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Method for preparing molecular imprinting solid-phase extraction film in separation capillary

A separation capillary, solid phase extraction membrane technology, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the problem of large back pressure, dead volume, difficult to fill and fix polymer particles, etc. problems, to achieve the effect of long service life, reduced dosage, and improved measurement sensitivity

Inactive Publication Date: 2013-02-06
CHENGDU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has problems such as dead volume caused by the interface, difficulty in filling and fixing polymer particles, and large back pressure.

Method used

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  • Method for preparing molecular imprinting solid-phase extraction film in separation capillary

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Experimental program
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Effect test

Embodiment 1

[0023] The polymerization solution was 0.05 mmol of methyltestosterone, 0.2 mmol of functional monomer methacrylic acid, 1 mmol of ethylene glycol dimethacrylate and 0.06 mmol of initiator azobisisobutyronitrile (AIBN) dissolved in 3 mL of acetonitrile Prepared.

[0024] The preparation method of the solid-phase extraction membrane imprinted on the column methyltestosterone is as follows:

[0025] (1) In the separation quartz capillary (100 μm in inner diameter, 60 cm in length), burn a window with a width of 3 mm near the injection port as the irradiation window of ultraviolet light; use 0.1 mol L -1 NaOH, 0.1 mol L -1 Rinse and activate the separation capillary with HCl for 30 min, then rinse with water and acetone for 5 min each, then dry the capillary with nitrogen flow;

[0026] (2) Suction 3-(methacryloyloxy)propyltrimethoxysilane acetone solution with a length of 1.5 cm and a volume ratio of 30% from the inlet port of the capillary through capillary action, seal both ...

Embodiment 2

[0030] The polymerization solution was 0.05 mmol of methyltestosterone, 0.2 mmol of functional monomer methacrylic acid, 1 mmol of ethylene glycol dimethacrylate and 0.06 mmol of initiator azobisisobutyronitrile (AIBN) dissolved in 3 mL of acetonitrile Prepared.

[0031] The preparation method of the solid-phase extraction membrane imprinted on the column methyltestosterone is as follows:

[0032] (1) In the separation quartz capillary (inner diameter 100 μm, length 60 cm), burn a window with a width of 3 mm near the injection port as the irradiation window for ultraviolet light; use 1 mol L -1 NaOH, 1 mol L -1 Rinse and activate the separation capillary with HCl for 30 min, then rinse with water and acetone for 5 min each, then dry the capillary with nitrogen flow;

[0033] (2) Suction 3-(methacryloyloxy)propyltrimethoxysilane acetone solution with a length of 1.5 cm and a volume ratio of 30% from the inlet port of the capillary through capillary action, seal both ends of t...

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Abstract

The invention discloses a method for preparing a molecular imprinting solid-phase extraction film in a separation capillary. According to the method disclosed by the invention, polymerization is initiated at the sample inlet end of the separation capillary by utilizing ultraviolet irradiation to directly prepare a layer of molecular imprinting solid-phase extraction film with the length of several millimeters, so that the molecular imprinting solid-phase extraction film is used in online solid-phase extraction in capillary electrophoresis. The method can be used for preparing various molecular imprinting solid-phase extraction films in the separation capillary; and the prepared capillary with the molecular imprinting solid-phase extraction films has the advantage of zero dead volume, prevention in filling of polymer, fixed steps, small back pressure and the like and can be used in online separation, gathering and subsequent capillary electrophoresis assay determination of a target object in complex samples such as biological samples, medicine samples, environmental samples and food samples.

Description

technical field [0001] The invention relates to a method for preparing a molecularly imprinted solid-phase extraction membrane in a separation capillary, and belongs to the technical field of sample pretreatment in capillary electrophoresis. Background technique [0002] Capillary electrophoresis technology has attracted extensive attention in recent years due to its advantages such as high resolution, fast analysis speed, and low sample consumption. Capillary electrophoresis has a variety of separation modes, which can be used for the analysis of inorganic ions, small organic molecules, peptides, proteins, nucleic acids and even cells. However, when applied to complex samples such as biology, medicine, environmental samples and food, this method needs to rely on efficient and highly selective sample pretreatment techniques. In capillary electrophoresis analysis, the sample pretreatment technology has two main purposes, namely, eliminating the matrix and enriching the targe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/28B01J20/30C08F222/14C08F220/06C08F4/04C08J9/26
Inventor 张信凤许淑霞王艳艳孙永华
Owner CHENGDU UNIVERSITY OF TECHNOLOGY
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