The analysis of archaeol is necessary to obtain greater knowledge about their presence in feces. This study was conducted to explore the capability of using data obtained from two spectroscopic methods, UV-Vis and FTIR and from electrochemical sensors to determine the composition of cattle feces. Principal Component Analysis and correlation analysis using the spectral data were used. By combining spectral and compositional data, useful calibrations were developed. These calibrations can be used to rapidly predict these constituents in new samples. On the basis of the results obtained here, electrochemical sensors were found successful for the rapid determination of archaeol and several other parameters in feces.