Percorrer por autor "Rosendo, Luana M."
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- An Update on the Implications of New Psychoactive Substances in Public HealthPublication . Simão, Ana Y.; Antunes, Mónica; Cabral, Emanuel; Oliveira, Patrik; Rosendo, Luana M.; Brinca, Ana Teresa; Alves, Estefânia; Marques, Hernâni; Rosado, Tiago; Passarinha, Luís A.; Andraus, Maristela; Barroso, Mário; Gallardo, EugeniaThe emergence of new psychoactive substances has earned a great deal of attention, and several reports of acute poisoning and deaths have been issued involving, for instance, synthetic opiates. In recent years, there have been profound alterations in the legislation concerning consumption, marketing, and synthesis of these compounds; rapid alert systems have also been subject to changes, and new substances and new markets, mainly through the internet, have appeared. Their effects and how they originate in consumers are still mostly unknown, primarily in what concerns chronic toxicity. This review intends to provide a detailed description of these substances from the point of view of consumption, toxicokinetics, and health consequences, including case reports on intoxications in order to help researchers and public health agents working daily in this area.
- Determinação da cocaína e metabolitos em águas residuais com recurso à extração em fase sólida e à cromatografia de gases acoplada à espectrometria de massa em tandemPublication . Alves, Estefânia; Catarro, Gonçalo; Rosendo, Luana M.; Rosado, Tiago; Barroso, Mário; Gallardo, Eugenia; Araújo, André RTSA cocaína (COC) é a segunda droga mais consumida na Europa, causando graves problemas de saúde pública, tendo contribuído para um aumento de overdoses fatais relacionadas com o consumo de drogas de abuso1. A análise de águas residuais (AR’s) para determinar o consumo de drogas tem-se tornado cada vez mais comum devido ao seu custo reduzido, elevadas precisão e confiabilidade, e por recorrer a uma matriz ambiental, não invasiva, que apresenta baixa probabilidade de adulteração. Neste estudo, foi desenvolvido e validado um método para determinar COC e os metabolitos ecgonina metil éster (EME), benzoilecgonina (BEG), cocaetileno (COET), e norcocaína (NCOC) em AR’s, utilizando extração em fase sólida (SPE) e cromatografia gasosa acoplada à espectrometria de massas em tandem (GC-MS/MS). O método foi otimizado e validado de acordo com as normas internacionais de validação. Foi obtida uma linearidade de 0,00625-5 ng/mL para todos os analitos, tendo sido obtidos coeficientes de determinação superiores 0,9990. O limite inferior de quantificação (LLOQ) para todos os compostos foi de 0,00625 ng/mL. As precisões e exatidão intra-dia, inter-dia e intermédias apresentaram coeficientes de variação abaixo de 15%, e uma exatidão de ±15% para todos os compostos analisados. Além disso, o procedimento permitiu alcançar recuperações entre 72% e 115%. Salienta-se que este procedimento é o primeiro método que utiliza a SPE, com cartuchos Strata TM-X-C, combinada com GC-MS/MS para a determinação de COC e metabolitos em AR’s. Este método torna-se então uma alternativa adequada para a monitorização da COC e dos seus metabolitos em amostras de AR’s, demonstrando elevada importância ambiental e forense.
- Determinação de Ketamina e Norketamina em amostras de cabelo por microextração em seringa empacotada e GC-MS/MSPublication . Simão, Ana Y.; Oliveira, Patrik; Rosendo, Luana M.; Rosado, Tiago; Andraus, Maristela; Barroso, Mário; Gallardo, EugeniaAs novas substâncias psicoativas (NSP) continuam a representar um desafio considerável para a saúde pública e um problema para a sociedade. A ketamina (KET) é uma destas substâncias. O cabelo tem vindo a ser utilizado como uma matriz complementar à urina e ao sangue nas análises toxicológicas. A microextração em seringa empacotada (MEPS) tem vindo a ser mais utilizada em análises toxicológicas pelas diversas vantagens que apresenta, nomeadamente a redução do uso de solventes, rapidez e possibilidade de reutilização do adsorvente, sendo por isso economicamente mais apelativa que a clássica extração em fase sólida. Neste trabalho apresenta-se o desenvolvimento de um método de clean-up com recurso à MEPS para a determinação de KET e o seu metabolito norketamina (NK) em amostras de cabelo por cromatografia gasosa acoplada à espectrometria de massa em tandem (GCMS/ MS)
- Determination of Ketamine and Norketamine in hair samples using MEPS as sample clean-upPublication . Simão, Ana Y.; Oliveira, Patrik; Rosendo, Luana M.; Rosado, Tiago; Gallardo, Eugenia; Andraus, Maristela; Barroso, MárioIntroduction and Aim: The use of hair samples to determine ketamine (K) and its metabolite, norketamine (NK), has been studied by several authors, using different clean-up approaches. However, microextraction by packed sorbent (MEPS), a miniaturized form of the classic solid-phase extraction has not been applied to date for the purpose. Therefore, a method to determine K and NK in hair samples was developed, optimized, and validated using MEPS as sample clean-up. Materials & Methods: Hair samples were scissor-cut into small fragments, and rinsed with methanol to remove dirt and externally deposited material. Following an overnight incubation with methanol at 65 ºC (no stirring), the compounds were analysed by GC-MS/MS without the need of derivatization procedures; MEPS conditions were: conditioning (5 x 250 µL of methanol and 4 x 250 µL of deionized water); load (10 x 150 µL of hair extract); washing (50 µL of 0.1% acetic acid and 50 µL of 10% methanol); and elution (100 µL of 3% ammonium hydroxide in methanol). Results & Discussion: The procedure resulted in acceptable recoveries, 39-61% for K and 32-43% for NK, and allowed reaching limits of quantification (LOQs) of 50 pg/mg for both analytes. The analytical method presented acceptable accuracy and precision with coefficients of variation typically lower than 15% and BIAS within ± 15%, except at the LOQ (20%). The method was successfully applied to 2 authentic samples, and ketamine concentrations were below 0.05 and 0.18 ng/mg. Norketamine was not detected. Conclusions: This work is the first analytical method using MEPS coupled to GC-MS/MS for the determination of K and NK in hair samples. Following a comparison with a SPE-based method using authentic samples, it was considered rapid and suitable for routine analysis. Acknowledgments: FCT (UIDB /00709/2020 and UIDP/00709/2020). A.Y. Simão acknowledges the PhD fellowship from FCT (2020.09070.BD).
- Differentiation of selegiline metabolites and illicit methamphetamine and amphetamine use in elderly postmortem cases: Insights from LC-MS/MS and immunoassay techniquesPublication . Costa, Suzel; Rosendo, Luana M.; Barroso, Mário; Franco, João MiguelAbstract: Introduction: In forensic toxicology, distinguishing between pharmaceutical metabolites and illicit substances is crucial for accurate case interpretation. This study explores two post-mortem cases involving elderly individuals where methamphetamine and amphetamine were detected, raising initial concerns about illicit drug use. Aims: To demonstrate the application of liquid chromatography-tandem mass spectrometry (LC-MS/MS) and immunoassay techniques in differentiating between selegiline metabolites and illicit methamphetamine and amphetamine. Methods: Blood samples from three deceased elderly individuals (ages 91 and 89) were analyzed using LC-MS/MS for the quantitative detection of selegiline and metabolites. Initial screening revealed methamphetamine and amphetamine levels suggestive of potential illicit use. Immunoassay testing for dextro isomers (those associated with drug abuse) was subsequently performed to differentiate between isomers. Results and Discussion: LC-MS/MS analysis confirmed selegiline in both cases, with methamphetamine and amphetamine detected. Immunoassay results were negative for dextro isomers, indicating that the detected substances were L-isomers, which is consistent with selegiline metabolism rather than illicit use. Conclusion: This study highlights the critical role of combining LC-MS/MS and immunoassay techniques in forensic toxicology. The negative immunoassay results for dextro isomers clarified that the methamphetamine and amphetamine present were metabolic byproducts of selegiline therapy. Accurate differentiation between therapeutic and illicit substances is essential to avoid misinterpretation, particularly in elderly individuals, where illicit drug use is infrequent. These findings emphasize the need for comprehensive analytical approaches in forensic investigations to ensure accurate and reliable results.
- High concentrations of nordiazepam may impair the detection of benzoylecgonine by GC-MS with derivatizationPublication . Costa, Suzel; Rosendo, Luana M.; Barroso, Mário; Gallardo, EugeniaIntroduction: Forensic toxicology plays a pivotal role in legal investigations, particularly in detecting substances in biological samples. However, the simultaneous presence of multiple substances can pose analytical challenges. For instance, nordiazepam, a major metabolite of some benzodiazepines, can interfere with the detection of benzoylecgonine, a primary metabolite of cocaine, when using gas chromatography-mass spectrometry (GC-MS) with N- methyl-N-(trimethylsilyl) trifluoroacetamide (MSTFA) derivatization. This interference could result in false negatives for benzoylecgonine detection. Aims: This study aims to assess whether N-methyl-N-(tert-butyldimethylsilyl)-trifluoroacetamide (MBDSTFA) derivatization can reduce interference from nordiazepam, thereby improving the detection and quantification of benzoylecgonine in biological samples. Methods: Solid phase extraction (SPE) was carried out on post-mortem blood samples using Oasis® MCX columns. Microwave derivatization with MSTFA or MBDSTFA followed after the extracts were evaporated. Results and discussion: Two derivatization reagents, MSTFA and MBDSTFA, were compared using GC-MS to evaluate their effectiveness. For this assessment, both the limit of detection (LOD) and limit of quantification (LOQ) for benzoylecgonine in this chromatographic method were 10 and 25 ng/mL, respectively. MBDSTFA derivatization significantly reduced analytical interference between nordiazepam and benzoylecgonine. In contrast, MSTFA derivatization resulted in substantial interference at high concentrations of nordiazepam, potentially leading to false negatives for cocaine detection. These findings highlight the superior performance of MBDSTFA in complex toxicological analyses. Conclusion: MBDSTFA derivatization is more effective than MSTFA for minimizing interference in the detection of benzoylecgonine in the presence of nordiazepam. This method enhances the specificity of forensic toxicological analyses and helps prevent false negatives for detecting cocaine consumption through its principal metabolite, thereby supporting more reliable legal and clinical decisions.
- Microextraction action by packed sorbent in forensic drug analysisPublication . Rosado, Tiago; Pelixo, Rodrigo; Pires, Bruno; Catarro, João Miguel; Rosendo, Luana M.; Brinca, Ana T.; Antunes, Mónica; Soares, Sofia; Simão, Ana Y.; Barroso, Mário; Gallardo, EugeniaMicroextraction by packed sorbent (MEPS) efficiently combines extraction, pre-concentration, and cleanup in a single device comprising two parts: the MEPS syringe and the packed sorbent bed1. MEPS has been used for several bioanalytical applications, including extraction of endogenous metabolites, biomarkers, and drugs from biological samples. It is particularly useful in metabolomics and pharmacokinetic studies2,3. Regarding MEPS applicability to forensic toxicology, urine is the most used specimen, followed by oral fluid (despite of its relatively high viscosity). Protein precipitation followed by centrifugation and with, or without dilution of the supernatant is the most commonly reported approach. The most detected compounds in forensic settings using MEPS are drugs of abuse [opiates and opioids (26%), cocaine (13%) cathinones (11%), dissociative hallucinogens (11%), cannabinoids and amphetamines (9% each) and other drugs (10%)] and medicinal drugs [antidepressants (9%), benzodiazepines/Z drugs (4%)]. MEPS was also applied to a beverage for forensic purposes e.g. to evaluate its composition in drug-facilitated crimes. An important feature in MEPS is the miniaturization of the sorbent. A careful selection of the sorbent will allow working with complex matrices, separating the target analytes from interferences and improve recoveries. The most widely selected sorbent was the silica based C18 that is a popular reversed-phase material (41%). Starting in the 2000s, new modifications of sorbents appeared. Overall, what the future holds for MEPS applications in forensic toxicology is promising, and ongoing research and technological advancements are likely to enhance the capabilities of MEPS approaches, making this technique an increasingly valuable tool for toxicological investigations.
- Opioid Monitoring in Clinical Settings: Strategies and Implications of Tailored Approaches for TherapyPublication . Rosendo, Luana M.; Rosado, Tiago; Zandonai, Thomas; Rincon, Karem; Peiró, Ana M.; Barroso, Mário; Gallardo, EugeniaThis review emphasises the importance of opioid monitoring in clinical practice and advocates for a personalised approach based on pharmacogenetics. Beyond effectively managing pain, meticulous oversight is required to address concerns about side effects, specially due to opioid-crisis-related abuse and dependence. Various monitoring techniques, along with pharmacogenetic considerations, are critical for personalising treatment and optimising pain relief while reducing misuse and addiction risks. Future perspectives reveal both opportunities and challenges, with advances in analytical technologies holding promise for increasing monitoring efficiency. The integration of pharmacogenetics has the potential to transform pain management by allowing for a precise prediction of drug responses. Nevertheless, challenges such as prominent pharmacogenetic testing and guideline standardisation persist. Collaborative efforts are critical for transforming scientific advances into tangible improvements in patient care. Standardised protocols and interdisciplinary collaboration are required to ensure consistent and evidence-based opioid monitoring. Future research should look into the long-term effects of opioid therapy, as well as the impact of genetic factors on individual responses, to help guide personalised treatment plans and reduce adverse events. Lastly, embracing innovation and collaboration can improve the standard of care in chronic pain management by striking a balance between pain relief and patient safety.
- Otimização de uma metodologia por microextração em seringa empacotada e cromatografia gasosa-espetrometria de massa em tandem para a identificação de arilciclohexaminas em amostras de cabeloPublication . Oliveira, Patrik; Simão, Ana Y.; Rosendo, Luana M.; Pedro, Soraia; Rosado, Tiago; Andraus, Maristela; Barroso, Mário; Gallardo, EugeniaAs novas substâncias psicoativas (NPS) têm vindo a tornar-se um problema cada vez mais um problema de saúde pública. Em Portugal, a ketamina (KET) entrou para a lista de NSP com o Decreto-Lei nº 54/2013. Inicialmente sintetizada com o intuito de substituir a fenciclidina (PCP) como anestésico, acabou por ser usada recreativamente devido aos seus efeitos alucinogénios e estimulantes. Recentemente, a esketamina (análogo da KET) foi introduzida com finalidade terapêutica no tratamento de depressão major refractária a outra terapêutica. Para distinguir o consumo terapêutico do recreativo é necessário que existam métodos que para a sua deteção e quantificação. Neste trabalho foi desenvolvido e otimizado um método para a deteção de KET e seu metabolito (norketamina – NK) em amostras de cabelo com recurso à microextração em seringa empacotada (MEPS) e cromatografia de gases acoplada à espetrometria de massa em tandem (GC-MS/MS). (1) Foi desenvolvido um método analítico para a determinação de KET e NK em amostras de cabelo com recurso à MEPS; (2) A GC-MS/MS foi crucial para deteção inequívoca dos analitos, aumentando a sensibilidade e seletividade do método; (3) As recuperações obtidas são adequadas e foram alcançados LODs baixos (alcançando os cut-offs (0,2 ng/mg) propostos pela Society of Hair Testing) (4) Primeiro método analítico que permite a determinação de KET e NK em amostras de cabelo com recurso a MEPS e GC-MS/MS
- Sensors in the Detection of Abused Substances in Forensic Contexts: A Comprehensive ReviewPublication . Rosendo, Luana M.; Antunes, Mónica; Simão, Ana Y.; Brinca, Ana Teresa; Catarro, Gonçalo; Pelixo, Rodrigo; Martinho, João; Pires, Bruno; Soares, Sofia; Cascalheira, José Francisco; Passarinha, Luís; Rosado, Tiago; Barroso, Mário; Gallardo, Eugeniaorensic toxicology plays a pivotal role in elucidating the presence of drugs of abuse in both biological and solid samples, thereby aiding criminal investigations and public health initiatives. This review article explores the significance of sensor technologies in this field, focusing on diverse applications and their impact on the determination of drug abuse markers. This manuscript intends to review the transformative role of portable sensor technologies in detecting drugs of abuse in various samples. They offer precise, efficient, and real-time detection capabilities in both biological samples and solid substances. These sensors have become indispensable tools, with particular applications in various scenarios, including traffic stops, crime scenes, and workplace drug testing. The integration of portable sensor technologies in forensic toxicology is a remarkable advancement in the field. It has not only improved the speed and accuracy of drug abuse detection but has also extended the reach of forensic toxicology, making it more accessible and versatile. These advancements continue to shape forensic toxicology, ensuring swift, precise, and reliable results in criminal investigations and public health endeavours.