OBJECTIVE： To establish the method for the concentration determination of amiodarone and its metabolite desethylamidarone in plasma. METHODS： The plasma was acidized with pH 5.4 monobasic potassium phosphate and extracted with ethyl ether. HPLC method was adopted， and Ultimate C18 column was used with mobile phase consisted of glacial acetic acid-triethylamine buffer solution（A）-methanol（B）（VA/VB＝19 ∶ 81） at the detection wavelength of 242 nm and flow rate of 1.0 ml/min using progestrone as internal standard. RESULTS： The linear range of amiodarone and desethylamiodarone were 0.2-4.0 μg/ml （r＝0.999 5） and 0.24-4.8 μg/ml （r＝0.999 8）， and their recoveries were 95.63％-100.10％ and 93.14％-106.70％ （RSD≤9.7％）. CONCLUSIONS： The method is simple， accurate and practical， and it can quickly and accurately determinate the blood concentration of amiodarone and desethylamiddarone.