A method is proposed for extraction, separation, identification and quantitative measurement of boldine (I) in pharmaceuticals. The extraction of (I) from the matrix (syrups, tablets, extracts) was realized with aqueous ammonium chloride (0.02 M, pH=3.0 with perchloric acid) and the clean-up of the extract was performed by solid-phase extraction by means of cartridges containing a strong cation-exchange sorbent, from which (I) was eluted with aqueous ammonium chloride (1 M, pH=10.0 with ammonia). The final eluate was examined by HPLC. Chromatography was performed on a C-8 column with a gradient elution from 15:85 to 30:70 of acetonitrile-water containing 0.1 M sodium perchlorate (pH=3.0), in 20 min. A diode array detector was used at 302 nm for detection. The method gives recovery values greater than 98% and the reproducibility is within 6.0%.