A solid-phase microextraction coating of hydroxycucurbitan ring and its preparation method and application

A technology of hydroxyl melon ring and coating, applied in the field of analytical chemistry, to achieve the effect of large enrichment multiple, good reproducibility and low detection limit

Inactive Publication Date: 2014-10-08
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 microextraction coating of a kind of hydroxyl cucurbit ring referred to by the present invention, to overcome the existing Deficiencies and limitations of commercial SPME fiber coatings and SPME stir bar coatings

Method used

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  • A solid-phase microextraction coating of hydroxycucurbitan ring and its preparation method and application
  • A solid-phase microextraction coating of hydroxycucurbitan ring and its preparation method and application
  • A solid-phase microextraction coating of hydroxycucurbitan ring and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 Preparation of high-purity fully substituted hydroxy cucurbit rings

[0032] The invention mainly adopts two kinds of hydroxy cucurbit rings (decahydroxy five-membered cucurbit ring, dodecahydroxy six-membered cucurbit ring) to chemically bond on the sol-gel network to prepare the coating. The common cucurbit ring five-membered or six-membered cucurbit ring is used as the starting material, and it is oxidized into a fully substituted hydroxyl cucurbit ring by potassium persulfate, and is separated and purified by Dowex strong acid type cation exchange resin. The synthesized crude hydroxy cucurbit ring was dissolved in 100 mL of a 20% acetic acid solution containing 0.03 mol / L hydrochloric acid, loaded onto a Dowex column pre-rinsed with a 20% acetic acid solution, washed with gradient, and a bottle of elution was collected every 250 mL. liquid. The first 20 bottles were rinsed with 20% acetic acid solution containing 0.03mol / L hydrochloric acid, then 20 bo...

Embodiment 2

[0033] Example 2 Preparation of Fully Substituted Hydroxycitrulline Sol-Gel SPM Coatings

[0034] Take a 10 mL polyvinyl chloride centrifuge tube and add hydroxy cucurbit (HO) in turn 2n Q [n] (n=5,6) 20mg, dichloromethane (CH 2 Cl 2 ) 700 μL, hydroxy-terminated polydimethylsiloxane (OH-PDMS) 150 μL, hydrogen-containing silicone oil (PMHS) 30 μL, tetraethyl orthosilicate (TEOS) 250 μL, γ-glycidyl ether oxypropyl trimethoxy Silane (KH-560) 250 μL was shaken and mixed, then 600 μL of 95% trifluoroacetic acid (TFA) was added, shaken for 3 min, and centrifuged at 12000 r / min for 5 min. The supernatant was taken as a sol-gel coating.

Embodiment 3

[0035] Example 3 Preparation of solid phase microextraction fibers

[0036] Pretreatment of quartz fibers: 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 h and drying, placed in 1 mol / L NaOH solution for 1 h to hydroxylate the quartz surface, and then placed in 0.1 mol / L HCl solution for 30 min to neutralize the residual NaOH on the surface, distilled water Wash and dry under nitrogen protection.

[0037] The treated quartz fibers were inserted into the sol-gel coating solution for 30 min, then pulled vertically, and the coating thickness was controlled by the number of dips. The coated quartz fibers were placed at room temperature for 24 h.

[0038] Remove the 5 μL microinjector needle cover, cut off 2 cm at the front end, and assemble it with the 1 μL microinjector inner core. And stick the prepared quartz fiber to the inner core to fix it, and then put it in the G...

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Abstract

The invention discloses a solid-phase microextraction coating of hydroxyl cucurbit rings and its preparation method and application, relates to analysis sample pretreatment technology, and belongs to the technical field of analytical chemistry. Potassium oxidation and separation and purification by cation exchange resin to obtain hydroxyl cucurbitan ring, the hydroxyl citrul ring is bonded to the sol-gel network by chemical reaction to obtain solid phase microextraction coating, and the coating is used to prepare solid phase microextraction fiber and Gas chromatography is used to analyze environmental water samples containing polycyclic aromatic hydrocarbons, and the coating is used to prepare solid phase microextraction stirring rods and high performance liquid chromatography to analyze non-steroidal anti-inflammatory drugs. The coating of the present invention Large surface area, large extraction capacity, is a new type of solid phase microextraction coating, used for analysis, high selectivity, low detection limit, wide linear range, good 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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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/282B01J20/32B01D15/08B01D15/20G01N30/06
Inventor 董南刘康张丽君
Owner GUIZHOU UNIV
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