Derivatization of glycerol and its formates with phenyl isocyanate in pyridine
Chemical interesterification reaction of rapeseed oil with methyl formate yield two layers of product - upper biofuel containing layer and lower glycerol formates containing layer. Our aim was to develop a method for analysis of lower layer of interesterification product containing glycerol, monoformin (MFG), diformin (DFG), and triformin (TFG) in lower layer of interesterification reaction. Underivatized glycerol and MFG cannot be determined with HPLC-PDA-MS. Derivatization was performed with phenyl isocianate and pyridine was tested as solvent. Reaction of 2-3 mg sample with 10 mkL PhNCO at 45 deg. Celsius in 100 mikroliters of pyridine was tested. Derivate of pure glycerol forms easily (paraugs 3) and precipitates in higher concentrations (paraugs 3 nogulsnes). Formine layer was found to degrade in these conditions, signal form DFG and MFG were not found (paraugs 15), instead glycerol was found along with partially derivatized intermediates.
Date
28.01.2019.
Keywords
derivatization, phenyl isocyanate, glycerol
