Mass spectrometric data characteristics of commonly abused amphetamines with sequential derivatization at two active...

There have been reports on improved chromatographic parameters derived from the incorporation of sequential derivatization in preparing biological specimens for the analysis of opiates. This current study was designed to characterize the mass spectrometric data resulting from sequential derivatizations of commonly abused amphetamines (along with all commercially available deuterated analogs) containing two active sites, i.e., amphetamine, methylenedioxyamphetamine, phenylpropanolamine. The first derivatization groups included in this study were trifluoroacetyl, pentafluoropropionyl, and heptafluorobutyryl, while t-butyldimethylsilyl was used as the second derivatization group. Products resulting from the first step and the two-step derivatization processes were analyzed by GC-MS. Full-scan mass spectrometric data were used to select ions with potential for designating the analytes and their respective isotopically labeled analogs in quantitative analysis protocols. Selected ion monitoring data were then collected and assessed to determine the quality of these ions when one or two different derivatization groups were incorporated in the sample preparation processes. A total of 77 full-scan mass spectra and 8 ion intensity cross-contribution tables, representing various forms of derivatization and isotopic analogs of the three amphetamines, are systematically presented for reference. Evaluations of these data concluded that many, but not all, products derived from "double derivatization" (sequential derivatization with two derivatization groups), generate ions of higher quality than those derived from "single derivatization".