This chapter describes the analysis of tocopherols in edible animal tissues undergoing saponification. First, a survey of the main techniques to extract tocopherols is presented, and their advantages and disadvantages are discussed. Next, we explain the steps involving saponification followed by solvent extraction. Finally, the method is described with all the steps for quantification, calibration curve construction, extraction, and analysis using RP-HPLC with a fluorescence detector. Tocopherol analysis is delicate and requires attention and care at various steps, starting with sample preparation. Thus, a good understanding of the steps and critical points of the analysis guarantees a more representative and reliable result.