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Solid-phase extraction filler, solid-phase extraction column and preparation method and application of solid-phase extraction filler

A solid-phase extraction column and extraction technology, which is applied in the field of instrument analysis, can solve the problems of low sample capacity, inability to complete rinsing and concentration in one step, and a single extraction functional group, achieving high reproducibility and high extraction recovery rate , high extraction efficiency

Inactive Publication Date: 2016-03-23
XUZHOU MEDICAL COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in actual use, the existing solid-phase extraction cartridges based on amorphous silica gel have technical problems such as single extraction functional groups, low sample capacity, and inability to complete rinsing and concentration in one step.

Method used

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  • Solid-phase extraction filler, solid-phase extraction column and preparation method and application of solid-phase extraction filler
  • Solid-phase extraction filler, solid-phase extraction column and preparation method and application of solid-phase extraction filler

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation method of solid phase extraction filler ODS-CD-HPS comprises the following steps:

[0032] (1) Synthesis of material CD-HPS: Dissolve 22 grams of β-cyclodextrin after vacuum drying (0.1mmHg, 110°C, 14h) in 500 ml of anhydrous dimethylformamide, add 24 mg of sodium hydride Finally, stir the reaction solution at room temperature under the protection of nitrogen to form a transparent solution; then add 3.5 ml of 3-(2,3-epoxypropoxy)propyltrimethoxysilane to the reaction solution, After reacting for 5 hours, add 20 grams of activated silica gel after vacuum drying (particle diameter is 10~20 μm, pore diameter is ), reacted at 120°C for 24 hours; after the reaction mixture was cooled to room temperature, filtered it with a G4 sand core funnel, and the filter cake was washed with dimethylformamide, water, and methanol in turn; finally, the filter cake was placed in a Soxhlet extractor , using acetone as a solvent to extract for 12 hours to obtain bonded sili...

Embodiment 2

[0038] The preparation method of solid phase extraction filler ODS-CD-HPS comprises the following steps:

[0039] (1) Synthesis of material CD-HPS: Dissolve 25 g of β-cyclodextrin after vacuum drying (0.2 mmHg, 120 ° C, 12 h) in 600 ml of anhydrous dimethylformamide, add 26 mg of sodium hydride Finally, stir at room temperature under the protection of nitrogen until the reaction solution is transparent; then add 4.2 ml of 3-(2,3-epoxypropoxy)propyltrimethoxysilane to the reaction solution, and react at 70°C under the protection of nitrogen for 6 After 1 hour, add 22 grams of activated silica gel (particle diameter is 10~20 μm, pore diameter is ), reacted at 110°C for 26 hours; after the reaction mixture was cooled to room temperature, filtered it with a G4 sand core funnel, and the filter cake was washed with dimethylformamide, water, and methanol in sequence; finally, the filter cake was placed in a Soxhlet extractor , using acetone as a solvent to extract for 14 hours to o...

Embodiment 3

[0044] The manufacture of solid-phase extraction cartridges includes the following steps: take a 1 ml empty column, directly fill with 8-10 mg of ODS-CD-HPS filler to form a compact and uniform column bed, and seal both ends of the filler with a sieve plate, To prevent packing leakage, one end of the column is a sample or solvent injection port, and the other end of the column is a sample or solvent outflow port, and the sample or solvent is injected from one end of the column.

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Abstract

The invention discloses solid-phase extraction filler and a preparation method thereof. The filler is filler ODS-CD-HPS bonding beta-cyclodextrin and octadecyl silane mixing functional groups. The invention further discloses a solid-phase extraction column filled with the filler ODS-CD-HPS. The solid-phase extraction column can be applied to pretreatment of biological samples and can be particularly applied to enrichment and analytical detection of medium-polarity and weak-polarity matter in body fluid and tissue homogenate of human bodies. Compared with an existing common solid-phase extraction column based on amorphous silica gel filler, the solid-phase extraction column only needs to be leached with an organic solvent with a small volume, and the extraction recycle rate, reproducibility and extraction efficiency of the medium-polarity and weak-polarity matter are high. Besides, when the solid-phase extraction column is used for pretreatment, leaching and concentrating are completed at a time, and the obtained leached liquid can be enriched and concentrated without extra heating, nitrogen blowing and other steps.

Description

technical field [0001] The invention belongs to the technical field of instrument analysis, and in particular relates to a solid-phase extraction filler, a solid-phase extraction small column and a preparation method and application thereof. Background technique [0002] The composition of biological samples is complex, and the matrix interference is serious. The analysis and detection of endogenous substances in biological samples has always been the focus of analysts. Existing biological sample pretreatment methods include organic solvent precipitation (OSP), liquid-liquid extraction (LLE), solid phase extraction (SPE), solid phase microextraction (SPME) and so on. Among them, solid phase extraction is the most widely used. [0003] The solid phase extraction method is mainly through the selective adsorption and desorption process of the sample components on the solid phase filler to realize the separation, purification and enrichment of the sample. Its main purpose is to...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30B01D15/08G01N30/06
Inventor 龚银汉印晓星魏群利
Owner XUZHOU MEDICAL COLLEGE
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