SIMULTANEOUS DETERMINATION OF AMPHETAMINE AND ITS ANALOGS IN HUMAN WHOLE-BLOOD BY GAS-CHROMATOGRAPHY MASS-SPECTROMETRY

A sensitive and specific gas chromatography-mass spectrometry (GC-MS) method for the determination of amphetamine (AM), methamphetamine (MA) , methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA ) and methylenedioxyethylamphetamine (MDEA) in whole blood was designe d, using the respective pentadeuterated analogs of the analytes as int ernal standards (I.S.). After alkalinisation of blood samples, the amp hetamines were extracted using diethyl ether, derivatized with heptafl uorobutyric anhydride, then purified by successive washings with deion ized water and 4% NH4OH. Extraction recoveries were 85.2% for AM, 90.9 % for MA, 76.5% for MDA, 84.1% for MDMA and 63.6% for MDEA. Chromatogr aphic separation was performed on a non-polar 30 mx0.32 mm HP 5 MS cap illary column using a temperature program. Detection was carried out i n the electron-impact, selected ion-monitoring mode, using three mass- to-charge ratios for each analyte and one for each I.S. Limits of dete ction ranged from 0.5 to 8 ng/ml and limits of quantification were 10 ng/ml for AM, MDMA and MDEA; 20 ng/ml for MA; and 50 ng/ml for MDA. Th e method was linear from this limit up to 1000 ng/ml for all analytes, with good intra-assay precision and good intermediate precision and a ccuracy over these ranges. There was no interferences from other sympa thomimetic drugs such as ephedrine, norephedrine or methoxyphenamine. This method is thus suitable for clinical and forensic toxicology, as well as for doping control. (C) 1997 Elsevier Science B.V.