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Preparation method of mixed hemi-micelle solid phase extractant based on magnetic carbon nanotubes

A technology of magnetic carbon nanotubes and solid-phase extraction agents, applied in chemical instruments and methods, material separation, instruments, etc., can solve the problems of time-consuming operation, high consumption of adsorbent, large particles, etc.

Inactive Publication Date: 2015-07-22
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although the mixed semimicelle solid phase extraction technique has various advantages, due to the A1 used in the adsorbent 2 o 3 and SiO 2 The particles of the carrier are relatively large and the specific surface area is small, so in the actual analysis process, the consumption of adsorbent is more
Moreover, this technology mostly uses column packing operation. In actual application, the steps are cumbersome and the operation is time-consuming.
Especially when it is applied to the research and determination of complex matrix samples, it needs to go through a relatively tedious and time-consuming sample pretreatment process

Method used

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  • Preparation method of mixed hemi-micelle solid phase extractant based on magnetic carbon nanotubes
  • Preparation method of mixed hemi-micelle solid phase extractant based on magnetic carbon nanotubes
  • Preparation method of mixed hemi-micelle solid phase extractant based on magnetic carbon nanotubes

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Experimental program
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Effect test

Embodiment 1

[0028] Add 0.5 g of multi-walled carbon nanotubes to 160 ml of concentrated HNO with a volume ratio of 1:3 3 - Concentrated H 2 SO 4 In the mixed solution, ultrasonically reacted for 6 hours, filtered under reduced pressure, washed repeatedly with distilled water until neutral, dried in vacuum at 60°C to constant weight, and set aside;

[0029]0.4g of the carboxylated carbon nanotubes prepared above, 2.4g of ferric chloride, 3.4g of sodium acetate and 3.4g of sodium acrylate were added to a mixed solvent consisting of 33.75ml of ethylene glycol and 11.25ml of diethylene glycol, and ultrasonically 1h to get a black mixed solution, transfer it to a reaction kettle made of polytetrafluoroethylene, seal it, and place it in a muffle furnace for 10h. After the reaction, cool to room temperature, wash with methanol and water several times, and vacuum at 60°C. Dry to constant weight and set aside;

[0030] Add 4.0mg of the above-prepared magnetic carbon nanotubes, 1.0mg of cetyltri...

Embodiment 2

[0032] Add 0.5 g of multi-walled carbon nanotubes to 160 mL of concentrated HMO with a volume ratio of 1:3 3 - Concentrated H 2 SO 4 In the mixed solution, ultrasonically reacted for 6 hours, filtered under reduced pressure, washed repeatedly with distilled water until neutral, dried in vacuum at 60°C to constant weight, and set aside;

[0033] Add 0.4 g of the carboxylated carbon nanotubes prepared above, 2.4 g of ferric chloride, 3.4 g of sodium acetate, and 3.4 g of sodium acrylate into a mixed solvent consisting of 33.75 mL of ethylene glycol and 11.25 mL of diethylene glycol, and ultrasonically 1h to get a black mixed solution, transfer it to a reaction kettle made of polytetrafluoroethylene, seal it, and place it in a muffle furnace for 10h. After the reaction, cool to room temperature, wash with methanol and water several times, and vacuum at 60°C. Dry to constant weight and set aside;

[0034] 4.0mg of the magnetic carbon nanotubes prepared above, 3.0mg of 1-dodecyl...

Embodiment 3

[0036] Add 0.5 g of multi-walled carbon nanotubes to 160 mL of concentrated HNO with a volume ratio of 1:3 3 - Concentrated H 2 SO 4 In the mixed solution, ultrasonically reacted for 6 hours, filtered under reduced pressure, washed repeatedly with distilled water until neutral, dried in vacuum at 60°C to constant weight, and set aside;

[0037] Add 0.4 g of the carboxylated carbon nanotubes prepared above, 2.4 g of ferric chloride, 3.4 g of sodium acetate, and 3.4 g of sodium acrylate into a mixed solvent consisting of 33.75 mL of ethylene glycol and 11.25 mL of diethylene glycol, and ultrasonically 1h to get a black mixed solution, transfer it to a reaction kettle made of polytetrafluoroethylene, seal it, and place it in a muffle furnace for 10h. After the reaction, cool to room temperature, wash with methanol and water several times, and vacuum at 60°C. Dry to constant weight and set aside;

[0038] Add 1.0g of magnetic carbon nanotubes to 150mL of ethanol and 25mL of dei...

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Abstract

The invention relates to a preparation method of a mixed hemi-micelle solid phase extractant based on magnetic carbon nanotubes. The preparation process mainly comprises three steps: preparation of magnetic carbon nanotubes; preparation of a mixed hemi-micelle solid phase extractant; and the process of solid phase extraction. A synthetic method provided by the invention is simple and easy to control. The prepared magnetic mixed hemi-micelle solid phase extractant has advantages of high extraction efficiency and large extraction sample area, can be used to save organic solvents, can be reutilized, is very suitable for rapid sample analysis requirements and is of great significance for researches on highly sensitive detection of flavonoid drugs.

Description

technical field [0001] The invention belongs to the field of new material science, and particularly relates to a preparation method of a mixed semimicelle solid-phase extraction agent based on magnetic carbon nanotubes, which is used as a sample pretreatment material to extract and enrich compounds in biological samples. Background technique [0002] Mixed semimicelle solid phase extraction is a new solid phase extraction technique. This technology is to adsorb various ionic surfactants or ionic liquids on the surface of various metal oxide carriers through electrostatic attraction, hydrophobic force, etc. to form mixed semi-micelles, and use them as solid-phase extraction adsorption reagents to enrich, purify and concentrate the analyte in the sample. This new solid-phase extraction technology has many advantages such as high extraction efficiency, large volume of extracted samples, saving organic solvents, easy elution and reusable adsorbent, etc., which is very suitable ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/283B01J20/30G01N30/08
Inventor 何华肖得力袁丹华戴昊何佳彭军李思桥
Owner CHINA PHARM UNIV
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