Phenyl bridge bond type fibrous porous silicon material and preparation method and application thereof

A fibrous, porous silicon technology, applied in the direction of material separation, analytical materials, chemical instruments and methods, etc., can solve problems such as residues, ecosystems and human health hazards, and achieve small amount of organic solvents, good adsorption performance, and high mechanical properties. Effect of Strength and Chemical Stability

Active Publication Date: 2018-09-25
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Sulfonamide antibiotics, as a class of broad-spectrum antibacterial drugs, are widely used in the prevention and treatment of hum

Method used

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  • Phenyl bridge bond type fibrous porous silicon material and preparation method and application thereof
  • Phenyl bridge bond type fibrous porous silicon material and preparation method and application thereof
  • Phenyl bridge bond type fibrous porous silicon material and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1. The recovery rate experiment of sulfa antibiotics in purified water

[0030] (1) Preparation of phenyl bridged fibrous porous silicon solid-phase extraction column:

[0031] Weigh 1.0 g of cetylpyridinium bromide, add 0.6 g of urea into 30 mL of water, and stir for 0.5 hour to obtain solution A. Add bis(triethoxysilyl)benzene / ethylorthosilicate and 1.5 mL amyl alcohol in a molar ratio of 1:6 to 30 mL cyclohexane and stir for 0.5 hour to obtain solution B. Add solution B to solution A, stir in a water bath at room temperature for 1 hour, then transfer to a 100 mL polytetrafluoroethylene reactor, and react at 120°C for 6 hours. After centrifugation and washing, a white powder was obtained. In an ethanol solution containing 1% of 36% hydrochloric acid, reflux for 24 hours, remove the surfactant, centrifuge, wash, and dry to obtain a phenyl bridged fibrous porous silicon filler. The morphology of phenyl bridged fibrous porous silicon is characterized by fiber ...

Embodiment 2

[0037] Example 2. The recovery rate experiment of sulfa antibiotics in milk

[0038] (1) Preparation of phenyl bridged fibrous porous silicon solid-phase extraction column:

[0039] Using dodecylpyridinium chloride as a structure-directing agent, the silicon source precursor is adjusted to bis(trimethoxysilylethyl)benzene and methyl orthosilicate with a molar ratio of 1:4, using the method of Example 1 The material synthesis step is to prepare phenyl-bridged fibrous porous silicon. A 3 mL empty column tube was filled with 60 mg of phenyl bridged fibrous porous silicon, and compacted with a sieve plate with a thickness of 1.0 mm and a pore diameter of 50 μm to obtain a solid phase extraction column. Pretreat with methanol and water before use, that is, rinse the cartridge with 5mL of methanol first, and then rinse the cartridge with 5mL of water.

[0040] (2) Extraction analysis process of milk with phenyl bridged fibrous porous silicon solid-phase extraction column:

[0041...

Embodiment 3

[0044] Example 3. The standard recovery experiment of sulfa antibiotics in honey

[0045] (1) Preparation of phenyl bridged fibrous porous silicon solid-phase extraction column:

[0046] Using cetyltrimethylammonium bromide as a structure-directing agent, the silicon source precursor was adjusted to [1,4-phenylenebis(methylene)]bis(trimethoxyl) with a molar ratio of 1:2 Silane) and butyl orthosilicate, using the same material synthesis steps as in Example 1, to prepare phenyl bridged fibrous porous silicon. A 10 mL empty column tube was filled with 200 mg of phenyl bridged fibrous porous silicon, and compacted with a sieve plate with a thickness of 2.5 mm and a pore diameter of 20 μm to obtain a solid phase extraction column. Pretreat with methanol and water before use, that is, rinse the cartridge with 5mL of methanol first, and then rinse the cartridge with 5mL of water.

[0047] (2) Extraction and analysis process of honey with phenyl bridge type fibrous porous silicon so...

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Abstract

The invention discloses a phenyl bridge bond type fibrous porous silicon material, and discloses a preparation method of the material and application of the material in the field of sulfonamide antibiotic analysis. The material is prepared by adopting a special microemulsion system, adopting a cationic surfactant as a structure directing agent, and adopting phenyl bridge bonded silane and an inorganic silicon source as a mixed silicon source precursor. The material prepared by the method is applied in enrichment of sulfonamide antibiotics in a sample in a solid phase extraction and enrichmentprocess, and the content of the sulfonamide antibiotics can be determined by liquid chromatography tandem mass spectrometry. The material has the advantages of a three-dimensional central radial fiberpleated porous structure, high specific surface area, high internal surface accessibility, and the like, and can effectively enrich and purify sulfonamide antibiotics in complex samples. The method has advantages of environmental friendliness, simple operation, high detection sensitivity, good reproducibility, and the like and has a huge application potential.

Description

technical field [0001] The invention belongs to the field of analysis materials and detection, and in particular relates to an analysis method of sulfonamide antibiotics based on phenyl-bridged fibrous porous silicon materials. Background technique [0002] Sulfonamide antibiotics, as a class of broad-spectrum antibacterial drugs, are widely used in the prevention and treatment of human, livestock, and aquatic animal diseases. serious harm to ecosystems and human health (Environmental Pollution, 2009, 157:2893-2902). In order to ensure the quality and safety of environmental water bodies and animal-derived foods, the residue analysis of sulfonamide antibiotics has increasingly become a key research object. [0003] The concentration of antibiotic residues in actual samples is low (mostly at the level of ng / L~μg / L), and the sensitivity of the instrument is limited. Therefore, the samples must be pretreated before analysis and detection (Analytica Chimica Acta, 2015, 890 21-4...

Claims

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Application Information

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IPC IPC(8): B01J20/282G01N30/02G01N30/08
CPCB01J20/282G01N30/02G01N30/08G01N2030/484
Inventor 徐桂菊赵汝松张贝贝王晓利李娜
Owner SHANDONG ANALYSIS & TEST CENT
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