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Preparation method of mixed hemi-micelle solid phase extractant based on Fe3O4 magnetic nanoparticles

A technology of magnetic nanoparticles and solid-phase extraction agents, applied in chemical instruments and methods, silicon compounds, alkali metal compounds, etc., can solve the problems of large particles, time-consuming operation, and high consumption of adsorbents, 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, however, due to the Al 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 time-consuming. Especially when it is applied to the research and determination of complex matrix samples, it also requires a cumbersome and time-consuming sample pretreatment process.

Method used

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  • Preparation method of mixed hemi-micelle solid phase extractant based on Fe3O4 magnetic nanoparticles
  • Preparation method of mixed hemi-micelle solid phase extractant based on Fe3O4 magnetic nanoparticles
  • Preparation method of mixed hemi-micelle solid phase extractant based on Fe3O4 magnetic nanoparticles

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Experimental program
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Effect test

Embodiment 1

[0027] Add 2.4g of ferric chloride, 3.4g of sodium acetate and 3.4g of sodium acrylate into a mixed solvent consisting of 33.75ml of ethylene glycol and 11.25ml of diethylene glycol, and ultrasonically obtain a black mixed solution for 1 hour, which is transferred to a poly In a reaction kettle made of tetrafluoroethylene, seal it, place it in a muffle furnace to react for 10 hours, cool to room temperature after the reaction, wash with methanol and water several times, vacuum dry at 60°C to constant weight, and set aside;

[0028] 4.0mg of the above-prepared Fe 3 o 4 Magnetic nanoparticles, 1.0mg cetyltrimethylammonium bromide (CTAB) and 2ml 0.02M sodium phosphate buffer solution with pH = 7.0 were sequentially added to the plastic tube, the mixture was ultrasonically dispersed for 5 minutes, and then balanced for 10 minutes. Afterwards, an external magnetic field was placed on the side wall of the plastic tube to separate the magnetic particles. After 2 seconds, the supernata...

Embodiment 2

[0030] Add 2.4g of ferric chloride, 3.4g of sodium acetate and 3.4g of sodium acrylate into a mixed solvent consisting of 33.75ml of ethylene glycol and 11.25ml of diethylene glycol, and ultrasonically obtain a black mixed solution for 1 hour, which is transferred to a poly In a reaction kettle made of tetrafluoroethylene, seal it, place it in a muffle furnace to react for 10 hours, cool to room temperature after the reaction, wash with methanol and water several times, vacuum dry at 60°C to constant weight, and set aside;

[0031] 4.0mg of the above-prepared Fe 3 o 4 Magnetic nanoparticles, 3.0 mg 1-dodecyl-3-methylimidazole chloride (C 12 mimCl) and 2m10.02M potassium phosphate buffer solution with pH=7.0 were sequentially added into the plastic tube, the mixed solution was ultrasonically dispersed for 5min, then equilibrated and left for 10min, and then an external magnetic field was placed on the side wall of the plastic tube to separate the magnetic particles. After 2s, ...

Embodiment 3

[0033] Add 2.4g of ferric chloride, 3.4g of sodium acetate and 3.4g of sodium acrylate into a mixed solvent consisting of 33.75ml of ethylene glycol and 11.25ml of diethylene glycol, and ultrasonically obtain a black mixed solution for 1 hour, which is transferred to a poly In a reaction kettle made of tetrafluoroethylene, seal it, place it in a muffle furnace to react for 10 hours, cool to room temperature after the reaction, wash with methanol and water several times, vacuum dry at 60°C to constant weight, and set aside;

[0034] 1.0g Fe 3 o 4 Add magnetic nanoparticles to 150mL ethanol and 25mL deionized water, ultrasonicate for 5min, then add 2mL ammonia water and 5mL tetraethyl orthosilicate in sequence, and react for 6h under stirring. After the reaction, add an external magnetic field to separate the product, wash with methanol and water several times , vacuum-dried at 60°C to constant weight, and set aside.

[0035] 4.0mg of the above-prepared Fe 3 o 4 SiO 2 Magne...

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Abstract

The invention relates to a preparation method of a mixed hemi-micelle solid phase extractant based on Fe3O4 magnetic nanoparticles. The preparation process mainly comprises three steps: preparation of Fe3O4 magnetic nanoparticles; 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 high extraction efficiency and is simple to operate. Pretreatment time of samples can be greatly shortened; a lot of poisonous and harmful solvents are not required; pollution is avoided; and loss of samples can be effectively reduced. The mixed hemi-micelle solid phase extractant is very suitable for rapid sample analysis requirements.

Description

technical field [0001] The invention belongs to the field of new material science, in particular to a Fe-based 3 o 4 The preparation method of the mixed semimicelle solid phase extraction agent of magnetic nanoparticles 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. Compared with the traditional environmental sample pretreatment method, this new sample pretreatment technology has high extraction efficiency, easy operation, can greatly shorten the sample pretreatment time, does not require a ...

Claims

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Application Information

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IPC IPC(8): B01J20/10B01J20/28B01J20/30B01D15/08
Inventor 何华肖得力袁丹华张婵戴昊邱盼子何佳
Owner CHINA PHARM UNIV
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