Preparation and application of SiO2-coated Uio-66 solid-phase extraction column

A solid phase extraction column, sio2-nh2 technology, applied in other chemical processes, material separation, instruments, etc., can solve the problems of low content and complex matrix, achieve high adsorption efficiency, large specific surface area, and overcome the effect of matrix effect

Active Publication Date: 2022-01-18
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its content in seawater is extremely low and the matrix is ​​complex, so it is still challenging to detect trace amounts of BTX

Method used

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  • Preparation and application of SiO2-coated Uio-66 solid-phase extraction column
  • Preparation and application of SiO2-coated Uio-66 solid-phase extraction column
  • Preparation and application of SiO2-coated Uio-66 solid-phase extraction column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A SiO 2 The preparation method of @Uio-66 solid-phase extraction column, it comprises the following steps:

[0037] 1) Solid phase extraction column packing SiO 2 Preparation of @Uio-66:

[0038] (a) SiO 2 Etching: to remove SiO 2 Capped alkyl, etched 1.50 g SiO with 10.0 mL 10wt% HF 2 , and the etching time was 1 min. Use a vortex machine to vortex during etching to avoid uneven etching. The resulting product was washed with methanol and centrifuged three times (250 rpm, 1 min), and the obtained solid was dried at 60 °C for 12 h to obtain etched SiO 2 .

[0039] (b) SiO 2 -NH 2 Preparation method: 0.50 g of 25 μm SiO 2Dissolve in 50.0 mL of ethanol, add 2.0 mL of 3-aminopropyltriethoxysilane under mechanical stirring, heat the solution to 80°C, and keep stirring for 6 h. The resulting product was washed with ethanol and centrifuged three times (250 rpm, 1 min), and the resulting solid was dried at 60 °C for 12 h to obtain SiO 2 -NH 2 , for SiO 2 Preparati...

Embodiment 2

[0048] 1) Solid phase extraction column packing SiO 2 Preparation of @Uio-66 (same as Example 1)

[0049] 2) Preparation of solid phase extraction column

[0050] (a) Take a 6.0 mL empty solid phase extraction column, put the sieve plate into the bottom first, install it in the solid phase extraction device, turn on the vacuum pump, and adjust the pressure of the device to 0.08 MPa.

[0051] (b) Weighing SiO 2 @Uio-66 The material is 0.20 g, pour the material into the empty solid phase extraction column, open the pressure valve, make the material flat and compact under pressure, and finally put it into the sieve plate, and continue to compact the material. can be obtained as SiO 2 @Uio-66 is a 6.0 mL solid-phase extraction column filled with filler.

[0052] 3) SiO2 2 @Uio-66 solid phase extraction column is used for the detection of BTX. The enrichment efficiency of the solid phase extraction column was 68.6%. The detection limit of this method is 10.0 ng L -1 .

Embodiment 3

[0054] 1) Solid phase extraction column packing SiO 2 Preparation of @Uio-66 (same as Example 1)

[0055] 2) Preparation of solid phase extraction column

[0056] (a) Take a 10.0 mL empty solid phase extraction column, put the sieve plate into the bottom first, install it in the solid phase extraction device, turn on the vacuum pump, and adjust the pressure of the device to 0.08 MPa.

[0057] (b) Weighing SiO 2 @Uio-66 The material is 0.40 g, pour the material into the empty solid phase extraction column, open the pressure valve, make the material flat and compact under pressure, and finally put it into the sieve plate, and continue to compact the material. can be obtained as SiO 2 @Uio-66 is a 10.0 mL solid-phase extraction column with packing material.

[0058] 3) SiO2 2 @Uio-66 solid phase extraction column is used for the detection of BTX. The enrichment efficiency of the solid phase extraction column was 58.5%. The detection limit of this method is 10.0 ng L -1 . ...

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Abstract

The invention belongs to the technical field of preparation of a modified Uio-66 material, and particularly relates to a preparation method of a solid-phase extraction column taking a metal organic framework coated silicon ball as a filler, and an application of the solid-phase extraction column in enrichment of short nude dinoflatoxin BTX in seawater. SiO2-coated Uio-66 has a micro-mesoporous structure, has an electrostatic adsorption effect, a hydrogen bond effect and a good steric hindrance effect with BTX, has a good compatibility between the aperture size and BTX, and has good water stability and acid and alkali resistance. The solid-phase extraction column with SiO2 and Uio-66 as the filler is used for effectively enriching BTX in seawater and is combined with high performance liquid chromatography-tandem triple quadrupole mass spectrometry (HPLC-MS / MS) to establish a method for detecting BTX in seawater, which has the advantages of high sensitivity, good reproducibility, high accuracy and the like. The method has a good application prospect in the aspects of ocean red tide early warning and ocean environment monitoring.

Description

technical field [0001] The invention belongs to the technical field of preparing modified Uio-66 materials, in particular to metal-organic framework SiO 2 @Uio-66 is the preparation of a solid-phase extraction column with fillers, and the enrichment method of brevetoxin in seawater by the solid-phase extraction column. Background technique [0002] Brevetoxin (BTX) is a red tide algae toxin mainly produced by dinoflagellates. BTX is a polyether fat-soluble algae toxin, which is a kind of neurological shellfish toxin. After human exposure, it will cause symptoms of digestive system and nervous system; skin contact with seawater containing brevetoxin can cause itching on the skin and mucous membranes and water scars; and this toxin can cause respiratory failure or ventricular fibrillation, so it is potentially fatal to humans. It enters the human body mainly when humans ingest BTX-containing seafood during red tides; at the same time, the aerosol formed along the coast conta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/283B01J20/30G01N30/02G01N30/08G01N30/72
CPCB01J20/103B01J20/226B01J20/283G01N30/02G01N30/08G01N30/72
Inventor 张兰刘泳君陈晖丁青青张文敏
Owner FUZHOU UNIV
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