Abstract— The hexafluoroisopropyl esters of trifluoroacetylated homovanillic acid (HVA) and 3‐hydroxy‐4‐methoxyphenylacetic acid (iso‐HVA) were the derivatives chosen for assay of these phenolic acids in lumbar cerebrospinal fluid (CSF) specimens from 65 control subjects. The mean value obtained in these specimens was 40.0 ± 23.5 ng/ml. Recovery of added HVA and iso‐HVA was 94 ± 2 per cent and reproducibility was ±5 per cent. CSF from Parkinson's disease patients undergoing treatment with l‐DOPA showed significant increases in HVA. Iso‐HVA was detected in those CSF samples obtained during l‐DOPA therapy.