Carbonyl compounds including aldehydes, ketones and dicarbonyl-type compounds are present in cigarette smoke, in tobacco, and nicotine products. Traces of these compounds are found also in the aerosols from e-cigarettes. Various procedures for capturing efficiently these types of compounds from cigarette smoke are presented in the chapter, together with GC–MS methods and HPLC methods used for this purpose. Typical analysis of carbonyl compounds is performed using dinitrophenyl hydrazine derivatization and the methods for performing this derivatization are discussed in the chapter. Also, the use of UV detection or MS/MS detection associated with the HPLC analysis is presented.