Abstract Procedures have been developed for the isolation of phenothiazines and chemically related compounds from pharmaceutical formulations, namely, injections, solutions, tablets, coated tablets, creams, sirups, lotions, and suppositories. In general, active substances are crystallized as picrates. A few compounds, however, gave better crystalline derivatives as free bases (levomepromazine and propericiazine), quaternary ammonium salt (thiazinamium), or chlorhydrate salts (amitriptyline and nortriptyline). The crystalline derivatives prepared were specifically identified by comparison of their Debye-Scherrer X-ray diffraction patterns with those for reference compounds obtained under the same conditions.