LC/ESI-MS/MS method for quantification of 28 synthetic cannabinoids in neat oral fluid and its application to preliminary studies on their detection windows

• Published in: Analytical and bioanalytical chemistry Vol. 405; no. 14; pp. 4691 - 4706
• Main Authors: Kneisel, Stefan, Speck, Michael, Moosmann, Bjoern, Corneillie, Todd M., Butlin, Nathaniel G., Auwärter, Volker
• Format: Journal Article
• Language: English
• Published: Berlin/Heidelberg Springer-Verlag 01.05.2013; Springer; Springer Nature B.V
• Subjects: Abstinence; Analytical Chemistry; Biochemistry; Blood; Cannabinoids; Cannabinoids - analysis; Cannabinoids - chemistry; Characterization and Evaluation of Materials; Chemical properties; Chemistry; Chemistry and Materials Science; Chromatography, Liquid - methods; Complex Mixtures - analysis; Complex Mixtures - chemistry; Drug withdrawal; Fluid dynamics; Fluid flow; Fluids; Food Science; Identification and classification; Ionization; Laboratory Medicine; Limit of Detection; Liquid chromatography; Mass spectrometry; Mathematical analysis; Metabolites; Methods; Monitoring/Environmental Analysis; Pharmaceutical chemistry; Phenyls; Pilot Projects; Psychotropic drugs; Reproducibility of Results; Research Paper; Saliva - chemistry; Spectrometry, Mass, Electrospray Ionization - methods; Substance Abuse Detection - methods; Tandem Mass Spectrometry - methods; Urine; Germany; United States > US; Spice; Neat oral fluid; LC/ESI-MS/MS; Synthetic cannabinoids; Detection window
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-013-6887-0

Serum and urine samples are commonly used for the analysis of synthetic cannabinoids in biofluids; however, their utilization as analytical matrices for drug abstinence control features some substantial drawbacks. While for blood collection invasive sampling is inevitable, the urinary analysis of synthetic cannabinoids is limited by the lack of available reference standards of the respective major metabolites. Moreover, the long detectability of synthetic cannabinoids in both matrices hampers the identification of a recent synthetic cannabinoid use. This article describes the development, validation and application of an LC/ESI-MS/MS method for the quantification of 28 synthetic cannabinoids in neat oral fluid (OF) samples. OF samples were prepared by protein precipitation using ice-cold acetonitrile. Chromatographic separation was achieved by gradient elution on a Luna Phenyl Hexyl column (50 × 2 mm, 5 μm), while detection was carried out on a QTrap 4000 instrument in positive ionization mode. The limits of detection ranged from 0.02 to 0.40 ng/mL, whereas the lower limits of quantification ranged from 0.2 to 4.0 ng/mL. The method was applied to authentic samples collected during two preliminary studies in order to obtain insights into the general detectability and detection windows of synthetic cannabinoids in this matrix. The results indicate that synthetic cannabinoids are transferred from the blood stream into OF and vice versa only at a very low rate. Therefore, positive OF samples are due to contamination of the oral cavity during smoking. As these drug-contaminations could be detected up to approximately 2 days, neat oral fluid appears to be well suited for detection of a recent synthetic cannabinoid use. Quantification of synthetic cannabinoids in biofluids by means of LC/ESI-MS/MS