MICROWAVE-INDUCED RAPID PREPARATION OF FLUORO-DERIVATIVES OF AMPHETAMINE, METHAMPHETAMINE, AND 3,4-METHYLENEDIOXYMETHAMPHETAMINE FOR GC-MS CONFIRMATION ASSAYS
Wc. Thompson et A. Dasgupta, MICROWAVE-INDUCED RAPID PREPARATION OF FLUORO-DERIVATIVES OF AMPHETAMINE, METHAMPHETAMINE, AND 3,4-METHYLENEDIOXYMETHAMPHETAMINE FOR GC-MS CONFIRMATION ASSAYS, Clinical chemistry, 40(9), 1994, pp. 1703-1706
We prepared trifluoroacetyl, pentafluoropropyl, and heptafluorobutyl d
erivatives of amphetamine, methamphetamine, and 3,4-methylenedioxymeth
amphetamine (MDMA) in 45 s, 1 min, and 6 min, respectively, by using m
icrowave irradiation. Conventional techniques require heating the reac
tion mixture for 15 min at 40 degrees C for trifluoroacetyl derivative
s, 15 min at 75 degrees C for pentafluoropropyl derivatives, and 40 mi
n at 60 degrees C for heptafluorobutyl derivatives. The mass-spectral
fragmentation patterns and the gas-chromatographic retention times of
the derivatives obtained by both microwave irradiation and conventiona
l heating were similar. Perfluorooctanoyl derivatives of amphetamine c
an be prepared quantitatively by either heating the reaction mixture f
or 30 min at 60 degrees C or by 1 min of microwave irradiation. Conver
sion of methamphetamine and MDMA to the corresponding perfluorooctanoy
l derivatives was not quantitative by either technique, although the y
ield of the derivative in the conventional technique was much higher.