OBJECTIVE： To establish the method for concentration determination of enalapril maleate in human urine and feces， and apply it in the clinic. METHODS： The urine and feces samples were collected and pre-processed， then tested by surface-enhanced Raman scattering spectrometry with ratio of sample to surface signal enhancer silver sol 1 ∶ 1（V/V）. The assay was carried out with the following parameters： excitation power 400 mW， excitation wavelength 785 nm， resolution 4.5 cm－1. The characteristic shift of enalapril maleate were （800±2）， （1 050±2）， （1 330±2）， （1 450±2）， （1 630±2） cm－1. The quantitation shift was （1 050±2） cm－1. RESULTS： The linear range of enalapril maleate were 0.50-100.00 μg/ml in urine and 2.00-100.00 μg/g in feces（r＝0.989 3， 0.978 0，n＝6）； the limits of quantitation were 0.50 μg/ml and 2.00 μg/g， and the limits of detection were 0.10 μg/ml and 1.30 μg/g. RSDs of intra-day and inter-day were both lower than 5％. The method recoveries were 95.24％-99.38％ and 86.73％-94.57％； the extraction recoveries were 84.29％-90.43％（RSD＝0.84％） and 82.36％-87.70％（RSD＝1.84％）， respectively. The urinal concentration of enalapril maleate in 15 hypertensive patients ranged 15.31-33.46 μg/ml， while the fecal concentration ranged 5.08-41.79 μg/g. There was no statistical significance in average urinal concentration and fecal concentration between “effective” patients and “no response” patients. CONCLUSIONS： Surface enhanced Raman scttering spectrometry can be used for the concentration determination of enalapril maleate in human urine and feces. It is simple and rapid.