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Laminar double-metal hydroxide modified capillary electrochromatography column as well as preparation method and application thereof

A capillary electrochromatography, layered bimetallic technology, applied in chemical instruments and methods, separation methods, other chemical processes, etc. Simple, good stability and reproducibility, good separation results

Active Publication Date: 2017-12-12
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, as an inorganic material with excellent properties, layered double metal hydroxides are rarely used in the field of capillary electrochromatography, mainly due to the existing fixation methods such as gel-sol coating, colloid deposition, Electrostatic adsorption methods cannot achieve stable fixation of layered double metal hydroxides on the inner wall of the capillary, which limits its application in capillary electrochromatography

Method used

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  • Laminar double-metal hydroxide modified capillary electrochromatography column as well as preparation method and application thereof
  • Laminar double-metal hydroxide modified capillary electrochromatography column as well as preparation method and application thereof
  • Laminar double-metal hydroxide modified capillary electrochromatography column as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Take a 50 cm long fused silica capillary (50 µm i.d. × 375 µm o.d.), and wash with NaOH, H 2 O, HCl and H 2 O for preprocessing.

[0030] 2) Weigh 20 mg of dopamine, dissolve it in 10 mmol / L Tris-HCl buffer, adjust the pH to 8.5, shake the pre-oxidized solution to light brown.

[0031] 3) The preoxidized dopamine solution was passed through the capillary pretreated in step 1), the flow rate was 0.03mL / h, and the modification time was 20 h. After washing with water, the solvent was blown off with nitrogen gas, and dried in an oven to obtain a polydopamine-modified capillary column.

[0032] 4) 0.232 g of cobalt nitrate hexahydrate, 0.152 g of aluminum nitrate nonahydrate and 0.168 g of urea were weighed and dissolved in 5 mL of pure water in turn to obtain a reaction solution of layered double metal hydroxide. Then pass this reaction solution into the polydopamine-modified capillary tube obtained after step 3), the two ends of the capillary tube are connected and s...

Embodiment 2

[0034] 1) Take a 50cm long fused silica capillary (50 µm i.d. × 375 µm o.d.), and wash with NaOH, H 2 O, HCl and H 2 O for preprocessing.

[0035] 2) Weigh 20 mg of dopamine, dissolve it in 10 mmol / L Tris-HCl buffer, adjust the pH to 9, shake the pre-oxidized solution to light brown.

[0036] 3) Pass the preoxidized dopamine solution through the capillary pretreated in step 1) at a flow rate of 0.03mL / h and a modification time of 12 h. After washing with water, the solvent was blown off with nitrogen gas, and dried in an oven. Repeat the modification once more to obtain a capillary column with a thicker polydopamine modification layer.

[0037] 4) 0.464 g of cobalt nitrate hexahydrate, 0.304 g of aluminum nitrate nonahydrate and 0.336 g of urea were weighed and dissolved in 5 mL of pure water in turn to obtain a reaction solution of layered double metal hydroxide. Then the reaction solution was passed into the polydopamine-modified capillary column obtained after step 3), ...

Embodiment 3

[0039] 1) Take a 50cm long fused silica capillary (50 µm i.d. × 375 µm o.d.), and wash with NaOH, H 2 O, HCl and H 2 O for preprocessing.

[0040] 2) Weigh 20 mg of dopamine, dissolve it in 10 mmol / L Tris-HCl buffer, adjust the pH to 9, shake the pre-oxidized solution to light brown.

[0041] 3) The preoxidized dopamine solution was passed through the capillary pretreated in step 1), the flow rate was 0.03mL / h, and the modification time was 20 h. After washing with water, the solvent was blown off with nitrogen gas, and dried in an oven. Repeat the modification once more to obtain a capillary column with a thicker polydopamine modification layer.

[0042] 4) 0.058 g of cobalt nitrate hexahydrate, 0.038 g of aluminum nitrate nonahydrate and 0.042 g of urea were weighed and dissolved in 5 mL of water in turn to obtain a reaction solution of layered double metal hydroxide. Then the reaction solution was passed into the polydopamine-modified capillary column obtained after step ...

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Abstract

The invention discloses a laminar double-metal hydroxide modified capillary electrochromatography column as well as a preparation method and application thereof and belongs to the field of capillary electrochromatography columns. Laminar double-metal hydroxide has the characteristics of strong anion exchange effect, large specific surface area, porosity and the like so that the laminar double-metal hydroxide is widely applied to fields including adsorption and extraction of substances and has a good chromatographic property. A proper fixing method is lacked so that the application of the laminar double-metal hydroxide to the field of capillary electrochromatography is limited. A polydopamine modification technology is adopted so that the fixation of the laminar double-metal hydroxide on a capillary inner wall is successfully realized and the application of the laminar double-metal hydroxide to the capillary electrochromatography is realized. The preparation method of the laminar double-metal hydroxide modified capillary electrochromatography column has a simple technology and is easy to operate; the prepared capillary electrochromatography column has relatively good stability and repeatability. The laminar double-metal hydroxide modified capillary electrochromatography column prepared by the preparation method has a very good separation effect on aromatic benzene series substances and phenolic substances.

Description

technical field [0001] The invention belongs to the field of capillary electrochromatographic columns, and in particular relates to a novel capillary electrochromatographic column modified by layered double metal hydroxides (CoAl-LDHs) and its preparation method and application. Background technique [0002] Capillary electrochromatography is a miniaturized separation technology that combines capillary electrophoresis and high performance liquid chromatography with a capillary column containing a chromatographic stationary phase as the separation column. Due to its dual separation mechanism of capillary electrophoresis and high performance liquid chromatography, it has the characteristics of high efficiency, high selectivity, rapidity, and less sample consumption. Among them, capillary column technology is a key link in capillary electrochromatography. Therefore, the preparation of new capillary column with excellent separation performance is of great significance to the dev...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01J20/30B01D15/20B01D15/22B01D15/38
Inventor 陈子林余欣虹周韦
Owner WUHAN UNIV
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