title: Simultaneous analysis of gamma-hydroxybutyric acid and its precursors in urine using liquid chromatography-tandem mass spectrometry.
abstract: We have developed a rapid method that enables the simultaneous analysis of gamma-hydroxybutyrate (GHB) and its precursors, i.e. gamma-butyrolactone (GBL) and 1,4-butanediol (1,4-BD) in urine. The method comprised a simple dilution of the urine sample, followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. Chromatographic separation was achieved using an Atlantis dC18 column, eluted with a mixture of formic acid and methanol. The method was linear from 1-80 mg/L for GHB and 1,4-BD and from 1-50 mg/L for GBL. The limit of quantification was 1 mg/L for all analytes. The procedure, which has a total analysis time (including sample preparation) of less than 12 min, was fully validated and applied to the analysis of 182 authentic urine samples; the results were correlated with a previously published GC-MS procedure and revealed a low prevalence of GHB-positive samples. Since no commercial immunoassay is available for the routine screening of GHB, this simple and rapid method should prove useful to meet the current increased demand for the measurement of GHB and its precursors.
authors.affiliation: Waters Corporation, MS Technologies Centre, Micromass UK Ltd., Atlas Park, Simonsway, Wythenshawe, Manchester M22 5PP, UK. michelle_wood@waters.com
authors.forename: Michelle
authors.initials: M
authors.lastname: Wood
authors.forename: Marleen
authors.initials: M
authors.lastname: Laloup
authors.forename: Nele
authors.initials: N
authors.lastname: Samyn
authors.forename: Michael R
authors.initials: MR
authors.lastname: Morris
authors.forename: Ernst A
authors.initials: EA
authors.lastname: de Bruijn
authors.forename: Robert A
authors.initials: RA
authors.lastname: Maes
authors.forename: Michael S
authors.initials: MS
authors.lastname: Young
authors.forename: Viviane
authors.initials: V
authors.lastname: Maes
authors.forename: Gert
authors.initials: G
authors.lastname: De Boeck
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006801:Humans; D006885:Hydroxybutyrates / Q000652:urine*; D013058:Mass Spectrometry / Q000379:methods*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D006885:Hydroxybutyrates; C111420:4-hydroxybutyric acid