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Preparation and investigation of LC packing made by microwave‐assisted solid‐phase synthesis
Authors:Eva Jambor  Agnes Bona  Janos Schmidt  Laszlo Mark  Robert Ohmacht
Affiliation:1. Institute of Biochemistry and Medical Chemistry, Medical School, University of Pecs, , Pecs, Hungary;2. Janos Szentagothai Research Center, University of Pecs, , Pecs, Hungary
Abstract:The preparation of the so‐called bonded phase liquid chromatographic packings is usually carried out by heating the silica, the silane, a catalyst, or a scavenger in an appropriate solvent (often toluene.) Due to the longtime of boiling, the procedure is time and energy consuming, and solvent intensive. The goal of this work is to present a simple, environment‐friendly preparation method with reduced solvent consumption to synthetize RP liquid chromatographic stationary phases. The effects of reaction conditions (amount of reagents, composition of the reagent, microwave energy, reaction time, reproducibility of the synthesis) are discussed. Pore structure, surface coverage, the change of the pore structure and surface coverage upon reaction are demonstrated, the efficiency of the column (van Deemter plot for different solutes) is presented. A variety of applications (aromatic hydrocarbons, halobenzenes, bioactive peptides, resveratrol from red wine) demonstrates the separation power of the new phase.
Keywords:HPLC  Microwave irradiation  Pore structure of packing  Preparation of RP  Solid‐phase synthesis  Stationary phase
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