A capillary gas chromatographic method is described for the determination of perindopril, an anti-hypertensive agent. The method is based on the derivatization of perindopril with pentafluorobenzyl bromide in acetone, using potassium carbonate as a base catalyst. Under a mild condition, the highly polar and nonvolatile perindopril was derivatized into a derivative with suitable chromatographic properties. The resulting derivative was separated on an SE-54 capillary column and detected by a flame-ionization detector.