A chemiluminescent method using flow injection (FI) was investigated for rapid and sensitive determination of enalapril maleate and atenolol, which are used in the treatment of hypertension. The method is based on the sensitizing effect of these drugs on the Ce(IV)-sulfite reaction. The different experimental parameters affecting the chemiluminescence (CL) intensity were carefully studied and incorporated into the procedure. The method permitted the determination of 0.01-3.0 microg mL(-1) of enalapril maleate in bulk form with correlation coefficient r = 0.99993, lower limit of detection (LOD) 0.0025 microg mL(-1) (S/N = 2) and lower limit of quantitation (LOQ) 0.01 microg mL(-1). The linearity range of atenolol in bulk form was 0.01-2.0 microg mL(-1) (r = 0.99989) with LOD of 0.0003 microg mL(-1) (S/N = 2) and LOQ of 0.01 microg mL(-1). In biological fluids the linearity range of enalapril maleate was 0.1-2.0 microg mL(-1) in both urine and serum, and for atenolol the linearity range was 0.1-1.0 microg mL(-1) in both urine and serum. The method was also applied to the determination of the drugs in their pharmaceutical preparations.