Identification and Purity Control of Thioacridine Derivatives by Gas and Capillary Liquid Chromatography with Mass Spectrometric Detection

ABSTRACT

Mass spectrometry combined with gas chromatography (GC‐MS) or capillary liquid chromatography (CLC‐MS) was successfully utilized for structural characterization and purity control of synthesized biologically active thioacridine derivatives. Obtained results document sufficient selectivity of GC‐MS and CLC‐MS towards structurally related impurities and degradation products accompanying the compound of desire in analyzed substances. Based on electron impact ionization mass spectra an attempt to estimate their exact structures was made. The results of structure elucidation were confirmed by more detailed fragmentation studies based on (MS)² and (MS)³ electrospray ionization mass spectra.

Keywords:

• Thioacridine derivatives
• Capillary liquid chromatography
• Gas chromatography
• Mass spectrometry

ACKNOWLEDGMENTS

This study was supported by COST grant no. 49/208028 and by research project J13/98:l13100002. The authors would like to thank Prof. Jacques Barbe (Gerctop Ura CNRS 1411, Faculté de Pharmacie, Marseille) for synthesizing the studied thioacridine derivatives and Dr. Pavel Coufal (Charles University, Faculty of Science, Prague) for kindly providing CLC components and helpful discussion.

Notes

^aDetermined by internal normalization method.

^bStandard deviation evaluated for three consecutive measurements.

^aDetermined by internal normalization method.

^bStandard deviation evaluated for three consecutive measurements.