Synthesis of the reversed stationary phase for solid phase extraction using trimethoxyoctadecyl silane

Du Huy Nguyen,Giang Tien Nguyen,Mai Anh Nguyen

doi:10.32508/stdj.v19i1.536

Abstract

Octadecyl grafting silica was synthesized using trimethoxyoctadecyl silane. Reaction conditions were optimized so that the carbon percentage of resulted material was similar to that of commercial products. Temperature and catalyst played very important roles in the reaction. The material was also undergone the end-capping process to reduce unreacted silanol groups. Final product owned 14.1 % of carbon content and 75 % of the unreacted silanols. Retention behavior of product was tested and compared to the same noes available on the market. Results showed that both resulted material and commercial had the same retention properties.

Highlights

Solid phase extraction (SPE) is a well-established sample pretreatment technique because it demands less organic solvents and can remove interferences simultaneously
conventional reversed phase (CRP) is synthesized by directly bonding alkoxyoctadecyl silane or chlorooctadecyl silane onto silica surface[2,3,4,5]
After cooling to room temperature, 2 g of silica were added to a flask, 20 mL of toluene, 0.5 mL of TMOS and 150 mg p-toluenesulfonic aicd were added

Summary

Introduction

Solid phase extraction (SPE) is a well-established sample pretreatment technique because it demands less organic solvents and can remove interferences simultaneously. In SPE chemical structure of sorbent materials play a decisive role[1]. The most popular sorbent material is conventional reversed phase (CRP) on silica support. CRP is synthesized by directly bonding alkoxyoctadecyl silane or chlorooctadecyl silane onto silica surface[2,3,4,5]. While chlorolsilane is very reactive, alkoxysilane is one of the least reactive reagents[3]. During the reaction with silica, chlorosilane produces HCl by-product which can damage the main product. The byproduct is alcohol which is harmless and easy to remove in distilled conditions. The less reactivity of alkoxysilane can be overcome by employing an appropriate catalyst [6]

Methods

Results

Conclusion