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Preparation method and application of guanidine salt ionic liquid modified magnetic solid-phase extraction adsorbent

An ionic liquid and adsorbent technology, which is applied in the field of magnetic solid phase extraction adsorbents modified by guanidine salt ionic liquids, can solve the problems of aggregation corrosion and insufficient extraction efficiency of nanoparticles, and achieves high dispersibility, increased hydrophilicity and extraction. Ability, particle size uniform effect

Active Publication Date: 2020-11-03
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

MSPE usually utilizes Fe 3 o 4 provides magnetism, however, bare Fe 3 o 4 The extraction efficiency of nanoparticles is insufficient, and irreversible aggregation and corrosion are prone to occur in complex sample matrices, so it is necessary to extract Fe 3 o 4 Nanoparticles are modified, and externally modified materials play an important role in improving selectivity and enrichment efficiency

Method used

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  • Preparation method and application of guanidine salt ionic liquid modified magnetic solid-phase extraction adsorbent
  • Preparation method and application of guanidine salt ionic liquid modified magnetic solid-phase extraction adsorbent
  • Preparation method and application of guanidine salt ionic liquid modified magnetic solid-phase extraction adsorbent

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Embodiment 1

[0039] Embodiment 1: Preparation of Fe modified by guanidinium salt ionic liquid 3 o 4 @SiO 2 -GIL Magnetic Nanocomposite

[0040] Preparation process: Dissolve 1,1,3,3-tetramethylguanidine (1mL), tetrabutylammonium bromide (0.17g), p-chlorobenzylamine (9g) and potassium carbonate (2g) in methanol (50mL ) at 60°C for 40h, then cooled to room temperature and filtered. The filtrate was evaporated in vacuo to remove the solvent, and the residue was washed three times with n-hexane, ethyl acetate and triethylamine, respectively. A small amount of water was added, followed by solid NaOH to bring the aqueous solution to pH=8. Water was removed by evaporation, and the resulting liquid was extracted with a mixed solution of ethanol:tetrahydrofuran (v / v, 1:1). The solid precipitate was removed by centrifugation and the solvent was removed by rotary evaporation. After centrifugation and evaporation, the resulting product was vacuum-dried at 60 °C to obtain a light yellow viscous l...

Embodiment 2

[0043] Embodiment 2: Preparation of Fe modified by guanidinium salt ionic liquid 3 o 4 @SiO 2 -GIL Magnetic Nanocomposite

[0044] The preparation process is shown in Figure 1(a). 1,1,3,3-tetramethylguanidine (2.5mL), tetrabutylammonium bromide (0.3g), 3-chloroethylamine hydrochloride (10g ) and potassium carbonate (6 g) were dissolved in methanol (50 mL) and refluxed at 75 °C for 20 h, then cooled to room temperature and filtered. The filtrate was evaporated in vacuo to remove the solvent, and the residue was washed three times with n-hexane, ethyl acetate and triethylamine, respectively. A small amount of water was added, followed by solid NaOH to bring the aqueous solution to pH = 8.3. Water was removed by evaporation, and the resulting liquid was extracted with a mixed solution of ethanol:tetrahydrofuran (v / v, 1:1.5). The solid precipitate was removed by centrifugation and the solvent was removed by rotary evaporation. After centrifugation and evaporation, the result...

Embodiment 3

[0047] Embodiment 3: Preparation of Fe modified by guanidinium salt ionic liquid 3 o 4 @SiO 2 -GIL Magnetic Nanocomposite

[0048] The preparation process is shown in Figure 1(a). 1,1,3,3-tetramethylguanidine (3mL), tetrabutylammonium bromide (0.1g), 3-bromopropylamine hydrochloride (11g) and Potassium carbonate (4 g) was dissolved in methanol (50 mL) and refluxed at 80 °C for 36 h, then cooled to room temperature and filtered. The filtrate was evaporated in vacuo to remove the solvent, and the residue was washed three times with n-hexane, ethyl acetate and triethylamine, respectively. A small amount of water was added, followed by solid NaOH to bring the aqueous solution to pH=9. Water was removed by evaporation, and the resulting liquid was extracted with a mixed solution of ethanol:tetrahydrofuran (v / v, 1:2). The solid precipitate was removed by centrifugation and the solvent was removed by rotary evaporation. After centrifugation and evaporation, the resulting produc...

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Abstract

The invention discloses a preparation method and application of a guanidine salt ionic liquid modified magnetic solid-phase extraction adsorbent, and belongs to the technical field of chromatographicanalysis pretreatment and environmental monitoring. The preparation method comprises the following steps: firstly, preparing amino-functionalized hexaalkyl guanidine salt ionic liquid, then coating the surface of a Fe3O4 material with SiO2 to obtain a Fe3O4@SiO2 magnetic material, and bridging Fe3O4@SiO2 with the hexaalkyl guanidine salt ionic liquid to obtain a guanidine salt ionic liquid modified magnetic nano material, namely the Fe3O4-coated SiO2-GIL nano composite material. The prepared Fe3O4@SiO2-GIL nano composite material is used for enriching PAHs in an environmental water sample by MSPE. The amino-functionalized hexaalkyl guanidine salt ionic liquid prepared by the method is short in alkyl chain and low in toxicity, the hydrophilicity of a magnetic adsorbent can be enhanced, andthe amino-functionalized hexaalkyl guanidine salt ionic liquid can be used for trace detection of PAHs in the environment in combination with liquid chromatography ultraviolet-visible spectrum detection.

Description

technical field [0001] The invention belongs to the technical field of chromatographic analysis pretreatment and environmental monitoring, and relates to a magnetic solid-phase extraction adsorbent modified by guanidinium salt ionic liquid, a preparation method and an application. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs) are a class of organic pollutants with two or more condensed aromatic hydrocarbons. They are very stable and are not easily degraded and metabolized in the human body. Therefore, you have bioaccumulation and are carcinogenic when exposed to PAHs. risk. PAHs are produced by the incomplete combustion of organic compounds, such as tree burning in natural environments and industries, as well as personal actions such as smoking and grilling. The distribution concentration of PAHs in the environment has increased with the increase of human activities, but it is still below the lowest detection limit of normal analytical techniques. I...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01J20/28B01J20/22B01J20/30G01N30/06G01N30/34G01N30/74
CPCB01J20/22B01J20/103B01J20/08B01J20/28009B01J20/281G01N30/06G01N30/34G01N30/74G01N2030/062Y02P10/20
Inventor 乔利珍于春梅孙瑞婷
Owner DALIAN UNIV OF TECH
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