A specific, sensitive, and precise assay for simultaneous quantitation of glyceryl trinitrate (GTN) and its metabolites 1,2and 1,3-glyceryl dinitrate (GDN) has been developed. The method involves one single extraction step with benzene, followed byevaporation at 55'C.One plof theextractwasinjected onto a capillary fused silica column with trifluoropropyl as the stationary phase.Thecolumnseparatedal1 thenitrateswithin 17 minutes using temperature programming from 90 to 155OC. The lower limits of detection were 0.05,0.5, and 0.1 nmol/l for GTN, 1,2-GDN and 1,3-GDN respectively. The calibration curves were linear in the concentration ranges 0.05-1 0.0 nmol/l (GTN), 0.5-10.0 nmol/l (1,2-GDN) and 0.1-10.0 nmol/l (1,3-GDN). Plasma concentration data from two patients receiving intravenous GTN infusion are presented.