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Method for preparing stationary phase coating material for trace substance identification and application of material

A coating material and stationary phase technology, applied in the field of stationary phase materials for chromatographic detection, can solve the problems of poor film-forming property and high melting point of cyclodextrin, and achieve the effects of low column loss rate, large adsorption capacity and uniform film formation

Inactive Publication Date: 2012-08-15
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, underivatized cyclodextrin has a high melting point and poor film-forming properties, so it needs to be properly modified to lower the melting point and improve film-forming properties.

Method used

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  • Method for preparing stationary phase coating material for trace substance identification and application of material
  • Method for preparing stationary phase coating material for trace substance identification and application of material
  • Method for preparing stationary phase coating material for trace substance identification and application of material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Preparation of fully dried cyclodextrin: Add 100ml of distilled water to a 300ml beaker and heat to a slight boiling point. Weigh 5 g of β-cyclodextrin, stir and heat to dissolve, filter while hot, and the filtrate crystallizes to obtain β-cyclodextrin crystals. Filter off the water, put β-cyclodextrin into a 50ml small beaker, place it in a vacuum drying oven at 110°C-120°C for 1 hour, and store in a desiccator.

[0038] The preparation method of fully dried THF is: metal sodium is refluxed until the benzophenone indicator turns blue.

[0039] Preparation method of stationary phase coating material for identification of trace substances: Take a Contes tube, fully dry, and under nitrogen protection, add MeHSi(CH 2 -CH=CH 2 ) 2 5ml, THF 10ml, 3 drops of Karstedt catalyst, react at 80°C for 8 hours. Evaporate the solvent to obtain HBP-allyl.

[0040] Take HBP-allyl 2ml, MeHSiCl 2 4ml, THF 10ml, 3 drops of Karstedt catalyst, react at 80℃ for 8 hours; infrared monitoring allyl g...

Embodiment 2

[0044] Preparation of fully dried cyclodextrin: Add 100ml of distilled water to a 300ml beaker and heat to a slight boiling point. Weigh 5 g of β-cyclodextrin, stir and heat to dissolve, filter while hot, and the filtrate crystallizes to obtain β-cyclodextrin crystals. Filter off the water, put β-cyclodextrin into a 50ml small beaker, place it in a vacuum drying oven at 110°C-120°C for 1 hour, and store in a desiccator.

[0045] The preparation method of fully dried n-hexane is: metal sodium is refluxed until the benzophenone indicator turns blue.

[0046] Preparation method of stationary phase coating material for identification of trace substances: Take a Contes tube, fully dry, and under nitrogen protection, add MeHSi(CH 2 -CH=CH 2 ) 2 5ml, 10ml n-hexane, 3 drops of Karstedt catalyst, react at 80°C for 8 hours. Evaporate the solvent to obtain HBP-allyl. HBP-allyl 2ml, MeHSiCl 2 4ml, 10ml of n-hexane, 3 drops of chloroplatinic acid catalyst, reacted at 90℃ for 6 hours; infrared...

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Abstract

The invention relates to a method for preparing a stationary phase coating material for trace substance identification and application of the material. The method comprises the following steps of: adding carbosilane hyperbranched macromolecules with allyl terminals and MeHSiCl2 into a solvent, adding a Kastedt catalyst, and performing hydrosilylation reaction in the presence of nitrogen; adding triethylamine, fully dried cyclodextrin and fully dried tetrahydrofuran (THF) for bonding reaction; and finally cooling and separating, thus obtaining the material. The material is coated on capillary inner columns; and the material has the advantages of uniform film formation, high column efficiency and high adsorption quantity, and has analysis and identification capability for trace substances.

Description

Technical field [0001] The invention relates to a stationary phase material for chromatographic detection, in particular to a stationary phase coating material for identification of trace substances, and a preparation method and application thereof. Background technique [0002] Trace analysis Because the content of the measured element in the sample is very low and the distribution is very uneven, especially in environmental samples, it often fluctuates greatly with time and space, which causes certain difficulties for the accuracy and reliability of trace analysis. In order to enhance the ability to detect trace components and remove basic interference, the separation and enrichment of trace components is often necessary. [0003] Solid phase microextraction is a new type of sample preparation technology developed in recent years. Because it abandons the large-scale use of solvents in traditional sample preparation technology, it becomes a zero solvent sample preparation, which ...

Claims

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Application Information

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IPC IPC(8): C09D187/00C08G81/00C08G77/60C08B37/16G01N30/02
Inventor 陈国文冯圣玉张晨周传健赵士贵李文杰
Owner SHANDONG UNIV
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