This presentation describes the analysis of GC-amenable pesticide residues in herbal preparations and tuber crops like yam (Dioscorea spp.), taro (Colocasia esculenta) and sweet potato (Ipomoea batatas L.). The use of the accelerated solvent extraction technique at elevated temperature and pressures proved critical for the fast and efficient solvent extraction of analytes from tubers. This presentation will describe our experience, challenges, and successes in the development, validation and implementation of methods for GC-MS/MS analysis of pesticide residues in herbal preparations using conventional sample extraction, and in tuber crops using the accelerated solvent extraction technique.