1. Validation of a method to detect cocaine and its metabolites in nails by gas chromatography–mass spectrometry
- Author
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Ovandir Alves Silva, Mauricio Yonamine, Simone Valente-Campos, and Regina Lúcia de Moraes Moreau
- Subjects
Detection limit ,Chromatography ,Coefficient of variation ,Reproducibility of Results ,Gas Chromatography-Mass Spectrometry ,Pathology and Forensic Medicine ,Norcocaine ,Substance Abuse Detection ,Matrix (chemical analysis) ,chemistry.chemical_compound ,Cocaine ,Nails ,chemistry ,Benzoylecgonine ,Humans ,Selected ion monitoring ,Gas chromatography ,Gas chromatography–mass spectrometry ,Law - Abstract
The objective of the present work was to compare previously published methods and provide validation data to detect simultaneously cocaine (COC), benzoylecgonine (BE) and norcocaine (NCOC) in nail. Finger and toenail samples (5mg) were cut in very small pieces and submitted to an initial procedure for external decontamination. Methanol (3 ml) was used to release analytes from the matrix. A cleanup step was performed simultaneously by solid-phase extraction (SPE) and the residue was derivatized with pentafluoropropionic anhydride/pentafluoropropanol (PFPA/PFP). Gas chromatography-mass spectrometry (GC-MS) was used to detect the analytes in selected ion monitoring mode (SIM). Confidence parameters of validation of the method were: recovery, intra- and inter-assay precision, as well as limit of detection (LOD) of the analytes. The limits of detection were: 3.5 ng/mg for NCOC and 3.0 ng/mg for COC and BE. Good intra-assay precision was observed for all detected substances (coefficient of variation (CV)
- Published
- 2006
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