Magnetic fullerene nano-material and application thereof to solid-phase extraction

A nanomaterial, fullerene technology, applied in other chemical processes, color/spectral characteristic measurement, alkali metal oxide/hydroxide, etc., can solve the problem of not being able to maintain magnetism, and achieve easy elution and strong adsorption Effect

Active Publication Date: 2017-09-26
YANGZHOU POLYTECHNIC INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The particles are superparamagnetic, meaning they are easily attracted to a magnet, but cannot remain magnetic after the field is removed

Method used

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  • Magnetic fullerene nano-material and application thereof to solid-phase extraction
  • Magnetic fullerene nano-material and application thereof to solid-phase extraction
  • Magnetic fullerene nano-material and application thereof to solid-phase extraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 200mL distilled water, add 0.2mmol C 60 Fullerene, 0.4mmol ferrous sulfate heptahydrate, 0.8mmol anhydrous ferric chloride, after feeding nitrogen and stirring for 15 minutes, heating to reflux temperature, keeping reflux for 20-30 minutes, cooling to 85-90°C, maintaining the temperature (85-90°C), add ammonia water (6mL) dropwise, continue to stir for 1-1.5h, the reaction solution is in a black turbid state, it naturally drops to room temperature, and after standing for 0.5h, it is adsorbed and separated by a magnet to obtain a black solid; After washing with distilled water for 3-5 times, vacuum-dry at 60°C for 12 hours to obtain a black solid powder, which is Magnetic C 60 Fullerene nanomaterials (abbreviated as C 60 -Fe 3 o 4 , figure 1 , hereinafter referred to as product A); the distilled water used in the present embodiment is the distilled water after ultrasonic.

Embodiment 2

[0026] Take 100mL distilled water, add 0.1mmol C 60Fullerene, 0.2mmol of ferrous sulfate heptahydrate, 0.4mmol of anhydrous ferric chloride, after argon gas stirring for 20 minutes, heating to reflux temperature, keeping reflux for 20-30 minutes, cooling to 85-90°C, maintaining Add ammonia water (5mL) dropwise at this temperature (85-90°C), continue to stir and react for 1-1.5h, the reaction solution is in a black and turbid state, it naturally drops to room temperature, and after standing for 0.5h, it is adsorbed and separated by a magnet to obtain a black solid; After washing with distilled water for 3-5 times, vacuum-dry at 60°C for 24 hours to obtain a black solid powder, which is Magnetic C 60 Fullerene nanomaterials (abbreviated as C 60 -Fe 3 o 4 , SEM image with figure 1 Consistent, hereinafter referred to as product B); The distilled water used in the present embodiment is the distilled water after ultrasonic.

Embodiment 3

[0028] Take 200mL distilled water, add 0.2mmol graphene, 0.4mmol ferrous sulfate heptahydrate, 0.8mmol anhydrous ferric chloride, stir for 15 minutes with nitrogen gas, heat to reflux temperature, keep reflux for 20-30 minutes, then cool down to 85 -90°C, maintain the temperature (85-90°C) and add ammonia water (6mL) dropwise, continue to stir for 1-1.5h, the reaction solution is black and turbid, naturally lowered to room temperature, after standing for 0.5h, use a magnet to separate , to obtain a black solid; after washing 3-5 times with distilled water, obtain a black solid powder at 60°C for 12h in vacuum, which is a magnetic graphene material (hereinafter referred to as product C); the distilled water used in the present embodiment is after ultrasonic distilled water.

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Abstract

The invention belongs to the field of materials and medicine analysis and in particular relates to a magnetic fullerene nano-material and application thereof to solid-phase extraction. A preparation method of the magnetic C60 fullerene nano-material provided by the invention comprises the following steps: (1) taking a proper amount of distilled water and adding C60 fullerene, ferrous sulfate heptahydrate and anhydrous ferric chloride; introducing nitrogen gas or argon gas and stirring for 15min to 20min; heating to refluxing temperature; after keeping refluxing for 20min to 30min, cooling to 85 DEG C to 90 DEG C; keeping the temperature (85 DEG C to 90 DEG C) and dropwise adding ammonia water; continually stirring and reacting for 1h to 1.5h, wherein a reaction solution is at a black muddy state; naturally cooling to room temperature; after standing for 0.5h, adsorbing and separating by utilizing a magnet to obtain a black solid; (2) after washing the black solid obtained by step (1) with distilled water for 3 to 5 times, drying for 12h to 24h at 60 DEG C in vacuum to obtain black solid powder, namely the magnetic C60 fullerene nano-material.

Description

technical field [0001] The invention belongs to the field of material and drug analysis, in particular to a magnetic fullerene nanometer material and its application in solid phase extraction. Background technique [0002] Because the drug concentration in the organism, especially the drug concentration in the serum is directly related to the drug effect. Therefore, from the aspects of clinical application and drug safety evaluation, it is necessary to establish a simple, sensitive and accurate analytical method for detecting the content of anegliptin in biological fluids and drugs. At present, the widely used drug analysis methods include high performance liquid chromatography, thin layer chromatography, ion exchange chromatography and so on. At present, there are few literature reports on the determination method of anegliptin content, but there is no report on the determination of anegliptin content by ultraviolet-visible spectrophotometry. [0003] In drug analysis, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/28B01J20/30B01D15/08G01N21/33
CPCB01D15/08B01J20/06B01J20/20B01J20/28009G01N21/33
Inventor 龚爱琴钱琛王元有徐洁
Owner YANGZHOU POLYTECHNIC INST
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