The metabolites of procaterol HCl in dog urine and faeces and in human urine were qualitatively analysed by an improved g.l.c.-mass spectrometric method. 2. Trimethylsilylated derivatives of procaterol metabolites were identified by mass fragmentography as procaterol glucuronide, 5-(2-amino-1-hydroxybutyl)-8-hydroxycarbostyril (desisopropylprocaterol), 5-formyl-8-hydroxycarbostyril, 8-hydroxycarbostyril and unchanged procaterol. 3. The metabolic pattern of procaterol HCl was species-independent in rats, dogs and man.