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A simple procedure for the correction of the decreasing detection response in a matrix‐assisted laser desorption/ionization time‐of‐flight (MALDI‐TOF) mass spectrum with increasing ion mass is reported. On the basis of the experimental MALDI‐TOF mass spectrum of a mixture of four polymethylmethacrylate (PMMA) standards (molecular masses in the range 4–100 kDa), present in equal molar abundance, an equation describing the MALDI‐TOF response has been derived. This equation has been used to correct any subsequently recorded MALDI spectrum. As an example, the procedure has been applied here to normalize the MALDI‐TOF mass spectrum of a 1,20‐di(bisphenoxy‐A)eicosane based copolyformal (I) containing porphyrin units in the main chain. © 1998 John Wiley & Sons, Ltd.
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