Magnetic mesoporous titanium dioxide core-shell type compound microsphere as well as preparation method and application thereof

A technology of mesoporous titanium dioxide and composite microspheres is applied in the preparation of microspheres, microcapsule preparations, magnetic properties of inorganic materials, etc. It can solve the problems of complicated separation and low purity, and achieve uniform particle size distribution, good effect and regular structure. Effect

Inactive Publication Date: 2012-08-01
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current methods for preparing mesoporous titania all need to generate pores by using a method similar to the template method, and this will make the purity of the formed mesoporous titania microspheres not high, and will cause a decrease in selectivity due to the presence of other impurities. ; In addition, these mesoporous titanium dioxide microspheres do not contain magnetic cores, so they require a high centrifugal speed for separation, which is relatively cumbersome and may cause some large molecular weight proteins or peptides to co-precipitate together in the process

Method used

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  • Magnetic mesoporous titanium dioxide core-shell type compound microsphere as well as preparation method and application thereof
  • Magnetic mesoporous titanium dioxide core-shell type compound microsphere as well as preparation method and application thereof
  • Magnetic mesoporous titanium dioxide core-shell type compound microsphere as well as preparation method and application thereof

Examples

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Embodiment 1

[0022] Example 1: The magnetic core is about 300nm, the thickness of the titanium dioxide shell is about 50nm, and the core-shell Fe with a pore diameter of about 20nm 3 o 4 mO 2 Preparation of Microspheres and Their Application to the Selective Isolation of Phosphopeptides at Very Low Levels in Biological Samples

[0023] 1. Preparation of citric acid-stabilized magnetic clusters

[0024] 1.2g ferric chloride hexahydrate (FeCl 3 ·6H 2 O), 2.4g ammonium acetate (NH 4 Ac), after dissolving 0.3g citric acid in 70mL ethylene glycol, put it into a 150mL three-neck flask, then raise the temperature to 140°C, keep it warm for 1 hour, then transfer the liquid in the flask to a 100mL Teflon-lined In a high-pressure reaction kettle, put the reaction kettle into an oven at 200°C for 24 hours, take it out, and cool it to room temperature with tap water. The product was separated by magnetic separation, washed with absolute ethanol to remove unreacted reactants, and finally the prod...

Embodiment 2

[0031] Example 2: a core-shell Fe with a magnetic core of about 150 nm, a titanium dioxide shell thickness of about 50 nm, and a pore diameter of about 20 nm 3 o 4 mO 2 Preparation of Microspheres and Their Application to the Selective Isolation of Phosphopeptides at Very Low Levels in Biological Samples

[0032] 1. The preparation of citric acid-stabilized magnetic clusters is the same as described in Example 1-1. The difference is that the reaction temperature in the flask was changed from 140°C to 20°C.

[0033] 2. Core-shell Fe 3 o 4 TiO 2 The preparation is the same as described in Example 1-2. The difference is that the amount of tetrabutyl titanate is changed from 1 mL to 0.6 mL.

[0034] 3. Core-shell Fe 3 o 4 mO 2 The preparation is the same as described in Examples 1-3.

[0035] 4. The test method for selectively separating extremely low-level phosphopeptides in biological samples is the same as that described in Examples 1-4. In this example, the selecti...

Embodiment 3

[0036] Example 3: a core-shell Fe with a magnetic core of about 300nm, a titanium dioxide shell thickness of about 100nm, and a pore diameter of about 20nm 3 o 4 mO 2 Preparation of Microspheres and Their Application to the Selective Isolation of Phosphopeptides at Very Low Levels in Biological Samples

[0037] 1. The preparation of citric acid-stabilized magnetic clusters is the same as described in Example 1-1.

[0038] 2. Core-shell Fe 3 o 4 TiO 2 The preparation is the same as described in Example 1-2. The difference is that the amount of tetrabutyl titanate is changed from 1 mL to 2 mL.

[0039] 3. Core-shell Fe 3 o 4 mO 2 The preparation is the same as described in Examples 1-3.

[0040] 4. The test method for selectively separating extremely low-level phosphopeptides in biological samples is the same as that described in Examples 1-4. In this example, the selectivity of the microspheres for phosphopeptides is the same as Example 1, the magnetic separation spe...

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Abstract

The invention belongs to the technical field of functional material and particularly relates to a magnetic mesoporous titanium dioxide core-shell type compound microsphere as well as a preparation method and applications thereof. The core-shell type compound microsphere takes a ferroferric oxide nano particle cluster as the core and takes mesoporous titanium dioxide with high crystallinity as the shell. The preparation method comprises the following steps: firstly, preparing the ferroferric oxide nano particle cluster with stable citric acid, secondly, wrapping the surface of the cluster with an amorphous titanium dioxide shell through a sol-gel method, and finally, obtaining the magnetic mesoporous titanium dioxide core-shell type compound microsphere through hydro-thermal treatment. By being provided with the mesoporous titanium dioxide shell with high crystallinity, the compound microsphere has the characteristics of high selectivity, high enrichment capacity, high sensitivity and high recovery rate to phosphoeptide; and since a magnetic core exists, the microsphere enriched in phosphoeptide can be separated by magnetism quickly and very conveniently. The method provided by the invention has the advantages that the operation is simple, the process is controllable, and the prepared compound microsphere can be used for analyzing and identifying phosphoeptide with ultra low concentration in a biological sample.

Description

technical field [0001] The invention belongs to the technical field of functional materials, and in particular relates to a magnetic mesoporous titanium dioxide core-shell composite microsphere and a preparation method and application thereof. Background technique [0002] In recent years, multifunctional magnetic composite microspheres have attracted widespread attention. Since the magnetic composite microspheres have both the magnetism of inorganic magnetic substances and the functionality of surface substances, they can quickly, conveniently and efficiently separate target bioactive molecules under the action of a magnetic field, thus being used in cell separation, separation and purification of proteins and peptides, Targeted drug delivery and other fields have good application prospects. From the perspective of application, for the separation and purification of proteins and peptides, ideal magnetic microspheres should have a regular core-shell structure, rich function...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02H01F1/01
Inventor 汪长春马万福陆豪杰张莹
Owner FUDAN UNIV
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