PURITY DETERMINATIONS IN THE BULK DRUG OF THE NOVEL INDOLOQUINONE ANTITUMOR AGENT EO9

The pharmaceutical development of the investigational cytotoxic drug E O9 included the structural characterization of the bulk drug by nuclea r magnetic resonance (NMR) spectroscopy, mass spectrometry (MS) and in frared (IR) spectroscopy, and analytical characterization by high-perf ormance liquid chromatography and ultraviolet/visible spectrophotometr y. The presence of impurities in the bulk drug was investigated. The i ntermediates in the synthesis of EO9 were structurally characterized b y NMR spectroscopy and MS, and analytically characterized by HPLC anal ysis with photodiode array (PDA) detection. All of the intermediates w ere below their limits of detection in EO9 bulk drug. The amounts of r esidual organic solvents were determined by gas chromatography. Methan ol and ethanol were detected, but the amounts present did not exceed t he limits as set in the United States Pharmacopeia XXII.