Abstract
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.
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Acknowledgments
We would like to thank the EU Commission (JUST/2009/DPIP/AG/0948), the German Ministry of Health and the City of Frankfurt (Main) for funding the project ‘Spice and synthetic cannabinoids’. In addition, we would like to thank Ilmari Szilvay (Finnish Customs Laboratory), Andrea Jacobsen-Bauer (State Bureau of Criminal Investigation of Baden-Württemberg, Germany), Christian Vidal (State Bureau of Criminal Investigation of Niedersachsen, Germany) and Folker Westphal (State Bureau of Criminal Investigation of Schleswig-Holstein, Germany) for providing JWH-019, JWH-307, AM-2233, JWH-387, JWH-412 and the ortho isomer of RCS-4 as reference substances.
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Stefan Kneisel and Michael Speck contributed equally to this work.
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Kneisel, S., Speck, M., Moosmann, B. et al. 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. Anal Bioanal Chem 405, 4691–4706 (2013). https://doi.org/10.1007/s00216-013-6887-0
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DOI: https://doi.org/10.1007/s00216-013-6887-0