1 A method is described for the simultaneous determination of amodiaquine (AQ) and desethylamodiaquine (AQm) in plasma, urine, whole blood and packed red cells. 2 After oral administration of AQ (600 mg) to seven healthy subjects, absorption of AQ was rapid, reaching peak concentrations in plasma, whole blood, and packed cells at 0.5 ± 0.03, 0.5 ± 0.1 and 0.5 ± 0.1 h respectively (mean ± s.e. mean). The apparent terminal half-life of AQ was 5.2 ± 1.7 h. AQ was detectable for no longer than 8 h. 3 AQ underwent rapid conversion to AQm, which reached peak concentrations in plasma, whole blood and packed cells at 3.4 ± 0.8, 2.3 ± 0.5 and 3.6 ± 1.1 h respectively. AQm was still detectable at the end of the sampling period (96 h) when the plasma concentration was 29 ± 8 ng ml-1. 4 The area under the plasma concentration vs time curve (AUC(0,oo)) for AQ was 154 + 38 ng ml-1 h; the corresponding value for AQm was 8037 ± 1383 ng ml -1 h. There were no significant differences in the values for AUC of AQ between plasma, whole blood, or packed cells. 5 The whole blood to plasma concentration ratio for AQm was 3.1 ± 0.2, and the AUC (0,24) for AQm in whole blood (6811 ± 752 ng ml-' h) was significantly greater than that in plasma (2304 ± 371 ng ml-' h), P < 0.001.6 The recovery of AQm from urine collected 0-24 h was 6.8 ± 0.8 mg (n = 6). In one subject urine was collected up to 5 months after dosing, and recoveries of AQ and AQm were 3.0 mg (0-1 month) and 57 mg (0,00) respectively. AQ and AQm were still detectable in urine 5 months after dosing.