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Chiral analysis of amphetamine-type stimulants using reversed-polarity capillary electrophoresis/positive ion electrospray ionization tandem mass spectrometry
Authors:Iwata Yuko T  Kanamori Tatsuyuki  Ohmae Yoshihito  Tsujikawa Kenji  Inoue Hiroyuki  Kishi Tohru
Affiliation:National Research Institute of Police Science, Chiba, Japan. togawa@nrips.go.jp
Abstract:Reversed-polarity (RP) capillary electrophoresis/positive ion electrospray ionization mass spectrometry (CE-ESI+ MS) and tandem mass spectrometry (MS/MS) were utilized for simultaneous chiral separation of nine amphetamine-type stimulants (ATS) (dl-norephedrine, dl-norpseudoephedrine, dl-ephedrine, dl-pseudoephedrine, dl-amphetamine, dl-methamphetamine, dl-methylenedioxyamphetamine, dl-methylenedioxymethamphetamine, and dl-methylenedioxyethylamphetamine). Using highly sulfated gamma-cyclodextrin (SU(XIII)-gamma-CD) as a chiral selector, the nine ATS were completely separated within 50 min. The migrated ATS-CD complex was dissociated at the ESI interface, and only ATS molecules went into the MS detector so that all 18 individual enantiomers were identified by their mass spectra. The detection limit of MS/MS was 10 times more sensitive than those for single MS. Seized d-methamphetamine hydrochloride samples dissolved at high concentration (20 mg/mL) were analyzed. Impurities originating in the precursor such as l-ephedrine and d-pseudoephedrine were detected and identified by tandem mass spectra.
Keywords:Amphetamine‐type stimulants  Chiral separation  Positive ion electrospray ionization  Reversed‐polarity capillary electrophoresis  Sulfated cyclodextrin
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