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Amphoteric electrolyte-modified hybrid silica gel material and solid-phase extraction method thereof

An amphoteric electrolyte, hybrid silica gel technology, applied in organic chemistry methods, chemical instruments and methods, zwitterion exchange, etc., to achieve high recovery, fast adsorption and desorption, and improved speed and accuracy.

Inactive Publication Date: 2013-03-27
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the composite adsorption mechanism of solid phase extraction is only a combination of reverse phase and anion (cation) ion exchange, and does not combine the cation exchange mechanism and anion exchange mechanism on the same stationary phase to achieve the extraction of acidic, neutral and alkaline samples.

Method used

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  • Amphoteric electrolyte-modified hybrid silica gel material and solid-phase extraction method thereof
  • Amphoteric electrolyte-modified hybrid silica gel material and solid-phase extraction method thereof
  • Amphoteric electrolyte-modified hybrid silica gel material and solid-phase extraction method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The synthetic route for the preparation of ampholyte-modified hybrid silica materials is as follows figure 1 As shown, tetraethoxysilane (TEOS) and aminopropyltriethoxysilane (APTES) were used as precursor molecules, cetyltrimethylammonium bromide (CTAB) was used as template agent, and absolute ethanol As a solvent, a hybrid silica material with amine groups on the surface was prepared by sol-gel method ( figure 1 ). The amine group of the hybrid silica gel material reacts with the excess aldehyde group of glutaraldehyde under the condition of pH 8.0 to form C=N, so that the surface of the hybrid silica gel is bonded to the aldehyde group, and the same method is applied to the Under the condition of pH 8.0, the aldehyde group at the other end of the glutaraldehyde bonded to the hybrid silica material reacts with the amine group of the excess ampholyte to form C=N, which is unstable and requires NaCNBH 3 Reduction of C=N to stable C-N ( figure 1 ).

[0029] The speci...

Embodiment 2

[0032] Weigh 50 mg of the ampholyte-modified hybrid silica gel material prepared in Example 1, put it into a 3mL column tube with a lower sieve plate with a pore diameter of 5 μm, fill it into an upper sieve plate with a pore diameter of 20 μm, shake it evenly with a vibrating bed, press the column Machine compaction.

Embodiment 3

[0034] The quartz capillary was sequentially passed through concentrated HNO 3(10min), distilled water, HF (10min), distilled water, 1mol / L NaOH (12h), distilled water, 0.1mol / L HCl (1h), distilled water, methanol after treatment, put the quartz capillary column in the gas chromatography furnace, 120°C N 2 Dry under flow for 3 h, add 112 μL tetraethoxysilane (TEOS), 118 μL aminopropyltriethoxysilane (APTES), 215 μL absolute ethanol, 32 μL water, and 8 mg cetyltrimethylammonium bromide (CTAB) After fully mixing, introduce it into the pretreated quartz capillary via a syringe, seal both ends with silicone rubber, heat at 40°C for reaction polymerization for 24 hours, and rinse the polymerized material with ethanol through a constant flow syringe pump to remove CTAB (30min ), then washed with water and 100mmol / L phosphate (pH 8.0) respectively, and then continuously pumped 100mmol / L phosphate (pH 8.0) containing 10% glutaraldehyde, reacted at 90°C for 0.5h, and washed with phosp...

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Abstract

The invention discloses an amphoteric electrolyte-modified hybrid silica gel material. An amphoteric electrolyte containing an amino group and a carboxyl group is bonded on a branch of the hybrid silica gel to obtain a hybrid silica gel material with an amphoteric group on the surface. A preparation method of the hybrid silica gel material comprises the following steps of: forming a hybrid silica gel material containing amino on the surface by taking tetraethoxy silane and aminopropyltriethoxy silane as precursor molecules and taking hexadecyl trimethyl ammonium bromide as a template agent; enabling the hybrid silica gel to react with the aldehyde group of glutaraldehyde to generate a hybrid silica gel material with a C=N bond; enabling the aldehyde group at the other end of glutaraldehyde on the hybrid silica gel material to react with the amphoteric electrolyte with the amino group and the carboxyl group to generate a hybrid silica gel material with double C=N bonds; and reducing with NaCNBH3 to reduce C=N into C-N to form a hybrid silica gel material with multiple -NH2 groups and multiple -COOH groups. A solid-phase extraction column or solid-phase extraction capillary tube prepared from the hybrid silica gel material gives play to the advantages of anion-cation exchange on the same material at the same time by controlling the pH value, and realizes synchronous extraction of acid, neutral and alkali samples; and moreover, the adsorption and desorption are fast, the reproducibility and recovery rate are high, and the speed and precision of detection and separation can be improved.

Description

technical field [0001] The invention relates to the technical field of sample pretreatment, in particular to a hybrid silica gel material modified with amphoteric electrolytes and a solid-phase extraction method thereof. Background technique [0002] Solid phase extraction (SPE) is a method of selective adsorption and selective elution to enrich, separate and purify samples, including liquid and solid phase physical extraction processes, not only suitable for the extraction and enrichment of food and environmental water It is suitable for trace organic compounds in samples, and is suitable for the enrichment of measured components in biological samples. [0003] The main representatives of the composite adsorption mechanism of solid phase extraction materials are Oasis MCX and Oasis WCX, whose adsorption mechanism combines reversed-phase retention and strong (weak) cation exchange, and is limited to the analysis of alkaline samples, or Oasis MAX and Oasis WAX, whose adsorpti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21C07B63/00C07C47/58C07C45/79C07C67/56C07C69/84C07D275/06C07C51/47C07C65/03B01J20/286B01J20/30B01D15/08
CPCB01J43/00B01J47/014
Inventor 王婷婷陈易晖陈明良胡敏杰李颖杨春风房江华高浩其
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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