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Preparation method of three-functional-group n-octadecyl bonded phase

A technology of n-octadecyl and trifunctional groups, which is applied in the field of preparation of bonded phases for high-performance liquid chromatography fillers, can solve problems such as n-octadecyl detachment and chromatographic column failure, reduce surface hydroxyl groups, and increase applicable pH range, stability-enhancing effects

Active Publication Date: 2010-12-29
微纯生物科技(广州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is well known that the silicon-oxygen bond can be hydrolyzed and broken, and this phenomenon is especially obvious under alkaline conditions, resulting in the detachment of n-octadecyl from the surface of silica gel, resulting in the failure of the entire chromatographic column

Method used

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  • Preparation method of three-functional-group n-octadecyl bonded phase
  • Preparation method of three-functional-group n-octadecyl bonded phase
  • Preparation method of three-functional-group n-octadecyl bonded phase

Examples

Experimental program
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Effect test

example 1

[0020] Add 1.5kg of unactivated silica gel particles and 15kg of 0.01wt% hydrofluoric acid to a 20L glass-jacketed reactor (Shanghai Heqi BL-601375), reflux for 20 hours, cool to room temperature, filter with 1 micron filter paper, and filter cake with 2L After washing with deionized water for at least three times, the activated silica gel was obtained after being dried for 20 hours under vacuum (15 kPa) and a temperature of 78° C.

example 2

[0022] In a 150mL three-necked bottle, add 10g of dry silica gel particles (5μm, specific surface area 300m 2 / g) and 100mL anhydrous toluene, stir well to make the mixture uniform (no obvious agglomerated particles observed by naked eyes), then add 1.12g pyridine and 3.21g n-octadecyltrichlorosilane, reflux for 20 hours under nitrogen protection, and cool to At room temperature, filter through 1 micron filter paper. The resulting filter cake was washed with 50 mL of toluene, acetone and deionized water, and then dried under vacuum (15 kPa) at a temperature of 78° C. for 20 hours to obtain uncapped trifunctional n-octadecyl-bonded silica particles. Particle C% was 18.4%.

example 3

[0024] In a 150mL three-necked bottle, add 10g of dry bonded uncapped silica gel particles (5μm, specific surface area 300m 2 / g) and 100mL of anhydrous toluene, stir well to make the mixture uniform (no obvious agglomerated particles observed by naked eyes), then add 1.46g pyridine and 2.66g triethylchlorosilane, reflux for 20 hours under the protection of nitrogen, cool to room temperature, and use Filter through 1 micron filter paper. The resulting filter cake was washed with 50 mL of toluene, acetone and deionized water, and then dried for 20 hours under vacuum (15 kPa) and a temperature of 78° C. to obtain triethyl-endcapped trifunctional n-octadecyl-bonded silica gel particle. Particle C% was 20.1%.

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Abstract

The invention provides a method for bonding three-functional-group n-octadecyl group on silica gel surface. In the method, n-octadecyl trichlorosilane is used as a raw material, and all the three chlorine atoms can react with hydroxyl groups on the surface of silica gel, so that the n-octadecyl group can be connected to the surface of silica gel through three silicon-oxygen bonds. Under proper chromatographic conditions, the filler prepared by the invention can be effectively used for isolation analysis on acidic, neutral and basic compounds. Compared with single-functional-group n-octadecyl bonded phase, the invention greatly enhances the stability of the bonded phase, thereby obviously prolonging the service life of the chromatographic column and widening the available pH range.

Description

field of invention [0001] The invention relates to a preparation technology of a high-performance liquid chromatography filler bonding phase, and provides a bonding method for carrying out a trifunctional n-octadecyl phase on the surface of high-purity silica gel. The bonded particles can be used as fillers for high performance liquid phase chromatography. technical background [0002] N-octadecyl-bonded silica gel is currently the most widely used HPLC packing. In traditional bonding, dimethyl n-octadecyl chlorosilane is used to react with hydroxyl groups on the surface of silica gel to bond n-octadecyl groups to the surface of silica gel. Its characteristic is that n-octadecyl is connected to the surface of silica gel through a silicon-oxygen bond (see schematic figure 1 ), so it is called monofunctional n-octadecyl phase. It is well known that the silicon-oxygen bond can be hydrolyzed and broken, and this phenomenon is especially obvious under alkaline conditions, resu...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30
Inventor 黄晓黄曦
Owner 微纯生物科技(广州)有限公司
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