The explosion of interest around the health benefits of whole grains has led to a new focus on the bioactive components of cereals, including their location and physiological effects. Measurements of these components require methodologies for analysis that must be accurate and reproducible and that provide adequate samples to allow wide screening. Provides the current knowledge and key methods for more than a dozen specific bioactive components in small grains. The development of routine analytical methods for this group of essential phytochemical and dietary fiber components will help food companies improve the health benefits of their products as well as their abilities to measure the bioactive ingredients in cereal-based foods.