RT Journal Article T1 Rapid Analytical Method for Quantification of Gamma-Hydroxybutyrate (GHB) in Hair by UPLC-MS/MS A1 Blanco-Ces, Miriam A1 Castro Ríos, Ana de A1 López Rabuñal, Ángela A1 Cobo Golpe, María A1 Cruz Landeira, Angelines A1 Lendoiro Belío, Elena K1 Alternative matrix K1 Drug-facilitated crime K1 GHB K1 Hair K1 UPLC-MS/MS AB Gamma-hydroxybutyrate (GHB), an endogenous compound related to the neurotransmitter gamma-aminobutyric acid (GABA), is used as a therapeutic and recreational drug and as a “weapon” in drug-facilitated crimes. The very short window of detection of GHB in conventional matrices (blood and urine) makes necessary the use of alternative matrices like hair. Hair has a long window of detection and the possibility to perform segmental analysis, which makes it very useful for proving GHB intake. In the present work, a method for quantification of GHB in hair was developed and validated. Hair (10 mg) was washed twice with dichloromethane and then incubated at room temperature with Milli-Q water in an ultrasound bath for 30 min. Analysis was performed by UPLC-MS/MS using a CORTECS UPLC HILIC (1.6 μm), 2.1 × 100-mm column, and a gradient with acetonitrile and ammonium acetate (10 mM) at pH 6.0, with a total run-time of 10 min. For detection, a triple quadrupole mass spectrometer in ESI negative mode was used. The method was validated, following the criteria established in the “AAFS Standard Practices for Method Validation in Forensic Toxicology” guideline, obtaining satisfactory results for linearity (0.5–50 ng/mg), accuracy (95.0%–103.2%), imprecision (< 10.2%), limit of detection (0.1 ng/mg) and quantification (0.5 ng/mg), exogenous selectivity (no interferences), matrix effect (less than −44.2%), extraction efficiency (> 86.4%), process efficiency (> 46.1%), and autosampler stability (< 4.3%). The method was used for the analysis of 26 authentic hair samples, 25 from non–drug users, obtaining values between < LOQ and 6.25 ng/mg of endogenous GHB and 1 from a former GHB chronic user to prove abstinence. PB Wiley SN 1942-7603 YR 2024 FD 2024-09-15 LK https://hdl.handle.net/10347/39836 UL https://hdl.handle.net/10347/39836 LA eng NO Blanco-Ces, M., de-Castro-Rios, A., Lopez-Rabuñal, A., Cobo-Golpe, M., Cruz, A. and Lendoiro, E. (2024), Rapid Analytical Method for Quantification of Gamma-Hydroxybutyrate (GHB) in Hair by UPLC-MS/MS. Drug Test Anal. https://doi.org/10.1002/dta.3798 NO M.C.- G. thanks the Universidade of Santiago de Compostela for her “Convocatoria de Recualificación do Sistema Universitario Español-Margarita Salas” postdoc grant under the “Plan de Recuperación Transformación” program funded by the Spanish Ministry of Universities with theEuropean Union's NextGenerationEU funds. Moreover, the authors would like to thank the Xunta de Galicia (Galicia, Spain) for the Consolidation andStructuring of Competitive Research Units Help (2021-PG054) DS Minerva RD 25 abr 2026