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Preparation method and application of stationary phase coating material for identification of trace substances

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 formation and high melting point of cyclodextrin, and achieve the effects of low column loss rate, large adsorption capacity and simple preparation process

Inactive Publication Date: 2014-10-08
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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  • Preparation method and application of stationary phase coating material for identification of trace substances
  • Preparation method and application of stationary phase coating material for identification of trace substances
  • Preparation method and application of stationary phase coating material for identification of trace substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

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

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

[0040] Take HBP-allyl 2ml, MeHSiCl 2 4ml, THF 10ml, 3 drops of Karstedt catalyst, react at 80°C f...

Embodiment 2

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

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

[0046] The preparation method of the stationary phase coating material used for the identification of trace substances: take a Contes tube, fully dry, under the protection of nitrogen, add MeHSi(CH 2 -CH=CH 2 ) 2 5ml, 10ml of n-hexane, 3 drops of Karstedt catalyst, react at 80°C for 8 hours. The solvent was evaporated to obtain HBP-allyl. HBP-allyl 2ml, MeHSiCl 2 4ml, 10ml of n-hexane, 3 drops of chloroplatinic acid catalyst...

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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, a preparation method and application thereof. Background technique [0002] In trace analysis, due to the low content and uneven distribution of the measured elements in the sample, especially environmental samples, they often fluctuate greatly with time and space, which has caused certain difficulties for the accuracy and reliability of trace analysis. In order to enhance the detection ability of trace components and remove basic interferences, separation and enrichment of trace components are often essential. [0003] Solid-phase microextraction is a new sample preparation technology developed in recent years. It has very important environmental protection significance because it abandons the extensive use of solvents in the traditional sample preparation technology and turns...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00C08G77/60C08B37/16G01N30/02
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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