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Preparation method of open tubular capillary electrochromatographic column

A capillary electrochromatography, capillary technology, applied in the field of chromatography, can solve the problems of difficult chromatographic separation, lack of chemically reactive groups, etc.

Active Publication Date: 2013-07-10
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the irregular particle size and shape of hydroxyapatite, it is rarely used in micro-chromatographic separation. Therefore, it is necessary to develop a preparation method of hydroxyapatite nanomaterials with uniform particle size and controllable morphology for application in micro-chromatography. System separation
[0005] Since hydroxyapatite is an inorganic material and lacks active groups for chemical reactions, it is difficult to fix it on the inner wall of the capillary for chromatographic separation

Method used

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  • Preparation method of open tubular capillary electrochromatographic column
  • Preparation method of open tubular capillary electrochromatographic column

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Cut off a 60cm long quartz capillary (50 μm i.d. × 375 μm o.d.), rinse with 1M NaOH for 2 hours, H 2 Rinse with O for half an hour, blow dry with nitrogen; weigh 10 mg of dopamine and dissolve in 5 mL of 10 mM Tris buffer, adjust the pH to 8.5, shake the prepared dopamine solution for 5 minutes, and then continuously inject it at a flow rate of 0.01 mL / min Put the pretreated capillary in water for 20 hours, wash with water, and blow dry with nitrogen to obtain a capillary whose inner wall is modified with a polydopamine coating; repeat the polydopamine modification step to obtain a capillary whose inner wall is modified with a multi-layer polydopamine coating. Then pass 1.5 times of simulated body fluid into the above-mentioned capillary tube containing multi-layer polydopamine coating, seal both ends of the capillary tube, put it in a 37°C water bath for incubation for 14 days, take it out, wash it with water, and obtain an open-tube capillary column of hydroxyapatite ...

Embodiment 2

[0023] Cut off a 60cm long quartz capillary (50 μm i.d. × 375 μm o.d.), rinse with 1M NaOH for 2 hours, H 2 Rinse with O for half an hour, blow dry with nitrogen; weigh 10 mg of dopamine and dissolve in 5 mL of 10 mM Tris buffer, adjust the pH value to 8.5, shake the prepared dopamine solution for 5 minutes, and pass it into the pre- Put the treated capillary in water for 20 hours, wash with water, blow dry with nitrogen, and obtain a capillary with polydopamine coating on the inner wall; pass 1.5 times simulated body fluid into the above capillary containing polydopamine coating, seal both ends of the capillary, and put After incubating in a water bath at 37° C. for 14 days, it was taken out and washed with water to obtain an open-tube capillary column of hydroxyapatite.

Embodiment 3

[0025] Cut off a 60cm long quartz capillary (50 μm i.d. × 375 μm o.d.), rinse with 1M NaOH for 2 hours, H 2 Rinse with O for half an hour, blow dry with nitrogen; weigh 10 mg of dopamine and dissolve in 5 mL of 10 mM Tris buffer, adjust the pH to 8.5, shake the prepared dopamine solution for 5 minutes, and then continuously inject it at a flow rate of 0.01 mL / min Put the pretreated capillary in water for 20 hours, wash with water, and blow dry with nitrogen to obtain a capillary whose inner wall is modified with a polydopamine coating; repeat the polydopamine modification step to obtain a capillary whose inner wall is modified with a multi-layer polydopamine coating. Then pass 1.5 times of simulated body fluid into the above-mentioned capillary containing multi-layer polydopamine coating, seal both ends of the capillary, put it in a 37°C water bath for incubation for 7 days, take it out, wash it with water, and obtain an open-tube capillary column of hydroxyapatite .

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Abstract

The invention relates to a preparation method of a novel open tubular capillary electrochromatographic column for fixing hydroxyapatite as a stationary phase by adopting a bio-ore physical-chemical method. The hydroxyapatite is used as an inorganic material, and is short of active groups, thereby being difficultly fixed on the wall of a capillary tube for capillary electrochromatographic separation. The preparation method comprises the steps of: introducing a pre-oxidized dopamine solution into a preprocessed capillary tube, forming a polydopamine coating on the inner wall of the capillary tube; and introducing a 1.5-time simulated body fluid into the capillary tube modified by polydopamine, placing the capillary tube in a water bath kettle being 37 DEG C for incubation for two weeks, and growing a hydroxyapatite crystal with a nano structure on the inner wall of the capillary tube. The preparation method provided by the invention is simple in process, easy to operate and low in cost; and the whole preparation process is carried out in a water solution without polluting the environment. A hydroxyapatite open tubular column prepared by adopting the preparation method has a good separation effect on a neutral compound, an alkali compound and an acidic compound.

Description

[0001] technical field [0002] The invention belongs to the technical field of chromatography and relates to a preparation method of an open-tube capillary electrochromatographic column. Background technique [0003] Capillary electrochromatography is a new type of efficient and rapid separation technology. It is developed by neutralizing the advantages of high efficiency of capillary electrophoresis and high selectivity of high performance liquid chromatography, and has the advantages of fast analysis speed, high column efficiency, and less consumption of samples and solvents. The core of capillary electrochromatography is the capillary electrochromatographic column. Therefore, the preparation of electrochromatographic columns with high column efficiency and good separation effect is the focus of research. [0004] Hydroxyapatite is the main mineral component of human bones and teeth. Due to its good biocompatibility, osteoconductivity and bioactivity, it is considered ...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01J20/28B01J20/30
Inventor 陈子林张娟
Owner WUHAN UNIV
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