Examination of Firearms Review: 2007 to 2010 - Interpol

ng/mL. The combination of the automated online SPE with LC-MS/MS can
significantly reduce time for sample preparation requirements. With the use of
tandem enzyme-alkaline hydrolysis, the total content of THC, 11-OH-THC, and
THC-COOH in urine could be determined by protein precipitation followed by
BSTFA deriviatization prior to GC-MS analysis. The calibration curves were
linear from 2.5 to 300 ng/mL for all analytes [339]. A two-dimensional GC-MS
(2D-GCMS) assay provides a new means of simultaneously quantifying
cannabidiol, THC, and metabolite biomarkers. Analytes were extracted from 1
mL of plasma by SPE, derivatized with N,O-bis(trimethylsilyl)
trifluoroacetamide with 1% trimethylchlorosilane, and analyzed by 2D-GCMS
with cryofocusing. The lowest points of calibration for all analytes were either
0.25 or 0.5 ng/mL [340].
With the use of pipette tip SPE with MonoTip C(18) tips for extraction of MA
and amphetamine from whole blood (0.1 mL), followed by derivatization with
trifluoroacetic anhydride, a GC-MS method was developed with LOD of 1.5
ng/mL for MA and 1.1 ng/mL for amphetamine [341]. An automated LC-MS/MS
method for the analysis of amphetamines (amphetamine, MA, MDMA, MDA,
MDEA, PMA, and ephedrine) using 100 and 50 µL of blood and urine,
respectively, was developed. The LOQs in blood and urine were 2.5 µg/L and
25 µg/L, respectively, and the runtime per sample was under 11 min [293].
A headspace GC-MS method was reported for the determination of GHB in
serum and urine by converting GHB to GBL in the presence of acid. The LODs
for serum and urine were 0.16 µg/mL and 0.17 µg/mL, respectively [342]. A
GC-MS method for quantitative determination of GHB and its precursors [GBL,
BD] in blood and/or urine samples was reported. GHB and BD were extracted
with tert-butylmethylether in test tubes preloaded with NaCl followed by acid
wash, solvent evaporation, and derivatization with MSTFA prior to GC-MS
analysis. When analyzing GBL, the salting-out step was omitted, and analysis
was performed with a GC-FID apparatus [343].
A UPLC-MS/MS method was validated for the confirmation and quantitation of
LSD, iso-LSD, N-demethyl-LSD (nor-LSD), and 2-oxo-3-hydroxy-LSD
(O-H-LSD) [344]. LOQs in blood and urine were 20 pg/mL for LSD and iso-LSD
and 50 pg/mL for nor-LSD and O-H-LSD. This was the first reported detection
of O-H-LSD in blood from a suspected LSD user.
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