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Clauwaert et al. applied the LC/ESI/TOF/MS for quantitative measure-
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ments of MDMA and its metabolite MDA in whole blood, serum, vitreous
humor, and urine. The LOQ was 1 mg/l and the linear dynamic range
extended over four decades. It was concluded that this technique achieves
the linear dynamic range for LC/ESI/MS/MS. The same group determined
MDMA, MDEA, and MDA in whole blood, urine, and vitreous humor of
rabbits using HPLC with fluorometric and tandem mass spectrometric detec-
tion. The LOD for fluorometric detection was 0.8 mg/l in blood and 2 mg/l
in urine. Very good correlation between both methods was found. The meth-
ods were used for a thanatochemical distribution study in rabbits. 74
Paramethoxyamphetamine (PMA) is a new designer amphetamine of
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relatively high toxicity. Mortier et al. described the method for determina-
tion of PMA together with amphetamine, MDMA, MDEA, and MDA in
biological fluids. Solvent extraction followed by sonic spray LC/MS(IT) was
applied. The matrix suppression was measured and was negligible for human
urine and liver or kidney.
Several therapeutic drugs act as amphetamine/methamphetamine pre-
cursors, and it is important to differentiate between the administration of
these drugs and illicit preparations. LC/MS has been applied for these pur-
poses. Benzphetamine (BMA) and its metabolites benzylamphetamine,
hydroxybenzphetamine, hydroxybenzylamphetamine, methamphetamine,
and amphetamine were isolated from urine with SPE, separated on an alka-
line mobile phase and detected with ESI/MS (SIM). The LODs were from
0.3 to 10 mg/l urine. This method allowed discrimination of the ingestion
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of BMA, amphetamine, and methamphetamine. Dimethylamphetamine and
its metabolites dimethylamine-N-oxide, methamphetamine, and amphet-
amine were determined in urine by ESI/LC/MS (SIM) after isolation with
SPE. LODs were 5 to 50 mg/l urine. 77
Selegiline, an inhibitor of monoamine oxidase-B used in the treatment
of Parkinson’s disease, is metabolized to methamphetamine and amphet-
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amine. Katagi et al. determined this drug as well as the specific metabolites
selegiline-N-oxide, methamphetamine, and amphetamine in human urine.
All compounds were isolated from urine using SPE C18 cartridges, separated
on a cation exchange column and subjected to ESI/MS detection in full scan
acquisition mode. In urine samples collected from selegiline patients, only
metabolites were detected. The method may serve for differentiation between
selegiline and methamphetamine intake. The excretion of selegiline-N-oxide
after selegiline administration in volunteers was studied with ESI/LC/MS. 79
2.3.2.2 Analysis of Alternative Samples
Wood et al. applied LC/ESI/MS/MS for determination of amphetamines
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(amphetamine, methamphetamine, MDMA, MDA, MDEA, and ephedrine)
© 2004 by CRC Press LLC