We describe a simple method for extracting 3-methoxy-4-hydroxyphenylglycol (MHPG) from plasma. The sample is applied to a 1-mL "Extrelut" column (EM Industries) and eluted 15 min later with ethyl acetate. After mixing the eluate with pentane and back-extraction into water, we inject 25 or 50 microL of the aqueous phase onto a Beckman 15 cm x 4.6 mm (i.d.) column packed with 5-micron ODS particles (Beckman). Peaks are detected with a coulometric detector. The resulting chromatogram is clean, with few extraneous peaks. The extraction recovery of MHPG is 55-60%, which allows for detection of as little as 0.2 microgram of the analyte per liter. The decrease in the concentration of MHPG in plasma of patients treated with phenelzine agrees with the decrease in monoamine oxidase activity in platelets of these patients.