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The derivatization of polyamines and amino acids with fluorescamine is a useful tool for the detection and quantitation of these compounds. High-pressure liquid chromatography (HPLC) separation coupled to postcolumn derivatization allows for the detection of nanomole amounts of material and is simple to use. Because the compounds of interest are derivatized after separation by HPLC, their biological functionality is not destroyed prior to analysis, allowing the mixture to be separated for other uses. This method also has the advantage of being able to detect small peptides and conjugated polyamines (e.g., glutathione and trypanothione) and with the use of acid hydrolysis, allows for their composition to be analyzed.