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Covalent organic framework compound solid phase micro-extraction fiber head and preparation method thereof

A technology of covalent organic framework and fiber extraction, which is applied in the field of analytical chemistry and food safety testing, can solve the problems of sample cross-contamination, retention, waiting for development, etc., achieve good thermal stability and solvent stability, and lower detection limit Effect

Active Publication Date: 2018-09-18
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Given the ubiquity of PAEs in the environment, these methods use a large number of solvents and containers, making samples prone to cross-contamination
Moreover, due to the complex matrix of plant samples and the complicated pretreatment process, it is easier to reduce the reliability of the results
The use of solid-phase microextraction to detect environmental pollutants such as phthalates mostly stays in simple aqueous matrices, and SPME for complex matrices such as fruits and vegetables still needs to be developed.

Method used

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  • Covalent organic framework compound solid phase micro-extraction fiber head and preparation method thereof
  • Covalent organic framework compound solid phase micro-extraction fiber head and preparation method thereof
  • Covalent organic framework compound solid phase micro-extraction fiber head and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Example 1: Preparation of solid phase microextraction fiber and solid phase microextraction device with titanium wire as the base and COF coating

[0052] (1) Pretreatment of metal fiber substrate

[0053] A titanium wire with a diameter of 0.25mm and a purity of 99.7% was used as the substrate of the solid-phase microextraction fiber, which was ultrasonically treated with purified water and ethanol for 10 minutes, and dried for later use.

[0054] (2) Electrochemical anodization is performed on titanium wires using an electrochemical workstation to form titanium dioxide nanotube arrays on the titanium wires

[0055] Prepare a 0.5wt% ammonium fluoride-ethylene glycol solution containing 3% water in a small clean plastic beaker, use a platinum electrode as a counter electrode, and insert a pretreated titanium wire into the solution as a working electrode at a depth of 3 cm. The spacing is 3.5cm. The current-time curve mode was selected, and different oxidation times (1...

Embodiment 2

[0064] Example 2: Extraction and detection of 15 PAEs in water samples using COF (COF-TpBD, COF-TpPa-1) coated solid-phase microextraction fibers

[0065] (1) Standard solution preparation: PAEs-methanol mixed standard solution with a concentration of 1000mg / mL, including dimethyl phthalate (DMP), diethyl phthalate (DEP), diisobutyl phthalate ester (DIBP), di-n-butyl phthalate (DBP), bis(2-methoxy)ethyl phthalate (DMEP), bis(4-methyl-2-pentyl phthalate) ) ester (BMPP), bis(2-ethoxy)ethyl phthalate (DEEP), dipentyl phthalate (DPP), dihexyl phthalate (DHXP), phthalic acid Butylbenzyl ester (BBP), bis(2-butoxy)ethyl phthalate (DBEP), dicyclohexyl phthalate (DCHP), bis(2-ethyl) phthalate Hexyl ester (DEHP), diphenyl phthalate (DphP), and di-n-octyl phthalate (DNOP) were serially diluted to 100 mg / mL and 10 mg / mL, and used as stock solution and intermediate solution, respectively. The concentration of the working solution for the standard curve is 5 μg / mL, 10 μg / mL, 20 μg / mL, 50 ...

Embodiment 3

[0079] Example 3: Extraction and detection of 11 kinds of PAEs in vegetables using COF (COF-TpBD) coated solid-phase microextraction fiber

[0080](1) Standard solution preparation: PAEs-methanol standard solution with a concentration of 1000mg / mL, including DMP / DEP / DIBP / DBP / DMEP / BMPP / DEEP / DPP / DHXP / BBP / DBEP / DCHP / DEHP / DphP / DNOP gradient Dilute to 100mg / mL, 10mg / mL, respectively as stock solution and intermediate solution. The concentration of the working solution for the standard curve is 5 μg / mL, 10 μg / mL, 20 μg / mL, 50 μg / mL, 100 μg / mL, 200 μg / mL, 500 μg / mL, 1000 μg / mL, ready for use.

[0081] (2) Pretreatment of samples to be tested

[0082] After 3 g of vegetables were fully crushed, 20 μL of 5 ppm standard working solution was added and mixed evenly, and a certain proportion of water was added to be fully ultrasonicated, oscillated, and directly put into the sample bottle of the SPME device prepared in Example 1.

[0083] (3) The specific steps of headspace extraction are...

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Abstract

The invention discloses a covalent organic framework compound solid phase micro-extraction fiber head and a preparation method thereof, and belongs to the technical fields of analytical chemistry andfood safety detection. A solid phase micro-extraction fiber made from a covalent organic skeleton compound is prepared, and is used to prepare the solid phase micro-extraction fiber head, and the fiber head is used for solid phase micro-extraction. The solid phase micro-extraction fiber having a covalent organic framework (COF) material coating on the surface has the characteristics of large specific surface area, porosity, large pi-pi conjugate system and large thermal stability, so the COF material has a remarkable enriching effect on aromatic compounds. The fiber head can be applied to headspace solid phase micro-extraction of volatile target substances from extraction solutions with complex matrix and direct extraction of extraction solutions with a clean matrix, and also can be applied to detection after being combined with a gas chromatograph or a gas chromatograph / mass spectrometer.

Description

technical field [0001] The invention relates to a solid-phase microextraction fiber head of a covalent organic skeleton compound and a preparation method thereof, belonging to the technical fields of analytical chemistry and food safety detection. Background technique [0002] Solid phase microextraction (SPME) is a solvent-free, simple and effective sample pretreatment technology integrating sampling, extraction, enrichment and sample injection. SPME has the advantages of solvent-free enrichment, simple operation, and easy connection with detection instruments. It has been widely used in the enrichment of various samples, such as environmental, food, drug, biological, judicial and clinical samples. The SPME technique is based on the adsorption equilibrium between the analyte and the sorbent coating on the fiber surface. Therefore, the properties of the fiber surface coating play a crucial role in the SPME process. Today, commercialized extraction fibers for SPME include p...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01D15/22G01N30/08
CPCB01D15/22B01J20/281G01N30/08G01N2030/062G01N2030/065
Inventor 庞月红岳琪杨成沈晓芳严秀平
Owner JIANGNAN UNIV
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