This guide is offered as an overview of the sample preparation considerations behind reliable, amino acid analysis of peptides and proteins contained in several common sources. The material can be used as a starting point for those who are performing amino acid analysis, as well as a resource for experienced analysts who are trying to resolve a related issue. Included is a list of select references that contain additional information on some of the discussed topics. The detailed procedures were obtained primarily from specific publications, AOAC official methods, and Waters Corporation’s 30 years of amino acid analysis experience. The overriding goal was to ensure likely success by presenting methods that carry levels of robustness when used as detailed in the document. Most of the included procedures have been used by analysts throughout the years. The hope is that these selections address many application needs.