The use of isotopic analyses grows each year, due to large area of expertise in several science areas. Several techniques are used to perform the determination of natural isotope concentrations and their variations, with isotopic ratio mass spectroscopy (IRMS) being the most widely used. An analytical technique that is gaining market space is the cavity ring-down spectroscopy. Unlike mass spectrometers, these analyzers require little or no sample treatment, thereby reducing the analysis time. The present study aimed to obtain the 13C/12C isotopic signature in solid and liquid samples using a laser analyzer. An isotopic analysis method using a total organic carbon analyzer coupled to a cavity ring-down spectrometer (iTOC-CRDS) was developed and implemented. The results were compared with those obtained by IRMS. The method performance was evaluated by the parameters of linearity; accuracy, using standard reference materials; precision, using parameters of repeatability and reproducibility and by calculating the associated uncertainties. The analyzed samples were sugar, biomass, bio-oil, biofuel, methanol and gasoline.