San Sebastián de los Reyes, Spain
San Sebastián de los Reyes, Spain

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Barroso M.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | Dias M.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | Vieira D.N.,Instituto Nacional Of Medicina Legal | LoPez-Rivadulla M.,Instituto Universitario Of Medicina Legal | Queiroz J.A.,University of Beira Interior
Biomedical Chromatography | Year: 2010

A simple and rapid method for the determination of methadone and its main metabolite EDDP in hair has been developed and validated. The analytes were completely extracted from the matrix after a short alkaline incubation, and the extracts were further cleaned up by solid-phase extraction using mixed-mode cartridges. Linearity was obtained from 0.1 (lower limit of quantitation, LLOQ) to 30-ng/mg for both compounds, with correlation coefficients higher than 0.99. Intra- and interday precision and accuracy were in conformity with internationally accepted guidelines for bioanalytical method validation, and the cleanup procedure presented mean extraction efficiencies higher than 90% for both analytes. This high efficiency greatly contributed to the low limits of quantitation achieved, and therefore this method can be successfully applied in the determination of methadone and EDDP in hair samples in clinical and forensic scenarios where these compounds are involved. Copyright © 2010 John Wiley & Sons, Ltd.


Barroso M.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | Costa S.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | Dias M.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | Vieira D.N.,Instituto Nacional Of Medicina Legal | And 2 more authors.
Journal of Chromatography A | Year: 2010

A simple and sensitive procedure, using p-tolylpiperazine (pTP) as internal standard (IS), has been developed and validated for the qualitative and quantitative analysis of 1-(3-trifuoromethylphenyl)piperazine (TFMPP), 1-(3-chlorophenyl)piperazine (mCPP) and 1-(4-methoxyphenyl)piperazine (MeOPP) in hair. Drug extraction was performed by incubation with 1M sodium hydroxide at 50°C for 40min, and the extracts were cleaned up using mixed-mode solid-phase extraction. The analytes were derivatized with N-methyl-N-(trimethylsilyl) trifluoroacetamide with 5% trimethylchlorosilane and analysed by gas chromatography-mass spectrometry in the selected ion monitoring mode. The method was linear from 0.05 (lower limit of quantitation) to 4ngmg-1, with correlation coefficients higher than 0.99 for all the compounds. Intra- and interday precision and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation, and the sample cleanup step presented a mean efficiency higher than 90% for all the analytes. Due to its simplicity and speed, this method can be successfully applied in the screening and quantitation of these compounds in hair samples, and is suitable for application in forensic toxicology routine analysis. © 2010 Elsevier B.V.


Barroso M.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | Dias M.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | Vieira D.N.,Instituto Nacional Of Medicina Legal | Lopez-Rivadulla M.,Instituto Universitario Of Medicina Legal | Queiroz J.A.,University of Beira Interior
Analytical and Bioanalytical Chemistry | Year: 2010

A simple procedure has been developed and validated for the qualitative and quantitative analysis of several opiates (morphine, 6-acetylmorphine, codeine, 6-acetylcodeine) and tramadol in hair. The analytes were extracted from within the matrix via an overnight incubation with methanol at 65 °C, and afterwards the samples were cleaned up by mixed-mode solid-phase extraction. The extracts were derivatized with N-methyl-N-(trimethylsilyl) trifluoroacetamide with 5% trimethylchlorosilane and analyzed by gas chromatography-mass spectrometry in the selected ion monitoring mode. The method was linear from 0.05 (lower limit of quantitation) to 50 ng/mg (40 ng/mg for tramadol), with correlation coefficients higher than 0.99 for all compounds, accomplishing the cut-off values proposed by the Society of Hair Testing for the detection of these substances in hair (0.2 ng/mg). Intra- and interday precision and trueness were in conformity with the criteria normally accepted in bioanalytical method validation, and the sample cleanup step presented a mean efficiency higher than 90% for all analytes. Furthermore, using these incubation conditions, 6-acetylmorphine did not significantly hydrolyze to morphine. For these reasons, and because of its simplicity, the proposed method can be successfully applied in the determination of these compounds in hair samples, and is suitable for application in routine analysis with forensic purposes. © 2010 Springer-Verlag.


Barroso M.,Instituto Nacional Of Medicina Legal | Gallardo E.,University of Beira Interior | Vieira D.N.,Instituto Nacional Of Medicina Legal | Lopez-Rivadulla M.,Instituto Universitario Of Medicina Legal | Queiroz J.A.,University of Beira Interior
Bioanalysis | Year: 2011

Hair has been used for years in the assessment and documentation of human exposure to drugs, as it presents characteristics that make it extremely valuable for this purpose, namely the fact that sample collection is performed in a noninvasive manner, under close supervision, the possibility of collecting a specimen reflecting a similar timeline in the case of claims or suspicion of a leak in the chain of custody, and the increased window of detection for the drugs. For these reasons, testing for drugs in hair provides unique and useful information in several fields of toxicology, from which the most prominent is the possibility of studying individual drug use histories by means of segmental analysis. This paper will review the unique role of hair as a complementary sample in documenting human exposure to drugs in the fields of clinical and forensic toxicology and workplace drug testing. © 2011 Future Science Ltd.


Barroso M.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | Gallardo E.,University of Beira Interior | Vieira D.N.,Instituto Nacional Of Medicina Legal Largo Da Se Nova | Queiroz J.A.,University of Beira Interior | Lopez-Rivadulla M.,Instituto Universitario Of Medicina Legal
Analytical and Bioanalytical Chemistry | Year: 2011

The use and abuse of illegal drugs affects all modern societies, and therefore the assessment of drug exposure is an important task that needs to be accomplished. For this reason, the reliable determination of these drugs and their metabolites in biological specimens is an issue of utmost relevance for both clinical and forensic toxicology laboratories in their fields of expertise, including in utero drug exposure, driving under the influence of drugs and drug use in workplace scenarios. Most of the confirmatory analyses for abused drugs in biological samples are performed by gas chromatographic-mass spectrometric methods, but use of the more recent and sensitive liquid chromatography-(tandem) mass spectrometry technology is increasing dramatically. This article reviews recently published articles that describe procedures for the detection of opiates in the most commonly used human biological matrices, blood and urine, and also in unconventional ones, e.g. oral fluid, hair, and meconium. Special attention will be paid to sample preparation and chromatographic analysis. © 2011 Springer-Verlag.


Bermejo Barrera A.M.,Instituto Universitario Of Medicina Legal | Tabernero Duque M.J.,Instituto Universitario Of Medicina Legal
Revista Espanola de Medicina Legal | Year: 2011

The determination of drugs of abuse in hair is now a routine technique in forensic toxicology laboratories following the Society of Hair Testing recommendations in 2004. It is an alternative biological sample that is, easily obtained, difficult to adulterate, does not require special storage conditions, and, furthermore, it demonstrates shows consumption prior to obtaining a blood or urine sample. For this reason, its applications are increasing in number, including the possibility of determining markers of chronic ethyl alcohol use. However, the analytical methods are not yet standardized; therefore, a correct interpretation of results must be performed, and the limitations of this biological sample must be taken into account. © 2011 Asociacion Nacional de Medicos Forenses. Published by Elsevier Espana, S.L. All rights reserved.

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