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A new enzymatic photometric assay for determination of methanol and ethanol in solutions containing both alcohols is described. The assay allows detection of methanol in the concentration range of tens of ppm in the presence of tens of percent of ethanol. The lower determination threshold for methanol is at least 0.002% in the presence of 45% ethanol, with a coefficient of variation of 0.02–0.05. General-purpose spectrophotometers and photoelectric colorimeters can be used in the measurements.