Health Sciences Research Centre

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Characterisation of Cannabis-Based Products Marketed for Medical and Non-Medical Use Purchased in Portugal

Publication . Pires, Bruno; Oliveira, Patrik; Simão, Ana Y.; Reis, João; Ramos, Sofia; Duarte, Ana Paula; Margalho, Cláudia; Rosado, Tiago; Barroso, Mário; Gallardo, Eugenia

Cannabis-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.

2024Journal article

Open access

Quantification of antidepressants in oral fluid and plasma samples using microextraction by packed sorbent and analysis by gas chromatography-tandem mass spectrometry

Publication . Soares, Sofia; Rosado, Tiago; Barroso, Mário; Gallardo, Eugenia

The consumption of antidepressants is extremely significant as they are a class of medications widely used in the treatment of numerous disorders and are therefore considered a public health problem throughout the world. The aim of this work was to develop and optimize two methodologies for the determination of selected antidepressants and metabolites (fluoxetine, venlafaxine, O-desmethylvenlafaxine, citalopram, sertraline, paroxetine), in 250 µL of sample (oral fluid and plasma) using microextraction by packed sorbent (MEPS) as the extraction technique and gas chromatography coupled to tandem mass spectrometry (GC–MS/MS) for analysis. The two methods were fully validated considering the internationally accepted criteria for bioanalytical procedures, presenting linearity within the studied range, with limits of quantification between 10 and 100 ng/mL, coefficients of determination (R2) of at least 0.99 and precision and accuracy with acceptable values of coefficients of variation and relative errors for all antidepressants in study and for both specimens. Recoveries ranged between approximately 12 and 93 % for oral fluid samples and between approximately 28 and 101 % for plasma samples. To our best knowledge, the described methods are the first to be reported using MEPS and GC–MS/MS for the identification of antidepressants in oral fluid and plasma samples, proving to be sensitive, simple, fast and capable of being applied in routine clinical and forensic toxicology scenarios.

2024Journal article

Open access

Opioid Monitoring in Clinical Settings: Strategies and Implications of Tailored Approaches for Therapy

Publication . Rosendo, Luana M.; Rosado, Tiago; Zandonai, Thomas; Rincon, Karem; Peiró, Ana M.; Barroso, Mário; Gallardo, Eugenia

This 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.

2024Journal article

Open access

Comparative study of sample preparation procedures to determine the main compounds in ayahuasca beverages by QuEChERS and high‐performance liquid chromatography analysis

Publication . Gonçalves, Joana; Rosado, Tiago; Barroso, Mário; Restolho, José; Fernández, Nicolás; Luís, Ângelo; Gallardo, Eugenia; Duarte, Ana Paula

Introduction : 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.

2024Journal article

Open access

Impacto da Derivatização Química na Deteção de Metabolitos de Cocaína na presença de Benzodiazepinas

Publication . Costa, Suzel; Rosendo, Luana; Barroso, Mário; Gallardo, Eugenia

A toxicologia forense desempenha um papel crucial em investigações legais, proporcionando informações essenciais sobre a presença e o impacto de várias substâncias em amostras biológicas. No entanto, esta área enfrenta desafios significativos devido a artefactos e interferências que podem dificultar a interpretação dos resultados. Este estudo aborda os desafios analíticos decorrentes da presença simultânea de cocaína e tranquilizantes benzodiazepínicos, especificamente o nordiazepam, em amostras biológicas. De facto, o nordiazepam, uma importante benzodiazepina, pode interferir na deteção e quantificação da benzoilecgonina, o principal metabolito da cocaína, quando se utiliza a cromatografia gasosa acoplada à espectrometria de massa (GC-MS). Recorreu-se à extração de fase sólida (SPE) em amostras de sangue post-mortem, usando colunas Oasis® MCX. Após a evaporação dos extratos, procedeu-se à derivatização por micro-ondas com MSTFA (N-metil-N-(trimetilsilil)trifluoroacetamida) ou MBDSTFA (N-metil-N-(terc-butildimetilsilil)-trifluoroacetamida). A análise foi realizada por cromatografia gasosa acoplada a um detetor de massa. Os resultados demonstraram que com a derivatização por MSTFA a presença de nordiazepam causava interferências significativas na deteção de benzoilecgonina, dificultando a confirmação qualitativa deste último composto. Este fenómeno foi evidenciado em cromatogramas onde picos cromatográficos correspondentes a fragmentos iónicos da benzoilecgonina foram observados mesmo quando apenas o nordiazepam foi injetado. Por outro lado, ao utilizar MBDSTFA como reagente derivatizante, não houve interferência significativa entre nordiazepam e benzoilecgonina às concentrações de 10 ng/mL e 25 ng/mL (limite de deteção e quantificação, respetivamente, da benzoilecgonina), ao contrário do observado com a derivatização por MSTFA. Este estudo destaca a necessidade de procedimentos de derivatização adequados de modo a diminuir o número de falsos negativos nos ensaios toxicológicos e enfatiza a importância de metodologias confiáveis em investigações forenses. A implementação de processos de validação rigorosos e o uso de agentes de derivatização alternativos, quando necessário, são cruciais para evitar interferências que prejudiquem a correta identificação dos tóxicos. As conclusões apresentadas contribuem para uma melhor compreensão das limitações da toxicologia forense, oferecendo recomendações práticas para aumentar a robustez das análises toxicológicas em casos envolvendo a cocaína.

2024-10Other

Embargoed access