Preparation of Attapulgite Capillary Monolithic Column and Its Application in Solid Phase Microextraction

Abstract

The invention provides a preparation method of an embedded attapulgite capillary monolithic column. The method comprises the following steps of mixing acidified attapulgite and an organic polymer solution at a mass ratio being 1:100 to 5:100; performing magnetic stirring for 1 to 5 hours at the normal temperature so that the acidified attapulgite is completely dispersed; then, injecting the material into a quartz capillary treated by gamma-2-methyl propyl trimethoxy silane; sealing the material; then putting the materials into a constant-temperature water bath pot for reaction for 16 to 24h at 60 to 85 DEG C; after the reaction is completed, using acetonitrile and water for flushing; preparing the material for use. The natural attapulgite nanometer materials are embedded into an organic polymer monolithic material for the first time; the embedded attapulgite capillary monolithic column is prepared. The preparation method has the advantages that the simplicity is realized; the cost is low; the reaction condition can be easily controlled; the prepared embedded attapulgite capillary monolithic column has higher mechanical intensity and higher permeability; when the prepared embedded attapulgite capillary monolithic column is used as an adsorbing agent to be applied to solid micro extraction, the advantages of great adsorption volume, high recovery yield, good reproducibility, low detection limit and the like are realized. The preparation method is applicable to the sample pretreatment of polar small-molecular compounds.

Description

technical field [0001] The invention relates to a chromatographic analysis sample pretreatment technology, in particular to a preparation of a capillary integral column embedded with attapulgite and a solid-phase microextraction method. Background technique [0002] In recent years, due to the advantages of simple preparation, good permeability, wide pH range, convenient modification and fast mass transfer, organic polymer monolithic columns have attracted extensive attention in the field of sample pretreatment. However, the lack of microporous structure of this material makes its specific surface area only tens of square meters per gram, and there are fewer interaction sites with the sample, and the column capacity is insufficient, resulting in its adsorption capacity for small molecules being lower than that of granular fillers. Even the overall silicone material. [0003] Nanomaterials have small crystal grains and large specific surface area, which make them produce qua...

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Problems solved by technology

However, the lack of microporous structure of this kind of material makes its specific surface area only tens of square meters per gram, and there are fewer interaction sites with the sample, and the column capacity is insufficient, resulting in its adsorption capacity for small molecules being lower than that of granular fillers. Even the overall silicone material

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