.6 mg of azobisisobutyronitrile;

[0048] S12: ultrasonically vibrate each component measured in step S11 for 15 minutes at room temperature, so that each component is uniformly mixed and dissolved;

[0049] S13: Transfer the mixed solution prepared in step S12 to a watch glass, and seal it with plastic wrap (only one small hole is left), and blow nitrogen for 5 minutes;

[0050] S14: The specification is 50μL (specification: length: 125mm, outer diameter / internal warp) into the watch glass, so that the capillary is filled with the mixed solution, and continue to blow nitrogen for 2min;

[0051] S15: completely seal the watch glass with plastic wrap, and polymeri...

Embodiment 2

[0056] A solid-phase microextraction fiber and a preparation method thereof. The preparation method of the solid phase microextraction fiber is as follows: figure 1 As shown, it includes the following steps:

[0057] S21: Accurately measure 504 μL of α-methacrylic acid, 168 μL of styrene, 1008 μL of trimethylpropane trimethacrylate, 2016 μL of dimethyl phthalate, and 34.95 mg of azobisisoheptanonitrile;

[0058] S22: ultrasonically vibrate each component measured in step S21 for 20 minutes at room temperature, so that each component is uniformly mixed and dissolved;

[0059] S23: Transfer the mixed solution prepared in step S22 to a watch glass, seal it with a plastic wrap (leaving only one small hole), and blow nitrogen for 8 minutes;

[0060] S24: The specification is 25μL (specification: length: 125mm, outer diameter / Nei Jing) capillary into a watch glass, so that the capillary is filled with the mixed solution, continue blowing nitrogen for 10min;

[0061] S25: compl...

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Abstract

The invention discloses a solid-phase micro-extraction fiber and a preparation method thereof. The preparation method comprises the steps of mixing alpha-methacrylic acid, styrene, an organic crosslinking agent, an organic pore-foaming agent and an azo initiator to obtain a mixed organic liquid; putting the mixed organic liquid in an oxygen-free environment, putting a capillary tube into the mixed organic liquid, and enabling the interior of a cavity of the capillary tube to be filled with the mixed organic liquid; in the oxygen-free environment, heating the mixed organic liquid put into the capillary tube up to 50-70 DEG C, and carrying out polymerization reaction; and after the polymerization reaction is finished, washing the capillary tube, and removing the capillary tube to obtain the solid-phase micro-extraction fiber. The preparation method of the solid-phase micro-extraction fiber is stable in polymerization reaction, free from a by-product of the reaction and easy in reaction control; the solid-phase micro-extraction fiber prepared by adopting the method is good in performance stability and has the universality.

Description

technical field [0001] The invention belongs to the technical field of polymer fibers and purification, in particular to a solid-phase microextraction fiber and a preparation method thereof. Background technique [0002] Traditional sample pretreatment methods mainly include liquid-liquid extraction, solid-phase extraction, liquid-solid extraction, Soxhlet extraction, ultrasonic-assisted extraction, hollow fiber-liquid phase microextraction, etc. However, these methods have certain limitations, such as The liquid-liquid extraction method takes a long time to extract, consumes a lot of organic solvents and most of them are toxic solvents; the solid phase extraction method has complicated separation and preparation operations, low recovery rate, poor reproducibility and stability. Therefore, these pretreatment techniques are increasingly unable to meet the requirements of modern separation and analysis when dealing with complex matrix samples or trace target compounds. Solid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/30
Inventor 张毅马梦梦岳振峰肖锋沈金灿林黎梁通雯肖陈贵
Owner FOOD INSPECTION CENT OF CIQ SHENZHEN
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