A new method was developed for the determination of trifluoperazine hydrochloride (TFPH) at trace levels in pharmaceuticals. This method involved formation of a TFPH-Pt(IV) complex at a specific pH, and extraction of this complex into an organic solvent. Flame atomic absorption spectrometry was used to measure the absorbance of platinum in the complex, and indirectly determine the concentration of TFPH. Under the optimized conditions, the linear dynamic range, detection limit, relative standard deviation (n = 5), and the recoveries of the standard addition method were 2−60 µg mL −1 , 0.085 µg mL −1 , 1.58−2.03, and 102.24 ± 0.43, respectively. The proposed method was applied to the determination of TFPH in the drug Stelazine (5 mg of TFPH per tablet) by both direct and standard addition procedures and gave results of 4.89 and 4.88 mg of TFPH per tablet. This method was compared statistically with the determination of TFPH by UV-Vis spectroscopy, and the difference in the precision from these methods was insignificant at the 95% confidence level.