Gas chromatography-mass spectrometry (GC-MS) and high-performance liquid chromatography/UV (HPLC/UV) were optimized for the simultaneous detection and quantitation of GHB and GHV in aqueous solutions. Derivatization, followed by GC-MS, was found to be a suitable technique for differentiating and quantifying GHB and GHC in aqueous solutions and beverages. Direct injection HPLC/UV was found to be suitable for the identification and quantitation of all analytes in aqueous solutions; however, the method was difficult to adapt to beverage analysis due to matrix interference. An extraction procedure was developed prior to HPLC analysis, but it had a significantly higher LOD and led to peak profiles that could not be reproduced. The derivatization of analytes, followed by the GC-MS analytical method was found to be best suited for forensic analysis of seized beverages believed to contain GHB and GHV. The use of a surrogate, in addition to an internal standard, was found to be an ideal application for forensic analyses. The similarities between GHB and GHV extend to synthesis from their analogs. When reacted with sodium hydroxide, gamma-valerolactone (GVL) and gamma-butyrolactone (GBL) undergo a saponification conversion to the sodium salts (NaGHB and NaGHV, respectively). These chemical similarities facilitate the formulation of accurate and sensitive confirmatory tests for simultaneous identification and quantification of GHB and GHV. Details on the materials and methods used in GC-MS and HPLC/UV are presented. 2 tables, 3 figures, and 17 references