Due to the toxic and carcinogenic effects of mycotoxins on humans and animals, their determination in food and feeds become an important issues. Sample preparation remains the bottle-neck of the entire analysis. Therefore, this book focus on the development of new sample preparation techniques, which are targeted to not only simplify the procedure, but only leads towards minimization of analysis time and reduction of organic solvents. Equally important is the HPLC analysis time which needs to be further reduced.