title: Quantitative analysis of delta9-tetrahydrocannabinol in preserved oral fluid by liquid chromatography-tandem mass spectrometry.
abstract: A rapid and sensitive method for the analysis of delta9-tetrahydrocannabinol (THC) in preserved oral fluid was developed and fully validated. Oral fluid was collected with the Intercept, a Food and Drug Administration (FDA) approved sampling device that is used on a large scale in the U.S. for workplace drug testing. The method comprised a simple liquid-liquid extraction with hexane, followed by liquid chromatography-tandem mass spectrometry (LC-MS-MS) analysis. Chromatographic separation was achieved using a XTerra MS C18 column, eluted isocratically with 1 mM ammonium formate-methanol (10:90, v/v). Selectivity of the method was achieved by a combination of retention time, and two precursor-product ion transitions. The use of the liquid-liquid extraction was demonstrated to be highly effective and led to significant decreases in the interferences present in the matrix. Validation of the method was performed using both 100 and 500 MicroL of oral fluid. The method was linear over the range investigated (0.5-100 ng/mL and 0. 1-10 ng/mL when 100 and 500 microL, respectively, of oral fluid were used) with an excellent intra-assay and inter-assay precision (relative standard deviations, RSD <6%) for quality control samples spiked at a concentration of 2.5 and 25 ng/mL and 0.5 and 2.5 ng/mL, respectively. Limits of quantification were 0.5 and 0.1 ng/mL when using 100 and 500 microL, respectively. In contrast to existing GC-MS methods, no extensive sample clean-up and time-consuming derivatisation steps were needed. The method was subsequently applied to Intercept samples collected at the roadside and collected during a controlled study with cannabis.
authors.affiliation: National Institute of Criminalistics and Criminology, Section Toxicology, Vilvoordsesteenweg 98, 1120 Brussels, Belgium. marleen.laloup@just.fgov.be
authors.forename: Marleen
authors.initials: M
authors.lastname: Laloup
authors.forename: Maria del Mar
authors.initials: Mdel M
authors.lastname: Ramirez Fernandez
authors.forename: Michelle
authors.initials: M
authors.lastname: Wood
authors.forename: Gert
authors.initials: G
authors.lastname: De Boeck
authors.forename: Cécile
authors.initials: C
authors.lastname: Henquet
authors.forename: Viviane
authors.initials: V
authors.lastname: Maes
authors.forename: Nele
authors.initials: N
authors.lastname: Samyn
mesh_terms: D001826:Body Fluids / Q000737:chemistry*; D002853:Chromatography, Liquid / Q000379:methods*; D013759:Dronabinol / Q000032:analysis* / Q000302:isolation & purification; D004355:Drug Stability; D006801:Humans; D008385:Marijuana Smoking / Q000378:metabolism; D013058:Mass Spectrometry / Q000379:methods; D009055:Mouth / Q000737:chemistry*; D015203:Reproducibility of Results; D012463:Saliva / Q000737:chemistry; D012680:Sensitivity and Specificity; D013048:Specimen Handling / Q000379:methods
chemical_list: D013759:Dronabinol