Comparative Analysis of Gamma-Hydroxybutyrate and Gamma-Hydroxyvalerate Using GC/MS and HPLC

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Abstract:

ABSTRACT:

This paper describes two analytical techniques used to separate and quantify gamma-hydroxybutyrate (GHB) and gamma-hydroxyvalerate (GHV). The first technique was a N,O-bis(trimethylsilyl)triflouro-acetimide–trimethylchlorosilane derivatization, followed by gas chromatography/mass spectrometry analysis using an HP-5 capillary column at a rate of 1.0 mL/min with a run time of 9.25 min. This technique was found to be sensitive (LOD 1 pg on column) and gave a low average error (5%) in a beverage study. When supplemented by a surrogate spike, the method yielded 97% analyte recovery from beverages. The second technique was high-performance liquid chromatography/UV (HPLC/UV) using a C-18 column with a (20:80% v/v) methanol:dibasic phosphoric buffer (10 mM, pH 3) at a rate of 1.00 mL/min with a run time of 7.5 min. UV detection occurred at 254 nm. This method was found to be less sensitive (LOD 0.05 g on column) for direct analysis of aqueous samples. To remove interferences seen in the beverage study, a liquid–liquid extraction before HPLC analysis was tested. However, a decreased sensitivity (LOD 100 g on column) and irreproducible peak profiles resulted.

Keywords: 4-methyl gamma-hydroxybutyrate; beverage; drug analysis; drug-facilitated sexual assault; forensic science; gamma-hydroxybutyrate; gamma-hydroxyvalerate; gas chromatography; high-performance liquid chromatography; surrogate spike

Document Type: Research Article

DOI: http://dx.doi.org/10.1111/j.1556-4029.2007.00392.x

Affiliations: C. Eugene Bennett Department of Chemistry, West Virginia University, 217 Clark Hall, Morgantown, WV 26056.

Publication date: March 1, 2007

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