In this series of papers, we are reporting on the rapid and sensitive detection of glycosides by high performance liquid phase separation methods such as high performance liquid chromatography (HPLC), capillary electrophoresis (HPCE), and capillary electrochromatography (CEC). In this report, which is the second in this series, we are describing the detection of glucosinolates via their acid hydrolysis degradation products. The rationale behind this approach is the lack of authentic standards, a fact that makes the routine analysis of glucosinolates rather difficult. Upon acid hydrolysis, glucosinolates hydrolyze, among other things, to carboxylated compounds that are reflective of the individual glucosinolates.