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Solid phase extraction column with multi-wall carbon nano-tube matrix and preparation thereof

A multi-walled carbon nanotube and solid-phase extraction column technology, which is applied in the preparation of test samples, chemical instruments and methods, and other chemical processes, etc., can solve the problem of poor fluid passing ability, inability to pass solvent, and improper selection of carbon nanotubes. And other issues

Inactive Publication Date: 2008-08-13
BEIJING JINXIU DADI AGRI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The pressure used in this method is relatively high, which will damage the length and tubular structure of the multi-walled carbon nanotubes, and the characteristics of the multi-walled carbon nanotubes will also change. , leading to poor fluid passing ability, too low flow rate, even in a vacuum state, the solvent cannot pass through
[0008] (2) Improper selection of the amount of carbon nanotubes and column volume

Method used

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  • Solid phase extraction column with multi-wall carbon nano-tube matrix and preparation thereof
  • Solid phase extraction column with multi-wall carbon nano-tube matrix and preparation thereof
  • Solid phase extraction column with multi-wall carbon nano-tube matrix and preparation thereof

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Embodiment 1

[0033] 1. Column material and specification

[0034]The specifications of the existing solid-phase extraction cartridges range from 50mg / 1mL to 10g / 60mL. The column tube material is polypropylene, and there are polyethylene sieve plates with 20 μm pore size on the upper and lower sides of the small column. All the above-mentioned column tubes can be used in the present invention. In the following examples, the present invention uses 0.25g-0.30g / 6mL.

[0035] 2. Granularity (length) of MWNTs

[0036] The packing particle size of the solid-phase extraction column is generally 20-60 μm, and the pore size of the polyethylene sieve plate is 20 μm. In order to prevent the filler from flowing out of the sieve plate, we choose MWNTs with a length of 5 μm-50 μm as the SPE filler.

[0037] 3. Selection of filling volume and filling height

[0038] The flow rate of the SPE column is related to the analysis speed. Generally, the flow rate is required to be 0.5-1mL / min. If the rate is t...

experiment example 1

[0044] The pork sample was purified with a 6 mL SPE column packed in Example 1 and a commercially available C18 column.

[0045] MWCNTs SPE columns need to be pretreated with ethyl acetate, acetone or methanol before use.

[0046] The specific process is as follows: the sample was extracted with acetonitrile, dried by rotary evaporation, 5mL K2HPO4 (pH 7.4) buffer solution and 2mL NaAc (pH 7.0) buffer solution were added to the residue, vortexed to dissolve, and then loaded on the solid phase extraction column. The C18 SPE column was sequentially activated with 5 mL of n-hexane-ethyl acetate (7:3, v / v), 5 mL of methanol and 5 mL of NaAc (pH 7.0) buffer solution, and the flow rate was controlled at 1-1.5 mL / min to buffer the above samples. The solution was directly passed through the C18 SPE column or MWCNTs SPE column, and the column was equilibrated with 5mL NaAc buffer solution, and the water was removed under reduced pressure for 5min, followed by rinsing with 5mL n-hexane ...

Embodiment 2

[0049] The same method as in Example 1 was used to fill a 3mL solid-phase extraction column, the filling height was 0.8-1.1cm, and the filling volume was 0.12g-0.15g / 3mL.

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Abstract

The present invention provides a solid phase extraction column of multi-walled carbon nantubes substrate and its preparing method, belonging to analytical instrument field. The characteristic of the solid phase extraction column of multi-walled carbon nantubes substrate is that the solid phase extraction column substrate is multi-walled carbon nantubes, the filling height of the multi-walled carbon nantubes is 0.8-1.1cm, the computing formula of the filling mass can be seen in the formula (I), wherein, numeric area of a is 0.12-0.15g. It is mainly fit for inverse extracting nonpolarity-medium polarity material, used for enriching, purifying target material in water sample or animal sample. Contrast to the traditional inverse solid phase extraction column (such as C18), the extraction column has a large loading capacity, the cost of the multi-walled carbon nantubes is lower, the material is easy to obtain, the invention employs commercial solid phase extraction column, has a simple preparation, easy to produce in batch.

Description

technical field [0001] The invention belongs to the field of chemical analysis testing instruments and equipment, and relates to a solid-phase extraction column (SPE) with multi-walled carbon nanotubes (WCNTs) as a matrix. Background technique [0002] Solid phase extraction has the characteristics of simple operation, convenience, avoiding emulsification, good repeatability, enrichment and purification functions, so solid phase extraction technology is widely used in the pretreatment process of analysis. Due to the complexity and variety of analyzed samples, it is still a hot spot in SPE research to find efficient and wide-ranging SPE packing materials. [0003] A carbon nanotube (CNT) is a nanoscale hollow tube formed by curling a graphite-like plane composed of a carbon six-membered ring, in which each carbon atom is fully bonded to the surrounding 3 carbon atoms through sp2 hybridization. Carbon nanotubes are composed entirely of surface carbon atoms, and they have a cl...

Claims

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Application Information

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IPC IPC(8): B01D15/08B01J20/281G01N1/34G01N1/40
Inventor 赵海香赵孟彬邓维
Owner BEIJING JINXIU DADI AGRI CO LTD
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