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Solid phase extraction column with functionalized multi-walled carbon nanotube substrate, and preparation method thereof

A technology of multi-walled carbon nanotubes and solid phase extraction columns, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of difficulty in dispersing into bundles and extensive application research of carbon nanotubes, so as to improve the recovery rate, Functional experimental scheme is flexible and changeable, and the effect of materials is easy to obtain

Active Publication Date: 2013-11-06
SHANTOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Carbon nanotubes are a kind of polymer inorganic material, and the adsorption force between the tubes is strong. Therefore, carbon nanotubes are insoluble in water and organic solvents and difficult to disperse in bundles, which limits the application research of carbon nanotubes in various fields. However, the main reason is broad

Method used

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  • Solid phase extraction column with functionalized multi-walled carbon nanotube substrate, and preparation method thereof
  • Solid phase extraction column with functionalized multi-walled carbon nanotube substrate, and preparation method thereof
  • Solid phase extraction column with functionalized multi-walled carbon nanotube substrate, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Fill a 3 mL solid-phase extraction column with the method in step A above, the filling height is 0.8-1.2 cm, and the filling volume is 0.08-0.15 g / 3 mL. Extraction of parabens in cosmetics using the solid-phase extraction column described above (spiked recovery and actual sample detection).

[0044] The f-MWCNTs SPE column needs to be pretreated with deionized water, ethyl acetate, acetone or methanol before use.

[0045] The specific process is as follows: 2 parts of 1 g cosmetic samples were weighed, 6 kinds of paraben ester preservative standard substances were added to sample 1 (all 6 kinds of preservatives were added in an amount of 2.5 μg), and no standard substance was added to sample 2. Place samples 1 and 2 in two different centrifuge tubes, use mobile phase to make up to 5 mL respectively, and extract ultrasonically for 30 min. After the extract is properly diluted, filter it with a 0.5 μm filter membrane, and the filtrates of samples 1 and 2 are used for soli...

Embodiment 2

[0052] Fill a 6 mL solid-phase extraction column with the method in step A above, the filling height is 0.8-1.2 cm, and the filling volume is 0.15-0.30 g / 6 mL. The polycyclic aromatic hydrocarbons in purified water samples were enriched using the solid phase extraction column described above.

[0053] The f-MWCNTs SPE column was pretreated with deionized water, ethyl acetate, acetone or methanol before use.

[0054] The specific process is as follows: seawater and river water samples were collected respectively, the samples were centrifuged separately, 200 mL of the supernatant was taken, filtered with a 0.5 μm filter membrane, and the filtrate was transferred to a corresponding 200 mL volumetric flask. Take two packed 6 mL f-MWCNTs SPE columns, activate them with deionized water, ethyl acetate, acetone or methanol, and let the above two filtrates pass through the f-MWCNTs SPE columns respectively, and control the flow rate under the vacuum pump to 3-5 mL / min. After all the ...

experiment example 3

[0055] Experimental example 3 Use the method in step A above to fill a 6 mL solid phase extraction column, the filling height is 0.8-1.2 cm, and the filling volume is 0.15-0.30 g / 6 mL. Neomycin residues were enriched in milk samples using the solid-phase extraction column described above.

[0056] The f-MWCNTs SPE column was pretreated with deionized water, ethyl acetate, acetone or methanol before use.

[0057] The specific process is as follows: Measure 10 mL of pure milk into a 15 mL polypropylene plastic centrifuge tube, add a certain volume of 10 μg / mL neomycin standard solution, shake evenly, and obtain a spiked milk sample containing a certain concentration of neomycin. Add 1 mL of 0.2 g / mL trichloroacetic acid solution, shake for 1 min, and centrifuge at 6000 g at 25 °C for 30 min. Carefully pipette 5 mL of the upper clear liquid for loading on the solid-phase extraction column. After the activation of the f-MWCNTs SPE column was completed, the supernatant was passed...

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Abstract

The invention specifically relates to a solid phase extraction column with a functionalized multi-walled carbon nanotube substrate, and a preparation method thereof. The substrate of the solid phase extraction column provided by the invention is functionalized multi-walled carbon nanotubes which are prepared from original multi-walled carbon nanotubes by purification, carboxylation, chlorination and functionalization covalence chemical modification. The functionalized multi-walled carbon nanotubes have a packing height of 0.8-1.2cm, and are mainly suitable for reversed-phase extraction of nonpolar to medium polar substances for concentrating and purifying target substances in a sample to be tested. The solid phase extraction column provided by the invention has large adsorption capacity on target substances and high recovery rate (92-103%) of target substances, has the characteristics of low preparation cost, easy availability of material, a simple functionalization process and strong adaptability, and is easy for mass production.

Description

technical field [0001] The invention belongs to the field of chemical analysis testing instruments and equipment. Specifically, the invention relates to a functionalized multi-walled carbon nanotube matrix solid-phase extraction column, and the invention also relates to a preparation method of the extraction column. Background technique [0002] Solid phase extraction (Solid phase extraction, SPE) technology has been developed in many fields since it came out in the late 1970s. In foreign countries, it has gradually replaced the traditional liquid-liquid extraction and has become a reliable and effective method for sample pretreatment. SPE technology is a separation and purification method based on the principle of liquid chromatography. The adsorbent is a stationary phase, and according to the adsorption of the solid-phase extractant to the liquid-phase analyte, when the analyte passes through the extractant, the target substance in the sample is adsorbed on the extractant...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/20B01J20/30
Inventor 高文华孙希萌张美金黄晓鹏纪淑英陈耀文陈图锋
Owner SHANTOU UNIV
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