Solid phase microextraction coating of hydroxyl cucurbituril as well as preparation method and application thereof

A hydroxyl cucurbit ring and coating technology is applied in the field of analytical chemistry to achieve the effects of diverse extraction structures, good stability and flexible extraction methods.

Inactive Publication Date: 2013-06-19
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to chemically bond a new coating on the solid phase microextraction fiber and solid phase microextraction stirring bar carrier, that is, the solid phase microe

Method used

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  • Solid phase microextraction coating of hydroxyl cucurbituril as well as preparation method and application thereof
  • Solid phase microextraction coating of hydroxyl cucurbituril as well as preparation method and application thereof
  • Solid phase microextraction coating of hydroxyl cucurbituril as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 Preparation of High Purity Fully Substituted Hydroxycutrul Rings

[0032] The present invention mainly adopts two kinds of hydroxyl cucurbit rings (decahydroxyl five-membered cucurbit rings, twelve-hydroxyl six-member cucurbit rings) to be chemically bonded on the sol-gel network to prepare the coating. The common melon ring five-membered melon ring or six-membered melon ring is used as the starting material, which is oxidized to a fully substituted hydroxy melon ring by potassium persulfate, and is separated and purified by Dowex strong acid cation exchange resin. Dissolve the synthesized crude hydroxycutrul ring in 100 mL of 20% acetic acid solution containing 0.03 mol / L hydrochloric acid, load the sample on a Dowex column pre-rinsed with 20% acetic acid solution, wash with gradient, and collect a bottle of elution for every 250 mL liquid. The first 20 bottles were rinsed with 20% acetic acid solution containing 0.03mol / L hydrochloric acid, then the 20 b...

Embodiment 2

[0033] Example 2 Preparation of Fully Substituted Hydroxycucurene Sol-Gel Solid-Phase Microextraction Coatings

[0034] Take a 10 mL polyvinyl chloride centrifuge tube and add hydroxyl cucurbitan (HO) 2n Q [n] (n=5,6) 20mg, dichloromethane (CH 2 Cl 2 ) 700 μL, hydroxyl-terminated polydimethylsiloxane (OH-PDMS) 150 μL, hydrogen-containing silicone oil (PMHS) 30 μL, tetraethyl silicate (TEOS) 250 μL, γ-glycidyl etheroxypropyl trimethoxy Then add 600 μL of 95% trifluoroacetic acid (TFA), shake for 3 min, and centrifuge at 12000 r / min for 5 min. Take the supernatant as a sol-gel coating.

Embodiment 3

[0035] Example 3 Preparation of Fibers for Solid Phase Microextraction

[0036] Pretreatment of quartz fiber: Take a quartz fiber with a length of 10 cm and a diameter of 20 μm, of which 1 cm is used as an adhesive sol-gel coating. After soaking in acetone for 3 hours and drying, place in 1 mol / L NaOH solution for 1 hour to carry out hydroxylation treatment on the quartz surface, and then put it in 0.1 mol / L HCl solution for 30 minutes to neutralize the residual NaOH on the surface, distilled water Wash and dry under nitrogen protection.

[0037] After the treated quartz fiber was inserted into the sol-gel coating solution for 30 min, it was pulled vertically, and the coating thickness was controlled by dipping times. Put the coated quartz fiber at room temperature for 24 h.

[0038] Remove the jacket of the 5 μL micro-sampler needle, cut off 2 cm from the front end, and assemble it with the inner core of the 1 μL micro-sampler. And glue the finished quartz fiber to the ...

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Abstract

The invention discloses a solid phase microextraction coating of a hydroxyl cucurbituril as well as a preparation method and an application thereof, relates to an analyzing sample pre-treatment technology, and belongs to the technical field of analytical chemistry. The solid phase microextraction coating is characterized in that a common pentabasic cucurbituril or six-membered cucurbituril is subjected to potassium peroxodisulfate oxidation and cation exchange resin separation and purification so as to obtain the hydroxyl cucurbituril through, the hydroxyl cucurbituril is bonded on a sol-gel mesh through a chemical reaction so as to obtain the solid phase microextraction coating, the coating is utilized to prepare a solid phase microextraction fibre which is combined with a gas chromatography, the environmental water sample containing polycyclic aromatic hydrocarbon is analysed, and the coating is utilized to prepare a solid phase microextraction stirring rod which is combined with a high performance liquid chromatography so as to analyze non-steroid antiinflammatory drugs. The solid phase microextraction coating provided by the invention has the advantages that the superficial area of the coating is large, and the extraction capacity is large; and the solid phase microextraction coating is a novel solid phase microextraction coating, is used for analyzing, high in selectivity, low in detection limitation, wide in linearity range, and good in selectivity.

Description

technical field [0001] The solid-phase microextraction technique is a novel analysis sample pretreatment technique, which belongs to the technical field of analytical chemistry, and specifically relates to a solid-phase microextraction coating of a hydroxyl cucurbitan ring and its preparation method and application. Background technique [0002] Solid phase microextraction (solid phase microextraction, SPME) technology is a novel sample pretreatment technology. The technology was first proposed by Professor Pawliszyn of the University of Waterloo in Canada in 1989, and was commercialized by Supelco in the United States in 1993. SPME integrates sampling, extraction, concentration, and sample injection. It has the advantages of simplicity, speed, portability, high efficiency, no need for organic solvents, and easy connection with gas chromatography, high performance liquid chromatography, gas chromatography, capillary electrophoresis and other analytical instruments. Therefor...

Claims

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Application Information

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IPC IPC(8): B01J20/282B01J20/32B01D15/08B01D15/20G01N30/06
Inventor 董南刘康张丽君
Owner GUIZHOU UNIV
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