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Synthetic drug genotoxic impurity analysis method based on solid phase microextraction

A technology for genotoxicity and drug synthesis, applied in analytical materials, alkali metal compounds, chemical instruments and methods, etc., can solve the problems of large matrix interference, low sensitivity, etc. Effect

Active Publication Date: 2020-06-12
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventional solid-phase extraction has disadvantages such as low sensitivity and large matrix interference

Method used

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  • Synthetic drug genotoxic impurity analysis method based on solid phase microextraction
  • Synthetic drug genotoxic impurity analysis method based on solid phase microextraction
  • Synthetic drug genotoxic impurity analysis method based on solid phase microextraction

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preparation example Construction

[0039] During the preparation of covalent organic framework nanospheres:

[0040] In some embodiments of the present invention, the reagents for washing the covalent organic framework nanospheres are absolute ethanol, anhydrous acetone, anhydrous dichloromethane, and absolute ethanol in sequence.

[0041] In some embodiments of the present invention, the covalent organic framework nanospheres are washed and then vacuum-dried at 40-60° C. for 10-15 hours.

Embodiment 1

[0044] Preparation of Covalent Organic Framework Nanospheres.

[0045] First, dilute 116.1 mg of tris-(4-aminophenyl)-amine and 130.6 mg of tris-(4-formylphenyl)-amine into 2 mL of N,N-dimethylformamide solution , the reaction solution was added to 25 mL of methanol, and stirred at room temperature for 10 minutes; then, 0.01 mL of glacial acetic acid solution was added to the solution. The above reaction solution was reacted in a water bath at 80° C. for 30 minutes. After the reaction was over, the excess reaction solution was removed, leaving a deep yellow precipitate. Finally, the precipitate was sequentially washed with absolute ethanol, anhydrous acetone, anhydrous dichloromethane, and absolute ethanol to remove residual solvents and excess raw materials remaining on the surface of the material. The washed material was vacuum dried overnight at 50 °C. The synthesized material was characterized by figure 2 It can be seen from the scanning electron microscope and the tr...

Embodiment 2

[0047] Preparation of fibers for solid-phase microextraction.

[0048] Take stainless steel fibers with a diameter of 120 microns and wash them with absolute ethanol and deionized water successively. After cleaning, the stainless steel fibers are pressed figure 1 Etching is carried out, the etching solution is hydrofluoric acid, and the etching time is 1 hour. Adhere the surface of the etched stainless steel fiber with high-temperature-resistant silicone sealant, place the treated fiber in an ethanol dispersion of covalent organic framework nanospheres (dispersion concentration is 100 mg / mL), and let it stand for one minute Take it out, the material will be evenly distributed on the surface of the stainless steel fiber. After the surface of the fiber is dry, it is aged for 3 hours under the gas chromatograph inlet, and the aging temperature is 250°C. Take it out and use it later.

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Abstract

The invention relates to a synthetic drug genotoxic impurity analysis method based on solid phase microextraction. The solid-phase microextraction fiber comprises covalent organic framework nano microspheres and a fiber carrier, wherein the covalent organic framework nano microspheres are loaded on the surface of the fiber carrier; wherein the covalent organic framework nano microsphere is formedby combining two ligands tri-(4-aminophenyl)-amine and tri-(4-formylphenyl)-amine. The determination of the genotoxic impurities in the raw material medicine is achieved. The solid-phase microextraction fiber has the characteristics of high temperature resistance, high repeated use frequency and high adsorption capacity.

Description

technical field [0001] The invention belongs to the technical field of detection of genotoxic impurities, and in particular relates to a solid-phase microextraction fiber, a preparation method thereof and an application in the analysis of genotoxic impurities of synthetic medicines. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] At present, the vast majority of drugs are produced by chemical synthesis or by modification of natural products. Either way, a variety of reagents are used in the synthesis. These reagents often have a small amount of residue or produce many by-products during the production process, forming impurities with certain unknown toxicity, especially ...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01J20/22B01J20/28B01J20/30G01N30/02G01N30/08
CPCB01J20/223B01J20/28023B01J20/281B01J2220/4812B01J2220/52B01J2220/54B01J2220/80G01N30/02G01N30/08G01N2030/062
Inventor 赵燕芳谢含仪李靖坤陈相峰李慧娟赵梅
Owner SHANDONG ANALYSIS & TEST CENT
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