In this study, the feasibility of Raman spectroscopy for studying the transesterification of canola oil with dimethyl carbonate to biofuel using triazabicyclodecene modified Mg-Al layered double hydroxide as a catalyst was investigated. The conversion of the oil was monitored at certain intervals over 1 h. The height of the C=C stretching mode of unsaturated fatty acids of the oil at 1655 cm(-1) was measured to determine the conversion of the oil. Deconvolution algorithms were developed to differentiate between the peaks and optimize the spectra for quantitative analysis using Gaussian distribution. The developed Raman spectroscopy method was validated by gas chromatography analysis of the reaction.