An HPLC method is described using conductimetric detection for the quantitative determination of sodium, potassium, magnesium, and calcium in cerebrospinal fluid (CSF) and plasma of conscious rabbits. This method enabled the four cations to be estimated with rapidity, sensitivity, accuracy, and precision. The mean millimolar concentrations +/- SD found in CSF and (plasma) of 15 untreated animals were as follows: sodium, 146.96 +/- 17.84 (135.06 +/- 20.11); potassium, 3.32 +/- 0.56 (4.57 +/- 1.03); magnesium, 0.90 +/- 0.20 (0.72 +/- 0.13); and calcium, 1.47 +/- 0.19 (3.32 +/- 0.59).