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A kind of polymer monolithic column and its preparation method and application

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

Inactive Publication Date: 2016-06-22
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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  • A kind of polymer monolithic column and its preparation method and application
  • A kind of polymer monolithic column and its preparation method and application
  • A kind of polymer monolithic column and its preparation method and application

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, add 20 μL of different concentrations of Kronosin working solution, and prepare the drug-containing human serum standard solution of the desired 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] Embodiment 3 monolithic column is used for the detection of human urine sample

[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 novel pipette straw macroporous polymer monolithic column and its preparation method and application. A method for preparing a polymer monolithic column, the monolithic column is prepared by in-situ thermally induced polymerization, and cellulose diacetate is used as a porogen, which specifically includes the steps of: (1) pretreatment of the inner wall of a pipette; (2) Preparation of the polymer monolithic column in the pipette straw; (3) Washing of the monolithic column; the monolithic column of the pipette prepared by the present invention has a larger through-hole size and a larger column bed volume, and can cooperate with a pipette Operation and use, the SPE operation can be completed under the discharge pressure of the pipette; the invention can realize the purpose of fast and high-efficiency enrichment of the target component to be tested.

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 Patents(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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