This paper is dedicated to Professor António-Rocha Gonsalves on the Occasion of his 70 thBirthday. This work is a tribute to and also the result of his lifelong collaboration with several pharmaceutical companies in Portugal and abroad and his pioneering role in establishing the use of HPLC, MS and later LC-MS-MS both at some of those companies and at several research institutions, to study real and complex chemical problems.
AbstractAn efficient LC/MS/MS methodology for the analysis of Alprazolam API and Alprazolam tablets was developed. The analysis of the MS 2 fragmentation profile, obtained from only one chromatographic assay, allows the identification of Alprazolam, its main degradation product, triazoaminoquinoleine (Imp G), the analysis of the MS 3 spectra allows the identification of 5-chloro-[5-methyl-4H-1,2,4-triazol-4-yl]benzophenone (Imp C) and with SIM mode the 5-chloro-[2-(3-aminomethyl-5-methyl-1,2,4-triazol-4-yl]benzophenone, opened-ring Alprazolam, proposed as precursor of triazoaminoquinoleine in basic and acid hydrolysis and only detected before by NMR analysis, was identified. With this method it is possible to study samples with only one chromatographic run, identifying unequivocally the impurities present, taking advantage of the MS-MS resource.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.