Cotton fabric is modified chemically to convey crease resistance to the cellulosic material by means of an appropriate crosslinking agent. For this purpose glyoxal was tested as a nonformaldehyde durable press agent. The cotton-bound glyoxal can be quantified by means of isocratic HPLC, whereby the glyoxal-treated fabric is hydrolyzed by a NaOH solution. During this pretreatment glyoxal is extracted from the cellulosic sample and converted into glycolate by an internal Cannizzaro reaction. The addition of glycols such as ethylene glycol or diethylene glycol into the formulation results in a remarkable decrease of the amount of glyoxal that is detected. This phenomenon can be explained by the fact that the glycol reacts with the glyoxal, thus hampering the internal Cannizzaro reaction. The acidic hydrolysis and the alkaline hydrolysis provide the same results, thus indicating that the alkaline treatment removes all the cotton-bound glyoxal. (C) 2003 Wiley Periodicals, Inc.