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A dendritic C18 silica microsphere stationary phase and its preparation and application

A silica, dendritic technology, applied in chemical instruments and methods, other chemical processes, liquid separation of solid adsorbents, etc., can solve problems such as slow adsorption-desorption kinetics, chromatographic peak tailing, etc., with few steps to achieve , The effect of high reaction efficiency and mild reaction conditions

Active Publication Date: 2017-12-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

Strong interactions between deprotonated silanols and protonated basic compounds tend to produce slow adsorption-desorption kinetics, resulting in peak tailing

Method used

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  • A dendritic C18 silica microsphere stationary phase and its preparation and application
  • A dendritic C18 silica microsphere stationary phase and its preparation and application
  • A dendritic C18 silica microsphere stationary phase and its preparation and application

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Embodiment Construction

[0030] EXAMPLES Separation of Basic Compounds Using Dendritic C18 Silica Microspheres as Stationary Phase.

[0031] Preparation of Dendritic C18 Silica Microsphere Stationary Phase:

[0032] 1) Disperse 8.50g of silica microspheres into 60mL of dry toluene (containing 3mL of anhydrous pyridine), then add 7mL of 3-aminopropyltriethoxysilane to it, and reflux the final reaction solution under the protection of argon After 24 hours, the product was washed 5 times with 30 mL of ethanol, and dried in a vacuum oven at 50°C for 24 hours to obtain 3-aminopropyl functionalized silica microspheres (SiO 2 -NH 2 );

[0033] 2) Take 2.5g SiO2 2 -NH 2 Disperse in methanol, then add propynyl acrylate 1.4mL dropwise, the final mixture was stirred at room temperature for 36h, the silica microspheres were taken out, washed with absolute ethanol, and then dried in a vacuum oven at 50°C for 12h , to obtain dendritic propynyl acrylate-modified silica microspheres (SiO 2 -N(CO 2 CH 2 C≡CH) ...

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Abstract

The invention relates to the preparation of a dendritic carbon octadecyl silica microsphere stationary phase and its application in the separation of basic compounds. Firstly, 3-aminopropyl group was introduced on the surface of silicon spheres, then dendritic propargyl acrylate was grafted on the surface of 3-aminopropyl-functionalized silicon spheres by Michael addition, and then 1-octadecanethiol and photoinitiator were added, 1 ‑Octadecathiol undergoes mercapto-alkyne addition reaction under the control of a photoinitiator to prepare a stationary phase with surface-modified dendritic octadecyl groups. The preparation process of the stationary phase is simple, the reaction conditions are mild, and it is successfully applied to the separation of basic compounds.

Description

technical field [0001] The invention relates to the separation of basic compounds, in particular to a dendritic C18 functionalized silica microsphere stationary phase and its preparation, as well as its application in the separation of basic compounds. Background technique [0002] Since more than 70% of the drugs are basic compounds (document 1. Chen et.al "Analysis of the acid–base reaction between solid indomethacin and sodium bicarbonate using infrared spectroscopy, X-ray powder diffraction, and solid-state nuclear magnetic resonance spectroscopy", "Journal of Pharmaceutical and Biomedical Analysis", 2005, 38 (4), 670-677.), so the separation of basic compounds is a very meaningful work. At present, high performance liquid chromatography is a commonly used method for the separation of basic compounds. The reversed-phase mode is the most widely used separation mode in liquid chromatography, and the reason is that it is easy to realize gradient elution in reversed-phase c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/10
Inventor 邹汉法黄光欧俊杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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