Detection of ɣ‐hydroxybutyric acid (GHB) and ɣ‐butyrolactone (GBL) in alcoholic beverages via total vaporization solid‐phase microextraction (TV‐SPME) and gas chromatography–mass spectrometry.

Total Vaporization Solid‐Phase Microextraction (TV‐SPME) relies on the same technique as standard SPME but completely vaporizes a sample extract, and analytes are sorbed directly from the vapor phase. On‐fiber derivatization may also be performed using TV‐SPME, where the fiber is first exposed to the headspace of a vial containing the derivatization agent, then exposed to a new vial containing the sample. ɣ‐Hydroxybutyric acid (GHB) and ɣ‐butyrolactone (GBL) are drugs of concern in that they may be used in drug facilitated sexual assault by surreptitiously spiking them into a victim's beverage. These drugs cause sedation, memory loss, and are difficult to detect in biological samples. One challenge in their analysis is that they can interconvert in aqueous samples, which was demonstrated in samples allowed to stand at room temperature for long periods. A volume study of GBL in water was performed with volumes ranging from 1 to 10,000 µl to compare the efficacy of TV‐SPME, headspace SPME, and immersion SPME. Lastly, water, beer, wine, liquor, and mixed drinks were spiked with either GHB or GBL with realistic concentrations (mg/ml) and microliter quantities were analyzed using a TV‐SPME Gas Chromatography‐Mass Spectrometry method. The GBL volume study demonstrated an increased sensitivity in GBL detection when TV‐SPME was utilized. Additionally, GHB and GBL were identified in various beverages at realistic concentrations. Overall, TV‐SPME is beneficial because it requires no sample preparation and uses smaller sample volumes than immersion and headspace SPME. [ABSTRACT FROM AUTHOR]