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Microminiaturized liquid phase chromatography separating method

A separation method and liquid chromatography technology, applied in the field of liquid chromatography separation, can solve the problems of lower detection sensitivity, limited application range, large amount of adsorbent, etc., and achieve the effects of improved detection sensitivity, convenient use, and fast separation speed

Inactive Publication Date: 2008-07-30
夏之宁 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the amount of adsorbent used in the thin-layer chromatography of the prior art is large, and the adsorbent (usually silica gel or aluminum oxide) with larger particle size and wider particle size range is generally used, resulting in low column efficiency and limiting its application range.
At the same time, in thin-layer chromatography, there is a serious lateral broadening of the sample spot, which reduces the detection sensitivity
Moreover, thin-layer chromatography, as a flat chromatography, is difficult to further miniaturize

Method used

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  • Microminiaturized liquid phase chromatography separating method
  • Microminiaturized liquid phase chromatography separating method
  • Microminiaturized liquid phase chromatography separating method

Examples

Experimental program
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Embodiment 1

[0020] Column preparation: The packed capillary column was prepared by the homogenization method. Take a quartz capillary 1 with an inner diameter of 0.05-1.0 mm and a length of about 30 cm, knock a small piece of silica gel (about 2 mm in length, 5 μm in diameter) into one port, and sinter at about 600 ° C for about 10 seconds to make a plug (this plug can be through the solvent and not through the packing); burn off the capillary coating entirely. Then, silica gel or ODS silica gel with a particle diameter of 3 μm or 5 μm is used as a filler 2 and dissolved in acetone to prepare a homogenate with a concentration of about 10%, and placed in a homogenate pool. Connect the capillary at one end of the homogenate tank and the high-pressure pump at the other end. Increase the pressure of the high-pressure pump to 30Mpa, press the homogenate into the capillary, and gradually reduce the pressure to normal pressure after the filler is filled with the capillary. Remove the capillary a...

Embodiment 2

[0029] Preparation of filled microchannels: firstly, glass is used as a raw material, and processed into a chip 8 with a size of 50mm×30mm×3mm. Then process three microchannels 9 on the chip, each microchannel has a width of about 0.1-1 mm, a depth of 0.05-0.5 mm, and a length of about 3 cm. Then bond (using thermal bonds and or chemical bonds and) the cover sheet 11 with 6 small holes 10 with a diameter of about 5 mm. The positions of the 6 small holes on the cover sheet are respectively aligned with the 6 ports at the two ends of the 3 microchannels.

[0030] The chip microchannel is filled by in-situ polymerization. Its steps are: after the bonding and completion, the prepared polymerization solution (polymer monomer butyl acrylate 23.6%, crosslinking agent ethylene glycol dimethacrylate 16%, azobisisobutyronitrile 0.4%, ethanol 30%, methanol 30%) is dropped into the small hole at one end of each microchannel on the chip, and the solution fills the microchannel under the a...

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Abstract

The microminiaturized liquid chromatographic separation method features that the method adopts dry filled capillary column or filled micro channel as separating channel and capillary effect as driving force in realizing sample separation. The present invention needs no additional driving device, and has the features of low cost, fast speed, high separation efficiency, high detection sensitivity and micro size.

Description

technical field [0001] The invention relates to a liquid chromatography separation method, in particular to a miniaturized liquid chromatography separation method. Background technique [0002] Since Izmailor and Schraiber first used thin-layer chromatography to separate the components in various plant tinctures in 1938, thin-layer chromatography (TLC) has played an important role in separation analysis. In thin-layer chromatography, the adsorbent is coated on the thin-layer plate, and the thin-layer plate is immersed in the developer after the sample is applied. The sample components are developed on the thin-layer plate driven by capillary action, and the separation is achieved. Thin-layer chromatography has the advantages of simple equipment, convenient operation, fast separation speed, and flexible and diverse detection methods. In particular, thin-layer chromatography is driven by capillary action - no external driving force is required, so it can be called "self-drive...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/84G01N30/02B01D15/08
Inventor 夏之宁喻彦林肖尚友李鸿乂
Owner 夏之宁