ISSN: 0022-1198
CODEN: JFSCA
Page Count: 6

Determination of Gamma-hydroxybutyrate in Water and Human Urine by Solid Phase Microextraction-Gas Chromatography/Quadrupole Ion Trap Spectrometry
Hall, B
University of Texas at Austin, TX

Brodbelt, J
University of Texas at Austin, TX

Song, M
University of Texas at Austin, TX

Blair, S
University of Texas at Austin, TX

(Received 31 March 2000; accepted 16 June 2000)

Abstract

A simple method of detection was developed for gamma-hydroxybutyrate (GHB). The method involves the derivatization of GHB using a hexyl-chloroformate procedure in aqueous media (such as water or urine), extraction of the derivatization product directly from the sample using solid-phase microextraction, and subsequent separation and detection with gas chromatography quadrupole ion trap mass spectrometry. The deuterated form of GHB (GHB-D⁶) is used as an internal standard for quantitation. The method was linear for GHB-spiked pure water samples from 2 to 150 µg/mL GHB with a detection limit of 0.2 µg/mL. Spiked urine samples showed linearity from 5 to 500 µg/mL GHB with a detection limit of 2 µg/mL. The SPME-GC/MS method is applied to actual case samples, and the results are compared to those values obtained using a conventional GC/MS method. Sensitivity and linearity are comparable to those seen using traditional methods of separation, yet the SPME method is superior due to the simplicity, speed of analysis, reduction in solvent waste, and ability to differentiate between GHB and gamma-butyrolactone (GBL).

Keywords:
forensic science, gas chromatography/mass spectrometry, solid phase microextraction, quadrupole ion trap, gamma-hydroxybutyrate, hexyl-chloroformate derivatization

Paper ID: JFS15023J
DOI: 10.1520/JFS15023J
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