Method for preparing Beta-cyclodextrin matrix stir extraction bar

A technology of cyclodextrin and extraction rods, which is applied in the field of preparation of β-cyclodextrin matrix stirring extraction rods, can solve the problems of SBSE technology application limitations, fragile materials, and high price of SBSE devices, so as to avoid competitive adsorption and increase adsorption The effect of improving ability and enrichment factor

Inactive Publication Date: 2011-05-11
TIANJIN CHUNFA BIO TECH GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Commercialized SBSE devices use glass rods as the carrier, the material is fragile, and there is only PDMS as a stationary phase coating, and the price of commercialized SBSE devices is relatively high, so the application of SBSE technology is greatly restricted

Method used

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  • Method for preparing Beta-cyclodextrin matrix stir extraction bar
  • Method for preparing Beta-cyclodextrin matrix stir extraction bar
  • Method for preparing Beta-cyclodextrin matrix stir extraction bar

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1 A kind of preparation method of β-cyclodextrin matrix stirring extraction stick:

[0038] Select a glass tube with a length of 20 mm and a diameter of 3 mm, seal a slightly shorter iron core in it with an alcohol blowtorch, and use CH on the surface of the rod in turn. 2 Cl 2 Treat for 30 minutes, 1mol / L NaOH solution for 8 hours, 0.1mol / L HCl solution for 4 hours, finally rinse with deionized water until neutral, and dry at 150°C under nitrogen flow.

[0039]Dilute 400 mg of hydroxyl-terminated polydimethylsiloxane with 600 μl of dichloromethane, add 130 mg of β-cyclodextrin, 100 mg of hydrogen-containing silicone oil, 100 μl of methyltrimethoxysilane and 100 μl of trifluoroacetic acid, stir well, and The treated rod is placed in the sol for 30 minutes and taken out, and gelled at room temperature for 12 hours; under the protection of nitrogen, carry out temperature-programmed aging at 120°C for 3 hours, at 180°C for 3 hours, and then at 240°C for 60 minu...

Embodiment 2

[0040] Example 2 A preparation method of a β-cyclodextrin matrix stirring extraction rod:

[0041] Select a glass tube with a length of 20 mm and a diameter of 3 mm, seal a slightly shorter iron core in it with an alcohol blowtorch, and use CH on the surface of the rod in turn. 2 Cl 2 Treat for 50 minutes, 1mol / L NaOH solution for 6 hours, 0.1mol / L HCl solution for 4 hours, finally rinse with deionized water until neutral, and dry at 150°C under nitrogen flow.

[0042] Dilute 400 mg of hydroxyl-terminated polydimethylsiloxane with 600 μl of dichloromethane, add 130 mg of β-cyclodextrin, 100 mg of hydrogen-containing silicone oil, 50 μl of glycidoxypropyltrimethylsilane and 50 μl of tetraethoxysilane and 100 μl trifluoroacetic acid, and stir well to obtain a sol. Put the treated rod in the sol for 30 minutes and take it out, and form a gel at room temperature for 12 hours; Keep at ℃ for 3h, then keep at 240℃ for 60min to complete the aging. After aging, place it in a Soxhlet ...

Embodiment 3

[0043] Embodiment 3 A preparation method of a β-cyclodextrin matrix stirring extraction rod:

[0044] Select a glass tube with a length of 20 mm and a diameter of 3 mm, seal a slightly shorter iron core in it with an alcohol blowtorch, and use CH on the surface of the rod in turn. 2 Cl 2 Treat for 30 minutes, 1mol / L NaOH solution for 6 hours, 0.1mol / L HCl solution for 4 hours, finally rinse with deionized water until neutral, and dry at 150°C under nitrogen flow.

[0045] Dilute 400 mg of hydroxyl-terminated polydimethylsiloxane with 600 μl of dichloromethane, add 170 mg of β-cyclodextrin, 120 mg of hydrogen-containing silicone oil, 90 μl of methyltrimethoxysilane and 110 μl of trifluoroacetic acid, stir well, and The treated rod was placed in the sol for 40 minutes and taken out, and gelled at room temperature for 12 hours; under the protection of nitrogen, it was subjected to temperature-programmed aging at 120°C for 3 hours, at 180°C for 3 hours, and then at 240°C for 30 m...

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Abstract

A method for preparing Beta-cyclodextrin matrix stir extraction bar relates to the trace analysis field of VOCs (volatile organic compounds) and semi VOCs in food, environment and biological samples. In the method, Beta-cyclodextrin is combined with PDMS (polydimethylsiloxane) to serve as the coating materials of the stir extraction bar coating, a bar body is used to serve as the matrix of the stir extraction bar coating for coating, and the bar body is made of an iron core which is shorter than the bar body and is sealed in a glass tube. As the Beta-cyclodextrin is combined with PDMS to serve as coating materials to make the stir extraction bar, the stir extraction bar enlarges the selection range of polarity of to-be-adsorbed substances selected by the coating, finishes stirring alone in the extraction process, and avoids the competitive adsorption of a stir bar in Fiber SPME (Solid-Phase Micro-Extraction). As the volume of extraction stationary phase is more than 50 times larger than that of SPME, the concentration time is obviously improved, and the stir extraction bar is particularly suitable for trace analysis.

Description

technical field [0001] The invention belongs to the field of trace analysis of volatile and semi-volatile organic substances, in particular to the field of trace analysis of volatile and semi-volatile organic substances in food, environment and biological samples, in particular a β-cyclodextrin matrix stirring Preparation method of extraction stick. Background technique [0002] Solid Phase Micro Extraction (Solid Phase Micro Extraction, SPME) is a novel sample pretreatment and enrichment technology emerging in the 1990s. It was first carried out in 1989 by the research group of Professor Pawliszyn of the University of Waterloo, Canada. It is developed and researched and belongs to the non-solvent selective extraction method. It can be used for the analysis of almost all kinds of volatile or semi-volatile substances in gas, liquid, biological, solid and other samples. The biggest feature of SPME is that it integrates sampling, extraction, enrichment, and sample injection, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/32
Inventor 邓莉郝学财邢海鹏盛家川
Owner TIANJIN CHUNFA BIO TECH GRP
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