Starch is a very important and common polysaccharide found in food and organic products. The most common standard methods to determine starch content in food are those established by the Association of Official Analytical Chemists (AOAC) or the American Association of Cereal Chemists (AACC). The determination of starch in foodstuffs is time-consuming and uses a lot of reagents, so the development of techniques that are faster and do not require sample preparation is interesting. Recently, distinct instrumental methods have been used in food analyses, as near infrared (NIR) spectroscopy and hyperspectral imaging (HSI). However, working with spectroscopy can be a challenge. Thus, this chapter shows a tutorial on NIR spectroscopy and hyperspectral imaging data acquisition for the detection and characterization of starch.