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Monolithic column for capillary electrochromatography and preparation method thereof

A capillary electrochromatography and monolithic column technology, applied in the field of capillary electrochromatography monolithic column and its preparation, can solve problems such as uneven interface of stationary phase, and achieve the effects of improving column performance and simple operation

Inactive Publication Date: 2012-05-30
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem that the stationary phase interface of the monolithic column of capillary electrochromatography is not smooth, the inventor proposes a method of leaving mercury in the air, that is, using the inhalation of mercury to suppress the capillary diffusion of the reaction solution in the column to obtain a flat stationary phase interface, and using the inhalation of mercury liquid to Length controls the position of the stationary phase interface

Method used

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  • Monolithic column for capillary electrochromatography and preparation method thereof
  • Monolithic column for capillary electrochromatography and preparation method thereof
  • Monolithic column for capillary electrochromatography and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0039] (1) Configure the reaction mixture

[0040] Mix 150 μL γ-MPS and 100 μL 0.1mol / L hydrochloric acid, sonicate for 20 minutes, cool to room temperature, add 50 μL HDMA and 800 μL toluene, then add 0.02 g AIBN, sonicate for 20 minutes, let stand until the layers are separated, and take the upper layer as the reaction mixture .

[0041] (2) Put 1 mL of mercury solution in a centrifuge tube, wash the mercury with twice distilled water and absolute ethanol in turn, rinse with the reaction mixture for 3 times, then add about 1 mL of the reaction mixture to the centrifuge tube, Due to the high density of mercury, it is in the lower layer of the centrifuge tube at this time.

[0042] (3) The total length of the pretreated capillary is 32cm, and the detection window is set at 12cm, that is, the length of the empty section in the capillary is set to 12cm, and a mark is made on the outer wall of the capillary at this length. The end of the capillary away from the detection window...

Embodiment 2

[0045] (1) Configure the reaction mixture

[0046] Mix 200 μL γ-MPS and 20 μL 0.1 mol / L hydrochloric acid, sonicate for 20 minutes, cool to room temperature, add 100 μL BMA, 400 μL n-propanol and 400 μL 1,4-butanediol, then add 0.02 g AIBN, sonicate for 20 minutes, statically Set until the layers were separated, and the upper layer mixture was taken as the reaction mixture.

[0047] (2) Put 1 mL of mercury solution in a centrifuge tube, wash the mercury with twice distilled water and absolute ethanol in turn, rinse with the reaction mixture for 3 times, then add about 1 mL of the reaction mixture to the centrifuge tube, Due to the high density of mercury, it is in the lower layer of the centrifuge tube at this time.

[0048] (3) The total length of the pretreated capillary is 52 cm, and the detection window is set at 12 cm, that is, the length of the empty section in the capillary is set to 12 cm, and a mark is made on the outer wall of the capillary at this length. The end ...

Embodiment 3

[0051] (1) Configure the reaction mixture

[0052] Mix 150 μL γ-MPS and 100 μL 0.1 mol / L hydrochloric acid, sonicate for 20 min, cool to room temperature, add 50 μL lauryl methacrylate and 800 μL toluene, then add 0.02 g AIBN, sonicate for 20 min, stand until the layers are separated, and take The upper layer mixture is the reaction mixture.

[0053] (2) Put 1 mL of mercury solution in a centrifuge tube, wash the mercury with twice distilled water and absolute ethanol in turn, rinse with the reaction mixture for 3 times, then add about 1 mL of the reaction mixture to the centrifuge tube, Due to the high density of mercury, it is in the lower layer of the centrifuge tube at this time.

[0054] (3) The total length of the pretreated capillary is 45cm, and the detection window is set at 12cm, that is, the length of the empty section in the capillary is set to 12cm, and a mark is made on the outer wall of the capillary at this length. The end of the capillary away from the detec...

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Abstract

The invention discloses a monolithic column for capillary electrochromatography, which is prepared by the following method: firstly, a reaction monomer which can pre-generate a stationary phase of the monolithic column is prepared into a reaction mixture, a position which is marked on the pretreated capillary is served as an interface connecting line of a detection window and the stationary phaseof the pre-prepared monolithic column for capillary electrochromatography; the capillary sucks mercury liquid and then sucks the reaction mixture, and the interface joint of the mercury liquid and the reaction mixture and the mark of the interface connecting line are controlled to be overlapped; the reaction mixture undergoes the curing reaction, and the liquid mercury is sucked out after the reaction mixture is cured; and the monolithic column for capillary electrochromatography with the smooth stationary phase is obtained by post-treatment. The interface position of the stationary phase of the monolithic column for capillary electrochromatography provided by the invention is easy to control, the interface is easy to smooth, and the operation is simple so as to facilitate beginners to use.

Description

(1) Technical field [0001] The invention relates to a capillary electrochromatographic monolithic column and a preparation method thereof, in particular to a capillary electrochromatographic monolithic column with a flat stationary phase interface and a preparation method thereof. (2) Background technology [0002] When capillary electrochromatography monolithic column is used for capillary electrophoresis-ultraviolet detection, it needs to have a light-transmitting detection window with a length of about 3mm, that is, the inside and outside of the capillary need to be in a light-transmitting state. For the outside of the capillary, the polyimide coating is generally removed by ablation, concentrated sulfuric acid corrosion, and scraping with a blade; it is difficult to make the inside of the capillary transparent, mainly by leaving the detection window inside the capillary blank or removing it. Stationary phase at the detection window. There are three main methods reported...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/60G01N30/56
Inventor 王园朝吴琼蔡诚
Owner HANGZHOU NORMAL UNIVERSITY
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