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Extraction material and preparation method thereof, and device and extraction method used for solid-phase micro-extraction

An extraction device and extraction technology are applied to extraction materials and production in the field of solid-phase microextraction. Steps, improve work efficiency, easy and accurate quantitative effect

Active Publication Date: 2012-09-26
上海新拓分析仪器科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The extraction fiber head is easily damaged by operation;
[0006] (2) The extraction specific surface area of ​​the extraction fiber head is relatively low;
[0007] (3) Imported solid-phase microextraction device is expensive
[0009] (1) The extraction rate of immersion or headspace extraction is not high;
[0010] (2) The immersion extraction method is easy to wear out the fiber head, which makes the life of the fiber head short and the production cost is high
[0011] In the field of solid-phase extraction, the main components of commonly used solid-phase extraction devices include extraction columns, etc. If the device is used for solid-phase microextraction directly, although the extraction can be completed without extraction fiber heads and high-pressure equipment, each time in the extraction column About several hundred milliliters of sample solution is required. During the extraction, the sample solution remains a lot, the dead volume is large, the concentration of the analytical solution is low, and it cannot be accurately quantified. In the later stage, concentration and constant volume steps are required to complete the extraction and quantification, which is time-consuming, laborious, and troublesome to operate. Compared with micro-extraction technology, it has the disadvantages of cumbersome operation and easy introduction of human error

Method used

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  • Extraction material and preparation method thereof, and device and extraction method used for solid-phase micro-extraction
  • Extraction material and preparation method thereof, and device and extraction method used for solid-phase micro-extraction
  • Extraction material and preparation method thereof, and device and extraction method used for solid-phase micro-extraction

Examples

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Embodiment 1

[0039] A kind of extraction material, described material is the polymer that is obtained after the polymerization reaction of methacrylic acid, ethylene glycol dimethacrylate, azobisisobutyronitrile and methanol, and its prepolymer liquid composition ratio is as follows: Acrylic acid: ethylene glycol dimethacrylate is 1:1 (molar ratio); (methacrylic acid + ethylene glycol dimethacrylate): methanol is 1:5 (molar ratio); azobisisobutyl The content of nitrile is 1% (mass ratio) of the total amount of materials.

[0040] A method for making an extraction material. Methacrylic acid, ethylene glycol dimethacrylate, azobisisobutyronitrile and methanol are mixed according to the ratio to form a pre-polymerization solution, and the pre-polymerization solution is reacted after ultrasonic treatment, and then the methanol The unreacted reagent is removed by passing through the reacted pre-polymerization solution to obtain the material for extraction. Wherein the ultrasonic power is 40W, ...

Embodiment 2

[0049] A kind of extraction material, described material is the polymer that is obtained after the polymerization reaction of methacrylic acid, ethylene glycol dimethacrylate, azobisisobutyronitrile and methanol, and its prepolymer liquid composition ratio is as follows: Acrylic acid: ethylene glycol dimethacrylate is 1:8 (molar ratio); (methacrylic acid + ethylene glycol dimethacrylate): methanol is 1:40 (molar ratio); azobisisobutyl The content of nitrile is 2% (mass ratio) of the total amount of materials.

[0050] A method for making an extraction material. Methacrylic acid, ethylene glycol dimethacrylate, azobisisobutyronitrile and methanol are mixed according to the ratio to form a pre-polymerization solution, and the pre-polymerization solution is reacted after ultrasonic treatment, and then the methanol The unreacted reagent is removed by passing through the reacted pre-polymerization solution to obtain the material for extraction. The ultrasonic power is 60W, and the...

Embodiment 3

[0062] A kind of extraction material, described material is the polymer that is obtained after the polymerization reaction of methacrylic acid, ethylene glycol dimethacrylate, azobisisobutyronitrile and methanol, and its prepolymer liquid composition ratio is as follows: Acrylic acid: ethylene glycol dimethacrylate is 1:4 (molar ratio); (methacrylic acid + ethylene glycol dimethacrylate): methanol is 1:25 (molar ratio); azobisisobutyl The content of nitrile is 1.5% (mass ratio) of the total amount of materials.

[0063] A method for making an extraction material. Methacrylic acid, ethylene glycol dimethacrylate, azobisisobutyronitrile and methanol are mixed according to the ratio to form a pre-polymerization solution, and the pre-polymerization solution is reacted after ultrasonic treatment, and then the methanol The unreacted reagent is removed by passing through the reacted pre-polymerization solution to obtain the material for extraction. The ultrasonic power is 50W, and t...

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Abstract

The invention provides an extraction material in the following component proportion: that methacrylic acid: ethylene dimethacrylate is 1:1 to 1:8 (in molar ratio); that (methacrylic acid +ethylene dimethacrylate): methanol is 1:5 to 1:40 (in molar ratio); and that the content of azodiisobutyronitrile is 1% to 2% of the total amount of the material (by mass). A preparation method of the extraction material comprises that the above materials are mixed according to the component proportion to form a pre-polymerization solution; that the pre-polymerization solution is processed by ultrasonic and reacts; and that that methanol is introduced into the reacted pre-polymerization solution to remove not reacted reagent. A solid-phase micro-extraction device comprises a draw-off device, an injection device and an extraction tube, wherein two ends of the extraction tube are connected to the draw-off device and the injection device respectively, and the extraction tube is axially equipped with a through hole which is filled with the extraction material. A solid-phase micro-extraction method comprises the steps of preparation, extraction, purification, desorption, and cleaning. According to the invention, the cost is low, and the working efficiency is high.

Description

technical field [0001] The invention relates to an extraction material and a production method, and an extraction device and method, in particular to an extraction material and a production method in the field of solid-phase microextraction, and a device and method for solid-phase microextraction. Background technique [0002] Solid-phase microextraction (solid-phase microextraction, SPME) technology is a novel sample pretreatment and enrichment technology that emerged in the 1990s. It was first carried out by the research group of Professor Pawliszyn of the University of Waterloo in Canada in 1989. It is developed and researched and belongs to the non-solvent selective extraction method. Immerse the fiber head in the sample solution or the headspace gas for a period of time, and at the same time stir the solution to accelerate the speed of equilibrium between the two phases. After the balance, take out the fiber head and insert it into the gas chromatography vaporization ch...

Claims

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Application Information

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IPC IPC(8): B01J20/282B01J20/30B01D15/08
Inventor 范义锋欧阳钢锋栾天罡邹世春张和清
Owner 上海新拓分析仪器科技有限公司
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