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Extracting head for solid phase micro extraction of dextrin derivative and its making process

A technology of cyclodextrin and derivatives, which is applied in the field of analytical chemistry and polymer chemistry, and can solve problems such as short service life, low operating temperature, and poor anti-solvent washing ability

Inactive Publication Date: 2006-05-17
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the types of coatings for commercial solid-phase microextraction tips are limited, which is difficult to meet the needs, and most of the commercial extraction tips are prepared by physical coating and partial cross-linking, which is difficult to avoid low operating temperature and poor solvent resistance. Weaknesses such as short lifespan

Method used

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  • Extracting head for solid phase micro extraction of dextrin derivative and its making process
  • Extracting head for solid phase micro extraction of dextrin derivative and its making process
  • Extracting head for solid phase micro extraction of dextrin derivative and its making process

Examples

Experimental program
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Effect test

Embodiment 1

[0014] Take 30 mg of 2,6-di-O-methyl-β-cyclodextrin, dilute with 150 μL of dichloromethane, add 90 mg of hydroxyl silicone oil (molecular weight 4000), add 100 μL of tetraethoxysilane (or methyltrimethoxysilane ), add 50 μL of 3-(2,3-propylene oxide) propyl trimethoxysilane, add 75 μL of trifluoroacetic acid containing 8% water (volume ratio), then add 5 mg of hydrogen-containing silicone oil (molecular weight is 2000), and ultrasonically vibrate 5 minutes, centrifuge at 8000r / min for 8 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 solution for about 40 minutes, and repeat the operation several times to obtain a certain thickness of the coating. After taking it out, place it in a desiccator for 18 hours. 2 Aged at 300°C for 2 hours under protection to obtain the desired solid-phase microextraction tip.

Embodiment 2

[0016] Take 60mg of 2,6-di-O-methyl-β-cyclodextrin, dilute with 220μL of dichloromethane, add 100mg of hydroxyl silicone oil (molecular weight: 5000), add 150μL of tetraethoxysilane (or methyltrimethoxysilane ), add 60 μL of 3-(2,3-propylene oxide) propyltrimethoxysilane, add 100 μL of trifluoroacetic acid containing 5% (volume ratio) of water, then add 10 mg of hydrogen-containing silicone oil (molecular weight is 3000), and ultrasonically vibrate 8 minutes, centrifuge at 16000r / min for 5 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 for about 60 minutes, and repeat the operation several times to obtain a certain thickness of the coating. After taking it out, place it in a desiccator for 24 hours. 2 Aged at 250° C. for 3 h under protection to obtain the desired solid-phase microextraction tip.

[0017] The beneficial effects obtained by adopting the technical s...

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Abstract

The extracting head for solid phase micro extraction of cyclodextrin derivative includes quartz fiber and its coating and the coating is composite coating of 2, 6-di-oxy-methyl-beta-cyclodextrin and hydroxyl silicon oil bonded to the surface of the quartz fiber. The preparation process of the extracting head includes the following steps: diluting 2, 6-di-oxy-methyl-beta-cyclodextrin with dichloromethane, adding hydroxyl silicon oil, tetraethoxy silane, 3-(2, 3-epoxy propane) propyl trimethoxy silane and water containing trifluoro acetic acid, adding hydrogen-containing silicon oil, ultrasonic vibration and centrifuging, and taking supernatant; inserting one end of the quartz fiber after eliminating protecting layer and drying into the sol liquid, taking out, drying and ageing under the protection of nitrogen to obtain the extracting head. The present invention has high heat stability, high solvent flush resistance, long service life, high in Benzedrine medicine capacity and excellent application foreground in medicine analysis, including stimulant detection.

Description

technical field [0001] The invention relates to a cyclodextrin derivative solid-phase microextraction extraction head and a preparation method thereof, that is, a composite coating solid-phase microextraction extraction of 2,6-di-O-methyl-β-cyclodextrin and hydroxyl silicone oil A head and a preparation method thereof belong to the field of polymer chemistry and also belong to the field of analytical chemistry. Background technique [0002] Solid-phase microextraction is a simple, rapid, sensitive, and solvent-free sample pretreatment method that integrates sampling, concentration, and injection. Its initial application is concentrated in the fields of environment, food, and spice analysis. It is increasingly used in the analysis of pharmaceutical samples. The analysis of micro and trace drug samples in complex biological matrices (for example, the detection of stimulant drugs in human body fluids) puts forward higher requirements for the selectivity and sensitivity of soli...

Claims

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Application Information

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IPC IPC(8): B01D11/00
Inventor 曾昭睿周晶晶
Owner WUHAN UNIV
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