Percorrer por autor "Rosado, Tiago"
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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.
- Analysis of opiates in urine using microextraction by packed sorbent and gas Chromatography- Tandem mass spectrometryPublication . Simão, Ana Y.; Monteiro, Catarina; Marques, Hernâni; Rosado, Tiago; Margalho, Cláudia; Barroso, Mário; Andraus, Maristela; Gallardo, EugeniaOpiates recreational consumption has always been a concern in society, public health, and in clinical toxicology analysis. The aim of this study was to develop and fully validate an analytical method, which was simple and rapid for the determination of tramadol, codeine, morphine, 6- acetylcodeine, 6-monoacetylmorphine and fentanyl using gas chromatography coupled to tandem mass spectrometry. The procedure includes the use of microextraction by packed sorbent for sample clean-up. A mixed mode sorbent was used, allowing the minimal use of solvents. The method was validated in urine samples, with the ability to detect and quantify all analytes with satisfactory linearity (in the range of 1 – 1000 ng/mL for all analytes, except for fentanyl (10–1000 ng/mL)). Extraction efficiency varied from 17 to 107%, which did not impair sensitivity, taking into account the low LLOQs obtained (1 ng/ mL for all analytes; and 10 ng/mL for fentanyl). The developed procedure proved to be fast, selective, and accurate for use in routine analysis, with a low volume of sample (250 µL).
- Characterisation of Cannabis-Based Products Marketed for Medical and Non-Medical Use Purchased in PortugalPublication . Pires, Bruno; Oliveira, Patrik; Simão, Ana Y.; Reis, João; Ramos, Sofia; Duarte, Ana Paula; Margalho, Cláudia; Rosado, Tiago; Barroso, Mário; Gallardo, EugeniaCannabis-based products have gained attention in recent years for their perceived therapeutic benefits (with cannabinoids such as THC and CBD) and widespread availability. However, these products often lack accurate labelling regarding their cannabinoid content. Our study, conducted with products available in Portugal, revealed significant discrepancies between label claims and actual cannabinoid compositions. A fully validated method was developed for the characterisation of different products acquired from pharmacies and street shops (beverages, herbal samples, oils, and cosmetic products) using high-performance liquid chromatography coupled with a diode array detector. Linearity ranged from 0.4 to 100 µg/mL (0.04–10 µg/mg) (THC, 8-THC, CBD, CBG, CBDA, CBGA), 0.1–100 µg/mL (0.01–10 µg/mg) (CBN), 0.4–250 µg/mL (0.04–25 µg/mg) (THCA-A), and 0.8–100 µg/mL (0.08–10 µg/mg) (CBCA). Among sampled beverages, none contained detectable cannabinoids, despite suggestive packaging. Similarly, oils often differed from the declared cannabinoid compositions, with some containing significantly higher CBD concentrations than labelled. These inconsistencies raise serious concerns regarding consumer safety and informed decision-making. Moreover, our findings underscore the need for stringent regulation and standardised testing protocols to ensure the accuracy and safety of cannabis-based products.
- Characterization of Antidepressant Consumption in a Portuguese Inland Population.Publication . Soares, Sofia; Rosado, Tiago; Santos, Vítor Hugo; Rei, Cristina; Amantegui, Patricia; Pissarra da Costa, António; Chaves, Telma; Valente, Rita; Duarte, Fábio; Pacheco, Susana; Martins, Marco; Dias, Kátia; Costa, Patricia; Costa, Rui; Castro, Sílvia; Sousa, Diana; Figueiredo, Diana; Soares, Isabel; Mouta, Salomé; Jesus, Bianca; Pires, Ana; Ribeiro, Cândida; Lobo, Sónia; Correia, Leonor; Malés, Sofia; Vale, Fátima; Moita, Carina; Moura, Carolina; Sousa, Joana; Afonso, Luís Rafael; Costa, Rita Santinho; Barroso, Mário; Gallardo, EugeniaMental disorders are a growing global concern, with depression being among the most prevalent. Portugal ranks second in antidepressant consumption within the OECD, following a threefold increase between 2000 and 2020. In inland regions such as Beira Interior, reduced healthcare services and distance from major hospitals further complicate access to care. This study analysed 142 patients from Beira Interior undergoing antidepressant therapy to characterise their demographic and clinical profile and to assess associations with adverse effects. A cross-sectional survey collected demographic data, clinical diagnoses, prescribed antidepressants, concomitant medications, and reported adverse effects. Both descriptive and inferential statistical analyses were performed. Most participants were female (81.0%), with a mean age of 57.8 years. Major depression was the most common diagnosis (76.1%). Selective serotonin reuptake inhibitors (47.4%) and trazodone (27.8%) were the most prescribed agents. Treatment had lasted one to five years in 59.9% of cases. Concomitant use of benzodiazepines (76.8%) and antipsychotics (48.6%) was frequent. Reported adverse effects included anticholinergic symptoms (38.7%) and confusion/agitation (26.8%). Women were more likely to use serotonin modulators, while patients >64 years had higher odds of using tetracyclic/unicyclic antidepressants, serotonin modulators, and multiple antidepressants. These classes were significantly associated with increased adverse effects. The findings reveal important risks related to polypragmasia and adverse reactions, underscoring the need for individualised prescribing, rigorous monitoring, and strict adherence to guidelines. Larger, stratified, and longitudinal studies are needed to clarify causality and optimise treatment outcomes.
- Chromatographic determination of antidepressants in plasma and saliva: Towards non-invasive therapeutic monitoringPublication . Soares, Sofia; Rosendo, Luana; Fonseca, Suzana; Gonçalves, Nuno; Franco, João; da Costa, António Pissarra; Rosado, Tiago; Barroso, Mário; Santos, Vítor Hugo; Rei, Cristina; Amantegui, Patricia; Chaves, Telma; Valente, Rita; Duarte, Fábio; Pacheco, Susana; Martins, Marco; Dias, Kátia; Costa, Patricia; Costa, Rui; Castro, Sílvia; Sousa, Diana; Figueiredo, Diana; Soares, Isabel; Mouta, Salomé; Jesus, Bianca; Pires, Ana; Ribeiro, Cândida; Lobo, Sónia; Correia, Leonor; Malés, Sofia; Vale, Fátima; Moita, Carina; Moura, Carolina; Sousa, Joana; Afonso, Luís Rafael; Costa, Rita Santinho; Gallardo, EugeniaDrug monitoring of antidepressants in plasma and oral fluid represents a valuable tool in clinical practice, enabling the optimisation of treatment efficacy and the reduction of adverse effects. Given the significant interindividual variability in antidepressant response-driven by factors such as metabolism, drug-drug interactions, and adherence to therapy-drug monitoring facilitates dose adjustment based on measured drug concentrations, ensuring levels remain within the therapeutic window. This study aimed at developing and validating a robust, rapid, and sensitive method for the simultaneous quantification of 21 selected antidepressants and their metabolites in only 100 μL of plasma and oral fluid. Sample preparation was performed using a simple protein precipitation protocol, followed by analysis via liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method was validated in accordance with internationally accepted bioanalytical guidelines, demonstrating linearity over the concentration range of 0.98-1000 ng/mL. Limits of quantification were established at 0.98 ng/mL for all analytes across both matrices. The extraction procedure yielded high recovery rates, and the method showed excellent selectivity, sensitivity, precision, and accuracy, confirming its suitability for routine toxicological applications. The validated method was successfully applied to 142 paired authentic plasma and oral fluid specimens from patients undergoing antidepressant therapy. Antidepressant concentrations were determined in both matrices, and treatment adherence was considered high, being confirmed in 88.7 % of patients. Correlation analysis between plasma and oral fluid concentrations produced promising results for several of the compounds under investigation, reinforcing the potential utility of oral fluid as a non-invasive alternative matrix in drug monitoring.
- Comparative study of sample preparation procedures to determine the main compounds in ayahuasca beverages by QuEChERS and high‐performance liquid chromatography analysisPublication . Gonçalves, Joana; Rosado, Tiago; Barroso, Mário; Restolho, José; Fernández, Nicolás; Luís, Ângelo; Gallardo, Eugenia; Duarte, Ana PaulaIntroduction : Ayahuasca is a psychoactive drink originally consumed by indigenous people of the Amazon. The lack of regulation of this drink leads to uncontrolled consumption, and it is often consumed in religious contexts. Objective :The aim of this work is to compare three miniaturised extraction techniques for extracting the main ayahuasca compounds from beverages. Methodology:Three sample pretreatment techniques were evaluated (dispersive liquid–liquid microextraction [DLLME], microextraction by packed sorbent [MEPS] and QuEChERS [Quick, Easy, Cheap, Effective, Rugged and Safe]) for the simultaneous extraction of N,N-dimethyltryptamine (DMT), tetrahydroharmine (THH), harmine, harmaline, harmol and harmalol from ayahuasca beverage samples. Then, the most promising technique (QuEChERS) was chosen to pre-concentrate the analytes, subsequently detected by high-performance liquid chromatography coupled to a diode array detector (HPLC-DAD). Results: The procedure was optimised, with the final conditions being 500 μL of extractor solvent, 85 mg of primary secondary amine (PSA) and 4 s of vortexing. The analytical method was validated, showing to be linear between 0.16 and 10 μg/mL for β-carbolines and between 0.016 and 1 μg/mL for DMT, with coefficients of determination (R2) between 0.9968 and 0.9993. The limit of detection (LOD) and lower limit of quantification (LLOQ) were 0.16 μg/mL for all compounds, except for DMT (0.016 μg/mL) and extraction efficiencies varied between 60.2% and 88.0%. Conclusion: The analytical methodology proved to be accurate and precise, with good linearity, LODs and LLOQs. This method has been fully validated and successfully applied to ayahuasca beverage samples.
- Desenvolvimento e otimização de uma nova metodologia para determinação de antidepressivos em plasma com extração por MEPS e análise por GC-MS/MSPublication . Soares, Sofia; Rosado, Tiago; Barroso, Mário; Gallardo, EugeniaO consumo de antidepressivos constitui uma problemática mundial e Portugal apresenta uma das taxas de doenças mentais mais elevadas da Europa1. A monitorização terapêutica está estabelecida para um pequeno número de medicamentos para os quais se verifica uma relação direta entre concentração e efeito farmacológico. Este trabalho tem como objetivo desenvolver uma metodologia para deteção de antidepressivos (fluoxetina, venlafaxina, citalopram, sertralina, paroxetina e metabolitos) em 250 μL de plasma por microextração em seringa empacotada (MEPS) e cromatografia gasosa acoplada à espectrometria de massa em tandem (GC-MS/MS). A técnica de MEPS foi otimizada utilizando a ferramenta estatística Design of Experiments e o número de strokes foi o único fator significativo. O procedimento final de extração foi: adicionar 250 μL de amostra com 500 μL de acetonitrilo, centrifugar, decantar e evaporar; dissolver o resíduo com 1 mL de tampão fosfato 25 mM (pH 5), adicionar o padrão interno e homogeneizar; acondicionamento com 250 μL de metanol e 250 μL de 0,1% de ácido fórmico em H2O; loading de 12x150 μL de amostra; lavagem de 4x50 μL com 1% de ácido fórmico em H2O; secagem por aspiração de 4x50 μL de ar; eluição de 6x100 μL com 1% de hidróxido de amónia em metanol; evaporar até a secura, derivatizar durante 2 minutos com microondas a 800 W e injetar 2 μL no sistema cromatográfico. Foram obtidas recuperações entre 12-93% e limites de quantificação entre 10-100 ng/mL. Este é o primeiro trabalho a utilizar a MEPS e GC-MS/MS na determinação de antidepressivos e metabolitos em amostras de plasma.
- Desenvolvimento e validação de um método para a determinação de canabinóides em urina por microextracção em seringa empacotada e GC-MSPublication . Rosendo, Luana; Rosado, Tiago; Oliveira, Patrik; Simão, Ana; Margalho, Cláudia; Costa, Suzel; Passarinha, Luís; Gallardo, Eugenia; Barroso, MárioDe acordo com o Observatório Europeu da Droga e da Toxicodependência, no último ano (dados de junho de 2022), existiam aproximadamente 22,2 milhões consumidores de canábis na Europa. A urina é uma das amostras mais utilizadas para a deteção e quantificação de canabinóides. (...)
- Deteção e quantificação dos principais constituintes de Ayahuasca com recurso a QuEChERS e HPLC-DADPublication . Gonçalves, Joana; Rosado, Tiago; Barroso, Mário; Restolho, José; Luís, Ângelo; Duarte, Ana Paula; Gallardo, EugeniaA Ayahuasca é uma bebida psicoativa originalmente consumida na bacia amazónica. Esta decocção possui N,N-dimetiltriptamina (DMT), responsável pelos efeitos psicoativos, e alcaloides β-carbolínicos, que inibem a Monoamina Oxidase A (MAO-A), permitindo que o DMT aceda ao sistema nervoso central. A legislação que regula o consumo de Ayahuasca é pouco rigorosa, uma vez que esta também é consumida em contexto religioso, levando muitas vezes a um consumo não controlado. Este estudo tem como objetivo a quantificação simultânea de DMT, tetrahidroharmina (THH), harmina, harmalina, harmol e harmalol em amostras de Ayahuasca. Assim, inicialmente foram comparadas três técnicas de extração: microextração líquido-líquido dispersiva (DLLME), microextração em seringa empacotada (MEPS) e Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS). Esta última mostrou ser a mais promissora, portanto foi submetida a um processo de otimização, onde foram testadas três variáveis (volume de solvente extrator, quantidade de amina primária secundária (PSA) e tempo de vórtex). As condições finais utilizadas foram 500 μL de solvente extrator, 85 mg de PSA e 4 segundos de agitação por vórtex. Posteriormente, foi utilizada cromatografia líquida de alta eficiência acoplada a um detetor de diode array (HPLC-DAD). O método analítico foi validado, apresentando linearidade entre 10 e 0,16 μg/mL (1 e 0,016 μg/mL para o DMT) com coeficientes de determinação superiores a 0,99. Os limites de deteção e quantificação foram de 0,16 μg/mL para as β-carbolinas e 0,016 μg/mL para o DMT e as eficiências de extração variaram entre 60 e 88 %. Este é o primeiro estudo que quantifica os principais constituintes de ayahuasca recorrendo à técnica de QuEChERS.
- 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.