The determination of gamma-aminobutyric acid (GABA) in cerebrospinal fluid and brain extracts is described. Its heptafluorobutyryl-isobutanol derivative was measured both by electron impact and chemical ionization mass fragmentography using GABA-d6 as internal standard. The derivatization product is stable for several days. The method is sensitive (1 ng absolute in cerebrospinal fluid and 30 pg in standard GABA solutions) and specific, when chemical ionization mode is applied. Normal values of GABA are in rat brain extracts (1.40 +/- 0.32 mumol/g fresh weight) and human CSF (18.3 +/- 10.0 ng/ml).