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Silica gel monolithic column modified by cyclodextrin modified nanocrystalline iron oxide

A silica monolithic column and nano iron oxide technology, applied in the preparation of organic compounds, organic chemistry, other chemical processes, etc., to achieve the effect of good reproducibility, improved separation effect, stable property and structure

Inactive Publication Date: 2015-04-15
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the use of cyclodextrin-modified nano-iron oxides in silica monolithic columns

Method used

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  • Silica gel monolithic column modified by cyclodextrin modified nanocrystalline iron oxide
  • Silica gel monolithic column modified by cyclodextrin modified nanocrystalline iron oxide
  • Silica gel monolithic column modified by cyclodextrin modified nanocrystalline iron oxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Prepare the contents of polyethylene glycol, urea, tetramethoxysilane, and γ-glycidyl etheroxypropyltrimethoxysilane according to the following data:

[0029] Column A: 200 mg polyethylene glycol, 310 mg urea.

[0030] Column B: 180 mg polyethylene glycol, 310 mg urea.

[0031] Column C: 160 mg polyethylene glycol, 370 mg urea.

[0032] Column D: 160 mg polyethylene glycol, 250 mg urea.

[0033] Column E: 160 mg polyethylene glycol, 310 mg urea.

[0034] It was dissolved in 2.0 mL of 0.01 mol / L acetic acid aqueous solution, and then 720 μL of TMOS and 800 μL of γ-GPTMS were added dropwise, and reacted in an ice bath at 0°C for 1 hour to obtain a transparent and uniform sol mixture. Use a syringe to manually inject the pretreated capillary to an appropriate length, seal both ends of the capillary, react in a water bath at 55°C for 12 hours, and rinse with secondary water and methanol respectively. Using acetonitrile:triethylamine phosphate buffer (5mmol / L, pH 7.0) as...

Embodiment 2

[0036] Cyclodextrin modified nano iron oxide is added according to the following data:

[0037] Column A: 6mg cyclodextrin modified nano iron oxide.

[0038] Column B: 4 mg cyclodextrin-modified nano iron oxide.

[0039] Column C: 2 mg of cyclodextrin-modified nano iron oxide.

[0040] Dissolve it in 1mL of mixed solution (0.1M0.1M sodium hydroxide solution:methanol: 1:1, volume ratio), sonicate for 5min, inject it into the prepared silica gel monolithic column, and place it in a water bath at 65°C for 12h. Rinse with secondary water and methanol respectively. Acetonitrile: triethylamine phosphate buffer (5mmol / L, pH 3.0) was used as the mobile phase of 90:10, the separation voltage was -20kV, the detection wavelength was 214nm, the flow rate was 0.1mL / min, and the pressure was 0.8MPa.

Embodiment 3

[0042] Cyclodextrin-modified nano-iron oxide-modified silica monolithic column for separation of phenolic compounds.

[0043] Apply the cyclodextrin-modified nano-iron oxide-modified silica monolithic column of the present invention (inner diameter 75 μm, total length 55 cm, effective length 35 cm), acetonitrile: triethylamine phosphate buffer (pH 3.0, 5 mmol / L) with a flow rate of 98:2 Phase, separation voltage -20kV, detection wavelength 214nm, flow rate 0.1mL / min, pressure 0.8MPa, using toluene as a marker, such as image 3 shown.

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Abstract

The invention discloses a silica gel monolithic column modified by cyclodextrin modified nanocrystalline iron oxide and a preparation method and application of the silica gel monolithic column, belonging to the technical field of chromatography. The preparation method comprises the following steps: (1) pre-processing a capillary tube; (2) preparing a silica gel monolithic column bed; and (3) modifying the silica gel monolithic column bed. The silica gel monolithic column modified by the cyclodextrin modified nanocrystalline iron oxide has such advantages of a nanometer material, as small grain size and large specific area; the problems that the operation of filling a traditional packing column is complex and tedious and the bubbles are produced due to a sintered plug are solved, and the defect that an open tubular column is low in capacity and small in phase ratio is overcome. The silica gel monolithic column is stable in property and good in reproducibility, and can be used in a relatively wide pH range, the electroosmotic flow can be controlled by regulating the pH of a flow phase, and the phenol substances can be well separated from aniline substances.

Description

technical field [0001] The invention belongs to the technical field of capillary chromatographic columns, and in particular relates to a cyclodextrin-modified nano-iron oxide-modified silica monolithic column and a preparation method and application thereof. Background technique [0002] Capillary electrochromatography is an efficient and rapid new micro-column separation method developed on the basis of electrophoresis technology and high performance liquid chromatography in recent years. As an important part of electrochromatographic separation technology, CEC columns can be divided into open-tubular columns, packed columns and monolithic columns. The capillary monolithic column overcomes the shortcomings of open-tubular columns, and avoids the need to make plugs for packed columns. It has the advantages of simple preparation, good permeability, and high column efficiency. [0003] Fe 3 o 4 Magnetic nanoparticles are a class of intelligent nano-magnetic materials, which...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/20B01J20/30C07C37/82C07C39/04C07C39/08C07C39/10C07C209/86C07C211/52C07C211/58C07C211/50
Inventor 吕海霞易姣姣秦文菲谢增鸿
Owner FUZHOU UNIV
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