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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 30, Issue 6, July/August 2006,
pp.375-379
GC–MS–MS Determination of Gamma-Hydroxybutyrate
in Blood and Urine
Richard Paul[1], Lolita Tsanaclis[2], Robert Kingston[2], Anthony Berry[1],
and Alan Guwy[1]
[1]University of Glamorgan, Pontypridd, CF37 1DL, Wales and
[2]TrichoTech, Limited., No. 1 Pentwyn Business Centre, Cardiff, CF23 7HB, Wales
A gas chromatographic–tandem mass spectrometric (GC–MS–MS)
method for determining trace concentrations of gamma-hydroxybutyrate (GHB) in
blood and urine has been developed. Multiple reaction monitoring was used to
detect parent and daughter ions of GHB, 233 and 147, respectively, following
liquid–liquid extraction with acetonitrile and derivatisation with N,O-bis[trimethylsilyl]trifluoroacetamide
(BSTFA). Deuterated GHB was used as an internal standard. The assay produced
excellent linearity and sensitivity without conversion to gamma butyrolactone.
The lower limit of quantitation (LLOQ) in 50 µL of sample was 2.5 µg/mL.
The expanded uncertainty values for intra- and interassay results were ±
0.097 and ± 0.123 ng/mL at a confidence level of 95% for blood and urine,
respectively. Endogenous concentrations of GHB were found to be in the range
of 0.3 to 6 µg/mL in urine and 0.5 to 2.3 µg/mL in blood, confirming
previously suggested cut-off values for forensic analysis.
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