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A sensitive and reliable analytical method for determining furosine in hair has been developed using liquid chromatography–tandem mass spectrometry. Fructose-N^α-formyl-d4-DL-lysine was synthesized and used as an internal standard. By the present method, glycated lysine levels in hair could be determined as fructose-lysine in only 0.1 mg of hair sample, ranging from 35.1–72.6 ng/mg hair among five healthy volunteers, which corresponded to 0.0635–0.153% of the total lysine contents in hair determined by amino acid analysis. © 1997 by John Wiley & Sons, Ltd.