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Copolymer monolithic column and preparation method and application thereof

A monolithic column and polymer technology, applied in chemical instruments and methods, other chemical processes, material separation, etc., can solve the problems of low back pressure, small monolithic column volume, poor permeability, etc.

Inactive Publication Date: 2014-10-22
GUANGDONG PHARMA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to overcome the problems of small volume and poor permeability of monolithic columns in the prior art, and provide a preparation method of polymer monolithic columns. The prepared monolithic column has the advantages of large column bed volume, good permeability, low back pressure, fast convective mass transfer and easy preparation, which greatly broadens the application range of the monolithic column.

Method used

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  • Copolymer monolithic column and preparation method and application thereof
  • Copolymer monolithic column and preparation method and application thereof
  • Copolymer monolithic column and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] In this example, the hydrophobic and weakly basic traditional Chinese medicine active monomer Kronoxin was used as a model drug to investigate the SPE enrichment effect of the prepared pipette monolithic column on the target drug component in methanol / water solution.

[0062] 1.1 Preparation of working solution

[0063] Accurately weigh 4.05 mg of coronoxine base in a 4 mL EP tube, dissolve in 2 mL of 60% methanol / water solution, and filter through a 0.22 μm syringe filter to obtain a 2.02 mg / mL stock solution of coronoxine. The stock solution was diluted with 60% methanol / water solution to obtain working solutions with different concentrations, among which the 24.2 μg / mL working solution was used for the investigation of the SPE conditions of the pipette monolithic column, and the others were used for the investigation of the adsorption performance of the monolithic column. Kronosin working solution with a concentration greater than 2.02mg∕mL was separately prepared se...

Embodiment 2

[0102] Example 2: Monolithic column is used for the detection of human serum samples

[0103] In this example, the hydrophobic and weakly basic traditional Chinese medicine active monomer Conoxin (CNX) was used as a model drug to investigate the SPE enrichment effect of the prepared pipette monolithic column on the target drug component in human serum.

[0104] 2.1 Preparation of human serum samples

[0105] 2.1.1 Preparation of CNX working solution

[0106] The preparation of CNX working solution is the same as "Item 1.1".

[0107] 2.1.2 Preparation and pretreatment of human serum standard solution

[0108] Take 200 μL of blank human serum and add 20 μL of different concentrations of Kronosin working solution to prepare a drug-containing human serum standard solution of the required concentration. Add 600 μL of methanol to the serum sample or serum standard solution, vortex to precipitate the protein, centrifuge at high speed (10,000 rpm) for 10 min, take the supernatant...

Embodiment 3

[0132] Example 3 Monolithic column used in the detection of human urine samples

[0133] In this example, the hydrophobic and weakly basic traditional Chinese medicine active monomer Conoxin (CNX) was used as a model drug to investigate the SPE enrichment effect of the prepared straw monolithic column on the target drug components in human urine samples.

[0134] 3.1 Preparation of human urine samples

[0135] 3.1.1 Preparation of CNX working solution

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Abstract

The invention relates to a macroporous copolymer monolithic column of a novel pipettor sucker and a preparation method and application of the copolymer monolithic column. The copolymer monolithic column is prepared by adopting an in-situ thermal initiation polymerization method by taking cellulose diacetate as a pore-forming agent. The preparation method particularly comprises the following steps: (1) pretreating the inner wall of the pipettor sucker; (2) preparing the copolymer monolithic column in the pipettor sucker; and (3) washing the monolithic column. The sucker monolithic column prepared by the preparation method disclosed by the invention has relatively large through hole size and large column bed volume, can be used by cooperating with a pipettor, can complete the SPE operation under the liquid discharge pressure of the pipettor, and can achieve the aim of enriching to-be-test target components rapidly and efficiently.

Description

technical field [0001] The invention relates to a polymer monolithic column, more particularly to a novel pipette straw macroporous polymer monolithic column and its preparation method and application. Background technique [0002] Currently, high-performance liquid chromatography-ultraviolet or mass spectrometry detection (HPLC-UV / MS) has become the main method for in vivo drug analysis. However, rapid and accurate chromatographic analysis of drug components in vivo has always faced the bottleneck of pretreatment of body fluid samples (especially blood samples). In recent years, many research fields such as pharmacology, clinical pharmacology, and clinical drug treatment detection are faced with the detection of an increasingly large number of physiological and body fluid samples. The development of rapid and efficient enrichment and purification methods for target components in body fluids is an important task. appears to be particularly important. [0003] Solid phase e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/30C08F220/18C08F220/06C08F2/44C08J9/28G01N30/08
Inventor 张红武吴顺娴司徒嘉露梁玉珊黄文丽钟飞燕
Owner GUANGDONG PHARMA UNIV
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