Instituto Nacional Of Medicina Legal Delegacao Do Sul

Lisbon, Portugal

Instituto Nacional Of Medicina Legal Delegacao Do Sul

Lisbon, Portugal
SEARCH FILTERS
Time filter
Source Type

da Fonseca B.M.,University of Beira Interior | Moreno I.E.D.,University of Beira Interior | Magalhaes A.R.,University of Beira Interior | Barroso M.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | And 5 more authors.
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences | Year: 2012

A new, simple and sensitive method was described for the simultaneous determination of nicotine, cotinine and trans-3'-hydroxycotinine in oral fluid samples using solid-phase extraction and gas chromatography/tandem mass spectrometry (GC-MS/MS). This technique was developed using only 0.2. mL of sample, and deuterated analogues were used as internal standards. The method was found to be linear between 0.5 and 1000. ng/mL, with determination coefficients higher than 0.996 for all analytes. Intra- and interday precision and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. All analytes were stable in the samples for at least 24. h at room temperature, for at least 72. h at 25 °C in processed samples and for at least three freeze/thaw cycles. Absolute recoveries ranged from 89 to 92% for all analytes. GC-MS/MS has demonstrated to be a powerful tool for the simultaneous quantitation of the analytes, providing adequate selectivity and sensitivity. In addition, its performance characteristics allow its routine use in the analysis of biomarkers of tobacco smoke exposure, extending the window of analyte detection in nicotine cessation programs, using a sample amount as low as 0.2. mL of human oral fluid. © 2012 Elsevier B.V.


Moreno I.E.D.,University of Beira Interior | da Fonseca B.M.,University of Beira Interior | Barroso M.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | Costa S.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | And 2 more authors.
Journal of Pharmaceutical and Biomedical Analysis | Year: 2012

A method using microextraction by packed sorbent (MEPS) and high performance liquid chromatography-diode array detection (HPLC-DAD) is described for the determination of piperazine-type stimulants in human urine. The studied compounds were 1-benzylpiperazine (BZP), 1-(3-trifluoromethylphenyl) piperazine (TFMPP), 1-(3-chlorophenyl) piperazine (mCPP) and 1-(4-methoxyphenyl) piperazine (MeOPP); 1-(2-chlorophenyl)-piperazine (oCPP) was used as internal standard (IS).The factors which might influence the extraction were screened previously using the fractional factorial design approach, and none of them influenced significantly the process.The procedure was linear for concentrations ranging from 0.1 (lower limit of quantitation - LLOQ) to 5μg/mL, with determination coefficients (R 2) higher than 0.99 for all analytes in all runs. The limits of detection were 0.1μg/mL for BZP and TFMPP, while for MeOPP and mCPP 0.05μg/mL was obtained. Intra- and interday precision ranged from 1 to 14%, and accuracy was within a ±15% interval for all analytes, fulfilling the criteria normally accepted in bioanalytical method validation. Under the optimized conditions, extraction efficiency was higher than 80% for all analytes, except BZP (50%).MEPS showed to be a rapid (<2. min) and simple procedure for the determination of piperazine-type stimulants in human urine, allowing reducing the handling time and costs usually associated to this type of analysis. Furthermore, the fact that only 0.1. mL of sample is required make this method a valuable and powerful tool for drug monitoring in human urine in situations where those compounds are involved, for instance in forensic scenarios. © 2011 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
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.


Moreno I.E.D.,University of Beira Interior | da Fonseca B.M.,University of Beira Interior | Magalhaes A.R.,University of Beira Interior | Geraldes V.S.,University of Beira Interior | And 4 more authors.
Journal of Chromatography A | Year: 2012

This paper describes the analysis of piperazine-type stimulants [1-benzylpiperazine (BZP), 1-(3-trifluoromethylphenyl)piperazine (TFMPP), 1-(3-chlorophenyl)piperazine (mCPP) and 1-(4-methoxyphenyl)piperazine (MeOPP)] in low volume urine samples (0.1mL) by microextraction in packed sorbent and liquid chromatography-diode array detection. Analyte extraction has been comprehensively optimized, and the influencing factors were screened by means of the fractional factorial design approach. Several parameters susceptible of influencing the process were studied, and these included extraction sorbent type (C8 and C18), sample dilution (1:2 and 1:4), number of aspirations through the device (2 and 8) and the amount of methanol on both the washing (0 and 10%) and eluting solvents (10 and 100%). The method was linear from 0.5 (lower limit of quantitation) to 5μgmL-1, with determination coefficients higher than 0.99 for all compounds. Intra- and interday precision ranged from 1 to 9%, trueness was within a ±11% interval for all analytes, and analyte recoveries were of about 70% for mCPP and TFMPP, and of about 10% for MeOPP and BZP. The method has shown to be selective, as no interferences from endogenous substances were detected by analysis of blank samples, and the analytes were stable in the samples for short periods at room temperature, after three freeze/thaw cycles and in processed samples. Due to its simplicity and speed, this method can be successfully applied in the screening and quantitation of these compounds in urine samples, and is suitable for application in forensic toxicology routine analysis. © 2011 Elsevier B.V.


Moreno I.,University of Beira Interior | Da Fonseca B.,University of Beira Interior | Oppolzer D.,University of Beira Interior | Martinho A.,University of Beira Interior | And 4 more authors.
Bioanalysis | Year: 2013

Background: The aim of this work was to develop and validate a method for the determination of Salvinorin A in human urine using microextraction by packed sorbent (MEPS) and GC-MS/MS. Results: The technique uses a sample volume as low as 0.2 ml, and the analyte was extracted using a C18 sorbent. The method showed to be linear between 20 and 1000 ng/ml and presented a LOD of 5 ng/ml. Intra- and inter-day precision and accuracy were acceptable. Absolute recoveries ranged from 71 to 80%. Conclusion: GC-MS/MS with MEPS demonstrated to be a fast and simple procedure for the quantification of Salvinorin A in urine. This is the first time that GC-MS/MS with MEPS was used for the determination of this compound in biological fluids. Furthermore, the device could be reused for up to 80 extractions, which accounted for a lower cost of analysis. © 2013 Future Science Ltd.


Da Fonseca B.M.,University of Beira Interior | Moreno I.E.D.,University of Beira Interior | Barroso M.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | Costa S.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | And 2 more authors.
Analytical and Bioanalytical Chemistry | Year: 2013

A method using microextraction by packed sorbent (MEPS) and gas chromatography-tandem mass spectrometry (GC-MS/MS) is described for the determination of seven antipsychotic drugs in human plasma. The studied compounds were chlorpromazine (CPZ), haloperidol (HAL), cyamemazine, quetiapine, clozapine, olanzapine (OLZ), and levomepromazine; promazine, protriptyline, and deuterated CPZ were used as internal standards. The validation parameters included selectivity, linearity and limits of detection and quantitation, intra- and interday precision and trueness, recovery, and stability and were studied according to internationally accepted guidelines. The method was found to be linear between the lower limit of quantitation and 1000 ng/mL, except for OLZ and HAL (200 ng/ mL), with determination coefficients higher than 0.99 for all analytes, and extraction efficiencies ranged from 62 to 92 %. Intra- and interday precision ranged from 0.24 to 10.67 %, while trueness was within a ±15 % interval from the nominal concentration for all analytes at all studied levels. MEPS has shown to be a rapid procedure for the determination of the selected antipsychotic drugs in human plasma, allowing reducing the handling time and the costs of analysis. Furthermore, GC-MS/MS has demonstrated to be a powerful tool for the simultaneous quantitation of the studied compounds, enabling obtaining adequate selectivity and sensitivity using a sample volume of as low as 0.25 mL. © Springer-Verlag Berlin Heidelberg 2012.


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.


Barroso M.,Instituto Nacional Of Medicina Legal Delegacao Do Sul | Moreno I.,University of Beira Interior | Da Fonseca B.,University of Beira Interior | Queiroz J.A.,University of Beira Interior | Gallardo E.,University of Beira Interior
Bioanalysis | Year: 2012

The last two decades have provided analysts with more sensitive technology, enabling scientists from all analytical fields to see what they were not able to see just a few years ago. This increased sensitivity has allowed drug detection at very low concentrations and testing in unconventional samples (e.g., hair, oral fluid and sweat), where despite having low analyte concentrations has also led to a reduction in sample size. Along with this reduction, and as a result of the use of excessive amounts of potentially toxic organic solvents (with the subsequent environmental pollution and costs associated with their proper disposal), there has been a growing tendency to use miniaturized sampling techniques. Those sampling procedures allow reducing organic solvent consumption to a minimum and at the same time provide a rapid, simple and cost-effective approach. In addition, it is possible to get at least some degree of automation when using these techniques, which will enhance sample throughput. Those miniaturized sample preparation techniques may be roughly categorized in solid-phase and liquid-phase microextraction, depending on the nature of the analyte. This paper reviews recently published literature on the use of microextraction sampling procedures, with a special focus on the field of forensic toxicology. © 2012 Future Science Ltd.

Loading Instituto Nacional Of Medicina Legal Delegacao Do Sul collaborators
Loading Instituto Nacional Of Medicina Legal Delegacao Do Sul collaborators