Preparation and application method of combined nano magnetic separating medium

A separation medium and nano-magnetic technology, applied in chemical instruments and methods, alkali metal compounds, other chemical processes, etc., can solve the problems of fixed phase type limitation, limited flexibility, preparation difficulty, etc., and achieve stable phase structure and easy operation The effect of convenience and simple preparation method

Inactive Publication Date: 2019-02-26
APPLE FLAVOR & FRAGRANCE GRP
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Problems solved by technology

However, this method fixes the three stationary phases according to a specific ratio, not only the type of stationary phase is strictly limited, but also the ratio is fixed, which limits its flexibility for method development
[0005] The preparation of multifunctional magnetic nano-separation media and its application in the field of separation, analysis and detection is one of the research hotspots in the field of analytical chemistry. It is necessary to combine multiple functional groups on the same nanoparticle, which brings great difficulty to the preparation.

Method used

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  • Preparation and application method of combined nano magnetic separating medium
  • Preparation and application method of combined nano magnetic separating medium

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preparation example Construction

[0030] 1. Preparation of magnetic nanoparticle matrix:

[0031] The magnetic magnetic nanoparticle matrix can be obtained by direct purchase or self-preparation. The general preparation method is to firstly prepare magnetic iron oxide nanoparticles as the core of its matrix, and further coat the porous silica shell on its surface.

[0032] Prepare magnetic iron oxide nanoparticles by solvothermal method, measure 100mL of ethylene glycol and place in a 250mL three-neck flask, add 2.7g of ferric chloride hexahydrate, after ultrasonication for 10min, add 7.2g of anhydrous sodium acetate, and mechanically stir for 30min , transfer the mixed homogenate to a stainless steel autoclave lined with polytetrafluoroethylene, and react in an oven at 200°C for 8h. Afterwards, with the assistance of an external magnetic field, the magnetic nanomatrix Fe was washed with ethanol and pure water respectively and collected. 3 o 4 , dried overnight at 60°C to obtain magnetic iron oxide nanopart...

Embodiment 2

[0053] 1) Prepare magnetic iron oxide nanoparticles by solvothermal method, measure 100mL of ethylene glycol and put it in a 250mL three-necked flask, add 2.7g of ferric chloride hexahydrate, after ultrasonication for 10min, add 7.2g of anhydrous sodium acetate, and mechanically stir After 30 minutes, the mixed homogenate was transferred to a stainless steel autoclave lined with polytetrafluoroethylene, and reacted in an oven at 200°C for 8 hours. Afterwards, with the assistance of an external magnetic field, the magnetic nanomatrix Fe was washed with ethanol and pure water respectively and collected. 3 o 4 , dried overnight at 60°C to obtain magnetic iron oxide nanoparticles.

[0054] 2) Weigh 150mg of the above-mentioned Fe 3 o 4 The particles were evenly dispersed in a mixed solution of 160mL ethanol, 40mL water and 2mL ammonia water, sonicated for 30min, 1.5mL TEOS was added dropwise, and mechanically stirred at room temperature for 8h. Magnetic separation, followed by...

Embodiment 3

[0062] Same as Example 1, the difference is the preparation of functionalized magnetic nano-separation medium in step 3: get 50 of the above-mentioned magnetic nano-material Fe 3 o 4 @SiO 2 @PGMA-NH2 was dispersed in 80 mL of ACN solution containing 60 mmol L-1 2,4,6-collidine. After passing nitrogen gas for 10 minutes, add 800 μL phosphorus oxychloride. Under nitrogen protection, stir at room temperature for 12h. The obtained material is washed with acetonitrile and water, and dried at 50° C. to obtain a magnetic nanometer material for enrichment and separation of selective phosphopeptides in dispersed biological samples. see figure 2 .

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Abstract

The invention discloses preparation and application method of a combined nano magnetic separating medium. Nano magnetic separating mediums with different characteristics are combined so as to enrich and separate components with different polarity characteristics in a complicated system at a time. A magnetic nano material matrix with a porous structure or a pore-free structure is modified to prepare nano magnetic separating mediums with different characteristics. Different kinds of separating materials are combined to form a mixed separating medium with special selectivity, and the separating medium has high adsorption selectivity and adsorption capacity on different target components. Through a magnetic separation technology, the nano magnetic separating medium with adsorbed target components is separated from the matrix of a complicated sample, and after heat desorption, quantitative analysis and qualitative analysis are performed by GC / MS. The provided combined nano magnetic separating medium can high-selectively and efficiently collect and enrich target compounds, the preprocessing method is convenient and efficient, the stability of the method is good, and the method can be conveniently and effectively adjusted so as to enrich specific target components in different samples.

Description

technical field [0001] The invention relates to the technical field of sample pretreatment and chromatographic analysis in analytical chemistry, and specifically relates to the preparation and application method of a combined nanometer magnetic separation medium. Background technique [0002] For the development of analytical methods for volatile components with specific structures in complex systems, there are already a variety of techniques to choose from, including extraction, adsorption, and so on. For the simultaneous enrichment and separation of multiple characteristic components with different structures and polarities in complex sample matrices, sample pretreatment technology has always been a hot research direction for analytical chemists. [0003] In recent years, the application of magnetic nano-separation materials in many fields such as biology and environment has attracted extensive attention, and has been successfully applied to the research of proteins and me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/32
CPCB01J20/06B01J20/103B01J20/223B01J20/264B01J20/28009B01J20/3278
Inventor 庄伟强茅富燕康维君张维冰
Owner APPLE FLAVOR & FRAGRANCE GRP
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