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Multifunctional mesoporous silicone solid-phase extraction agent and preparation method and application thereof

A technology of solid-phase extraction agent and mesoporous silica gel, which is applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the problems that are not suitable for the analysis of polar ionic drugs, and achieve the cost of preparation Inexpensive, strong selectivity and enrichment ability, solve the effect of low extraction efficiency

Active Publication Date: 2019-01-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the current functionalized mesoporous silica gel materials are monofunctional materials, that is, they can only be used as a single-mode extraction agent and are not suitable for the analysis of polar ionic drugs.
The present invention prepares a multifunctional mesoporous silica gel material through a simple two-step reaction, and uses it as a reversed-phase / strong anion exchange mixed-mode extractant to separate and enrich NSAIDs in environmental water samples. Not yet reported in

Method used

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  • Multifunctional mesoporous silicone solid-phase extraction agent and preparation method and application thereof
  • Multifunctional mesoporous silicone solid-phase extraction agent and preparation method and application thereof
  • Multifunctional mesoporous silicone solid-phase extraction agent and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0021] (1) Dissolve 13.8g Pluronic P123 and 7.6g mass concentration of 35% concentrated hydrochloric acid in 250mL water, stir fully for 4h, after P123 is completely dissolved to transparent, add 24.8g ethyl orthosilicate dropwise under vigorous stirring, the mixture The solution was continuously stirred in a water bath at 35 °C for 24 h. Then the mixture was transferred into a reactor and hydrothermally treated at 120 °C for 48 h. After cooling, it was suction filtered and washed with water. Finally, the product was moved into a muffle furnace and calcined at 550°C for 2 hours to obtain mesoporous silica gel;

[0022] (2) Soak the obtained mesoporous silica gel in 3mol / L hydrochloric acid solution overnight, then dehydrate and activate at 160°C for 6 hours, cool and store in a desiccator for later use;

[0023] (3) Disperse 4g of the above-mentioned activated mesoporous silica gel in 110mL of anhydrous toluene, add 4mL of 3-(2-aminoethylamino)propyltrimethoxysilane under st...

Embodiment 2

[0025] Example 2: (1) Dissolve 13.8g of Pluronic P123 and 7.6g of concentrated hydrochloric acid with a mass concentration of 35% in 250mL of water, and stir thoroughly for 4 hours. After the P123 is completely dissolved to transparent, add 24.8g of ethyl orthosilicate dropwise under vigorous stirring ester, the mixture was continuously stirred in a water bath at 35°C for 24h. Then the mixture was transferred into a reactor and hydrothermally treated at 140 °C for 48 h. After cooling, it was suction filtered and washed with water. Finally, the product was moved into a muffle furnace and calcined at 550°C for 2 hours to obtain mesoporous silica gel;

[0026] (2) Soak the obtained mesoporous silica gel in 3mol / L hydrochloric acid solution overnight, then dehydrate and activate at 160°C for 6 hours, cool and store in a desiccator for later use;

[0027] (3) Disperse 4g of the above-mentioned activated mesoporous silica gel in 110mL of anhydrous toluene, add 4mL of 3-[2-(2-amino...

Embodiment 3

[0029] Embodiment 3: the preparation method of multifunctional mesoporous silica gel extractant of the present invention

[0030] The schematic diagram of the functionalization of the multifunctional mesoporous silica gel extractant provided by the present invention is as follows: figure 1 shown.

[0031] (1) Dissolve 13.8g Pluronic P123 and 7.6g mass concentration of 35% concentrated hydrochloric acid in 250mL water, stir fully for 4h, after P123 is completely dissolved to transparent, add 24.8g ethyl orthosilicate dropwise under vigorous stirring, the mixture The solution was continuously stirred in a water bath at 35 °C for 24 h. Then the mixture was transferred into a reactor and hydrothermally treated at 130 °C for 48 h. After cooling, it was suction filtered and washed with water. Finally, the product was moved into a muffle furnace and calcined at 550°C for 2 hours to obtain mesoporous silica gel;

[0032] (2) Soak the obtained mesoporous silica gel in 3mol / L hydroc...

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Abstract

The invention provides a preparation method of a multifunctional mesoporous silicone solid-phase extraction agent. The preparation method of the multifunctional mesoporous silicone solid-phase extraction agent is characterized in that firstly, SBA-15 mesoporous silicone serves as a base material, 3-(2-aminoethylamino)propyl-trimethoxysilane or 3-[2-(2-aminoethylamino)ethylamino]propyl-trimethoxysilane which contains more than 2 amino groups serves a silylation reagent, multi-amino mesoporous silicone is obtained, then, ring-opening reaction of amino groups and epoxy groups is adopted, the multi-amino mesoporous silicone further reacts with excess phenyl glycidyl ether, and the mesoporous silicone extraction agent has high-density surface multifunctional groups is obtained. The mesoporous silicone extraction agent has high specific surface area of a mesoporous material, the high-density surface multifunctional groups and supramaximal extraction capacity and also has a reversed-phase adsorption effect of multiple phenyl groups and a powerful anion exchange function of quaternary ammonium groups, and therefore the mesoporous silicone extraction agent is a high-selectivity mixed-mode solid-phase extraction agent. The mesoporous silicone extraction agent is quite suitable for analyzing acid non-steroidal anti-inflammatory drugs in large-volume environmental water samples.

Description

technical field [0001] The invention relates to the preparation and application of a multifunctional mesoporous silica gel solid-phase extraction agent for separating and enriching non-steroidal anti-inflammatory drugs in water environment, and belongs to the fields of environmental monitoring and new materials. Background technique [0002] Non-steroidal anti-inflammatory drugs (NSAIDs) are a class of antipyretic, analgesic and anti-inflammatory drugs commonly used in clinical practice. They are widely used in the relief of rheumatic diseases, arthritis, various fevers and various pain symptoms. Fen, naproxen and ketoprofen. At present, NSAIDs are one of the most widely used drugs in the world. Because they are difficult to be effectively removed in sewage treatment plants, active substances of such drugs continuously enter the water environment, causing persistent water environment pollution. In recent years, NSAIDs pollutants have been detected in sewage, surface water a...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30B01D15/08C02F1/28C02F1/42C02F101/30
CPCB01D15/08B01J20/103B01J20/22B01J20/28083C02F1/285C02F1/42C02F2001/422C02F2101/30
Inventor 李云陈吉平黄超囡王龙星
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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