Preparation method for mixed hemimicelle solid-phase extraction agent based on DMSA@Fe3O4 magnetic nanoparticles

A technology of magnetic nanoparticles and mixed semimicelles, applied in chemical instruments and methods, alkali metal compounds, chemical/physical processes, etc.

Inactive Publication Date: 2017-04-05
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to overcome the shortcoming in the above-mentioned traditional complex matrix sample pretreatment technology, provide a kind of preparation method based on the ferroferroic oxide magnetic nanoparticle mixed semimicelle solid-phase extraction agent modified by dimercaptosuccinic acid, utilize this The magnetic solid-phase extractant prepared by the method is applied to the extraction of sulfonamide antibiotics in environmental water samples. The extractant has the following advantages: less amount of extractant, high extraction efficiency; environmental protection, low cost; simple operation, fast extraction speed; Good stability, renewable and reusable

Method used

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  • Preparation method for mixed hemimicelle solid-phase extraction agent based on DMSA@Fe3O4 magnetic nanoparticles
  • Preparation method for mixed hemimicelle solid-phase extraction agent based on DMSA@Fe3O4 magnetic nanoparticles

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Effect test

Embodiment 1

[0027] After mixing 15mL oleylamine and 15mL benzyl ether, add 1.0596g iron acetylacetonate, and after ultrasonication for 20min, pour the mixed liquid into the lining of the reaction kettle, seal it, and place it in a muffle furnace for 2h at 185°C, and the reaction is over. After cooling to room temperature, washing with absolute ethanol several times, vacuum drying at 60°C to constant weight to obtain ferroferric oxide magnetic nanoparticles;

[0028] Disperse 10 mg of ferroferric oxide magnetic nanoparticles prepared above into 1 mL of toluene, add 1 mL of dimethyl sulfoxide solution dissolved with 10 mg of dimercaptosuccinic acid, sonicate for 2 h, place on a shaker at 25 ° C for 24 h, and then take it out. Wash with absolute ethanol, centrifuge 3 times, and finally disperse the obtained dimercaptosuccinic acid-modified ferroferric oxide magnetic nanoparticles in 1 mL of distilled water;

[0029] Take 50mL blank environmental water sample in the Erlenmeyer flask, adjust t...

Embodiment 2

[0031] After mixing 15mL oleylamine and 15mL benzyl ether, add 1.0596g iron acetylacetonate, and after ultrasonication for 20min, pour the mixed liquid into the lining of the reaction kettle, seal it, and place it in a muffle furnace for 2h at 185°C, and the reaction is over. After cooling to room temperature, washing with absolute ethanol several times, vacuum drying at 60°C to constant weight to obtain ferroferric oxide magnetic nanoparticles;

[0032] Disperse 10 mg of ferroferric oxide magnetic nanoparticles prepared above into 1 mL of toluene, add 1 mL of dimethyl sulfoxide solution dissolved with 10 mg of dimercaptosuccinic acid, sonicate for 2 h, place on a shaker at 25 ° C for 24 h, and then take it out. Wash with absolute ethanol, centrifuge 3 times, and finally disperse the obtained dimercaptosuccinic acid-modified ferroferric oxide magnetic nanoparticles in 1 mL of distilled water;

[0033] Take 100mL blank environmental water sample in the Erlenmeyer flask, adjust ...

Embodiment 3

[0035] After mixing 15mL oleylamine and 15mL benzyl ether, add 1.0596g iron acetylacetonate, and after ultrasonication for 20min, pour the mixed liquid into the lining of the reaction kettle, seal it, and place it in a muffle furnace for 2h at 185°C, and the reaction is over. After cooling to room temperature, washing with absolute ethanol several times, vacuum drying at 60°C to constant weight to obtain ferroferric oxide magnetic nanoparticles;

[0036] Disperse 10 mg of ferroferric oxide magnetic nanoparticles prepared above into 1 mL of toluene, add 1 mL of dimethyl sulfoxide solution dissolved with 10 mg of dimercaptosuccinic acid, sonicate for 2 h, place on a shaker at 25 ° C for 24 h, and then take it out. Wash with absolute ethanol, centrifuge 3 times, and finally disperse the obtained dimercaptosuccinic acid-modified ferroferric oxide magnetic nanoparticles in 1 mL of distilled water;

[0037] Take 50mL blank environmental water sample in the Erlenmeyer flask, adjust t...

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Abstract

The invention relates to a preparation method for a mixed hemimicelle solid-phase extraction agent based on dimercaptosuccinic acid modified ferroferric oxide magnetic nanoparticles. The preparation process mainly comprises the four steps of preparation of ferroferric oxide magnetic nanoparticles, preparation of the dimercaptosuccinic acid modified ferroferric oxide magnetic nanoparticles, preparation of the mixed hemimicelle solid-phase extraction agent and a solid-phase extraction process. The synthetic method provided by the invention is simple and convenient, target object separation can be achieved just through little absorbing agents and short equilibrium time in the extraction process, the extraction capacity is high, lots of toxic and harmful solvents do not need to be used, and environmental friendliness is achieved; and meanwhile, influences of complex matrix effects of environmental samples can be effectively reduced, and the method is quite suitable for the rapid analyzing requirement of trace PPCPs compounds in complex matrixes.

Description

technical field [0001] The invention belongs to the field of new material science, in particular to a method for preparing a mixed semimicelle solid-phase extraction agent based on dimercaptosuccinic acid-modified ferroferric oxide magnetic nanoparticles, and using it as a sample pretreatment material to extract Extraction and enrichment of trace pharmaceuticals and personal care products (Pharmaceutical and Personal Care Products, PPCPs) in complex matrices. Background technique [0002] PPCPs mainly refer to various drugs (such as antibiotics, steroids, anti-inflammatory drugs, sedatives, antiepileptic drugs, contraceptives, nerve stimulants, etc.) agents, disinfectants, etc.). PPCPs are a new class of global pollutants, and their residues are a research hotspot in the current environmental field. In recent years, with the continuous development of detection and analysis methods, there are more and more reports on the detection of residual PPCPs in complex matrices. Ant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30B01D15/08
Inventor 王娜肖得力邱盼子袁丹华何华
Owner CHINA PHARM UNIV
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