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- Portuguese Validated Versions of the Alcohol Use Disorders Identification Test: A Systematic Review ProtocolPublication . Cardoso, Diogo Phalempin; Oliveira, Daniela; Antunes, Beatriz; Saraiva, Rosa; Angus, Kathryn; Gallardo, Eugenia; Rosário, FredericoIntroduction: Alcohol consumption ranks among the top ten risk factors contributing to the global disease burden. Several international organizations recommend the use of the Alcohol Use Disorders Identification Test to screen for at-risk drinkers. However, a fully validated Portuguese version of this test is lacking. The aim of this study is to systematically review validated versions of the Alcohol Use Disorders Identification Test in the Portuguese language, the documented problems and solutions in its application and proposed cut-offs to identify at-risk drinkers. Material and Methods: A systematic search will be performed in Ovid MEDLINE, CINAHL, PsycINFO, ÍndexRMP, LILACS, African Journals Online and SciELO databases, along with grey literature searches to identify validation studies of the AUDIT in Portuguese. Two authors will independently extract data and assess the studies’ methodological quality, using QUADAS-2 and CASP checklists. Discussion: This review will compare different validation studies of the Alcohol Use Disorders Identification Test in Portuguese-speaking countries, reporting, where possible, the psychometric properties, performance characteristics, suggested cut-offs and any documented limitations and suggestions. The results of this review could be used to propose an update of the alcohol screening and brief intervention guidelines in Portugal. The results could also prove useful to support the implementation of alcohol screening delivery by healthcare providers in Portugal and other official Portuguese-speaking countries. Conclusion: This review will provide important information on the validity of the Alcohol Use Disorders Identification Test as a screening tool for at-risk drinking in Portugal and other official Portuguese speaking countries.
- Editorial: Current Analytical Trends in Drug Testing in Clinical and Forensic ToxicologyPublication . Gallardo, Eugenia; Barroso, Mário; Concheiro-Guisan, Marta; de-Castro-Ríos, AnaEditorial on the Research Topic: Current Analytical Trends in Drug Testing in Clinical and Forensic Toxicology The articles included in this collection cover novel analytical approaches, including chromatographic and spectrometric methods, and sample preparation techniques for the investigation and analysis of several classes of compounds. These compounds include novel psychoactive substances (NPS) as well as other drugs and substances within the scope of clinical and forensic toxicology, and other fields, such as doping control. Current trends in bioanalysis require the constant development of novel analytical tools, which includes efficient sample collection procedures and adequate sample preparation protocols in order to maximize compound detection, even at trace levels. Taking into account that the number of substances possibly present in a sample are increasing, efficient multi-analyte methods are usually necessary.
- Solid Phase-Based Microextraction Techniques in Therapeutic Drug MonitoringPublication . Soares, Sofia; Rosado, Tiago; Barroso, Mário; Gallardo, EugeniaTherapeutic drug monitoring is an established practice for a small group of drugs, particularly those presenting narrow therapeutic windows, for which there is a direct relationship between concentration and pharmacological effects at the site of action. Drug concentrations in biological fluids are used, in addition to other clinical observation measures, to assess the patient’s status, since they are the support for therapy individualization and allow assessing adherence to therapy. Monitoring these drug classes is of great importance, as it minimizes the risk of medical interactions, as well as toxic effects. In addition, the quantification of these drugs through routine toxicological tests and the development of new monitoring methodologies are extremely relevant for public health and for the well-being of the patient, and it has implications in clinical and forensic situations. In this sense, the use of new extraction procedures that employ smaller volumes of sample and organic solvents, therefore considered miniaturized and green techniques, is of great interest in this field. From these, the use of fabric-phase extractions seems appealing. Noteworthy is the fact that SPME, which was the first of these miniaturized approaches to be used in the early ‘90s, is still the most used solventless procedure, providing solid and sound results. The main goal of this paper is to perform a critical review of sample preparation techniques based on solid-phase microextraction for drug detection in therapeutic monitoring situations.
- Analysis of Cannabinoids in Biological Specimens: An UpdatePublication . Antunes, Mónica; Barroso, Mário; Gallardo, EugeniaCannabinoids are still the most consumed drugs of abuse worldwide. Despite being considered less harmful to human health, particularly if compared with opiates or cocaine, cannabis consumption has important medico-legal and public health consequences. For this reason, the development and optimization of sensitive analytical methods that allow the determination of these compounds in different biological specimens is important, involving relevant efforts from laboratories. This paper will discuss cannabis consumption; toxicokinetics, the most detected compounds in biological samples; and characteristics of the latter. In addition, a comprehensive review of extraction methods and analytical tools available for cannabinoid detection in selected biological specimens will be reviewed. Important issues such as pitfalls and cut-off values will be considered.
- 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).
- Development and optimization of a new method to determine antidepressants in oral fluid by microextraction by packed sorbent and analysis by GC-MS/MSPublication . Soares, Sofia; Rosado, Tiago; Barroso, Mário; Gallardo, EugeniaBetween 2013 and 2016, the consumption of antidepressants doubled in Portugal, with around 30 million packages of medication for depression, anxiety and other mental health problems dispensed annually. This phenomenon has even given rise to several alerts, which was highlighted in the 2017 report of the National Program for Mental Health, as Portugal has one of the highest rates of mental illness in Europe1. Therapeutic drug monitoring is well established for a small number of drugs, namely for those where a direct relationship between concentration and pharmacological effect at the site of action exists, which in turn is predictably reflected in the response. Drug concentrations in the various biological fluids are used in conjunction with other clinical observation measures to assess the patient's condition, and further support the individualization of therapy. Within this group of drugs targeted for monitoring are antidepressants. In recent years, oral fluid has gained more and more importance in the field of therapeutic drug monitoring, as a non-invasive and painless alternative to traditionally sampled specimens (e.g. blood, plasma). MEPS is a miniaturized solid-phase extraction (SPE) and therefore has a great advantage in the reduced operating volumes and consequently lower amounts of sample and organic solvents are required. As a result, MEPS decreases the time required for extraction, clean-up and concentration of analytes. This is the first work that uses MEPS as sample preparation technique for the determination of antidepressants and metabolites in oral fluid samples (250 µL). The simple extraction procedure proved to be efficient, requiring only 250 µL of biological sample, making it an excellent alternative for the determination of these compounds in routine clinical and forensic toxicology laboratories and for therapeutic monitoring purposes.
- O fluido oral na monitorização terapêutica de fármacos antidepressivosPublication . Soares, Sofia; Rosado, Tiago; Barroso, Mário; Gallardo, EugeniaIntrodução: Entre 2013 e 2016, o consumo de fármacos antidepressivos duplicou em Portugal, com cerca de 30 milhões de embalagens de medicamentos dispensadas anualmente, apresentando uma das taxas de doenças mentais mais elevadas da Europa (Soares et al., 2021). A monitorização terapêutica é uma prática instituída para um pequeno número de fármacos, como os antidepressivos, para os quais há uma relação direta entre a sua concentração e o efeito farmacológico no local de ação. As concentrações dos fármacos nos fluidos biológicos são utilizadas conjuntamente com outras medidas de observação clínica para avaliar o estado do doente, sendo o suporte para a individualização da terapêutica ao permitir a caracterização de alterações farmacocinéticas observadas durante o curso do tratamento, a deteção de alterações no estado fisiopatológico do doente, ou a modificação da farmacocinética base do fármaco, mas também para a avaliação da adesão à terapêutica. Este trabalho descreve o desenvolvimento de um método analítico com potencial na aplicação clínica para a determinação de antidepressivos (fluoxetina, venlafaxina, citalopram, sertralina, paroxetina e metabolitos) em apenas 0,1 mL de fluido oral com amostragem por dried saliva spots (DSS) e análise por cromatografia gasosa-espectrometria de massa em tandem (GC-MS/MS). Métodos: Foi utilizado um GC-MS/MS modelo 7000B da Agilent Technologies. Todas as condições relativas ao equipamento foram previamente otimizadas. Relativamente à otimização dos DSS, foram avaliados os tempos de secagem e extração, solvente de extração e volume de solvente de extração com recurso à ferramenta estatística Design of Experiments. Resultados: Após otimização, as condições finais do processo de extração foram: 1 hora de secagem, 1 mL de metanol e 5 minutos de extração. O método foi validado apresentando linearidade dentro da gama estudada (dentro do intervalo terapêutico), com limites de deteção e quantificação entre 10 e 100 ng/mL. Todos os parâmetros de validação estudados estiveram de acordo com o preconizado por agências internacionais como a EMA e a FDA. Conclusões: Este é o primeiro trabalho que utiliza DSS como técnica de extração de antidepressivos e metabolitos em amostras de fluido oral, mostrando-se uma alternativa sensível, simples e rápida às técnicas convencionais, podendo ser aplicado rotineiramente na monitorização terapêutica, avaliação da adesão à terapêutica, e ainda no âmbito de toxicologia clínica e forense. Agradecimentos: Este trabalho tem o apoio dos fundos FEDER através de POCI-COMPETE 2020-Operational Programme Competitiveness and Internationalisation in Axis I-Strengthening research, technological development and innovation (Project POCI-01-0145-FEDER-007491) e da FCT-Fundação para a Ciência e a Tecnologia (Projecto UID/Multi/00709/2020). Sofia Soares gostaria de agradecer à FCT a bolsa com a referência SFRH/BD/148753/2019.
- Microextração em seringa empacotada (MEPS) como técnica de clean-up para a determinação de catinonas sintéticas em cabeloPublication . Simão, Ana; Dinis, Pedro; Margalho, Cláudia; Andraus, Maristela; Barroso, Mário; Gallardo, EugeniaIntrodução: O consumo de catinonas sintéticas, substâncias conhecidas como “bath salts”, tem crescido ao longo dos últimos anos tornando-se um problema de saúde pública. Várias metodologias têm sido desenvolvidas por diferentes autores. No entanto, a técnica miniaturizada – microextração em seringa empacotada (MEPS), tem sido pouco explorada para a determinação de catinonas sintéticas em cabelo. Objetivos: Neste sentido, propomos a otimização desta técnica como clean-up com recurso à técnica analítica cromatografia líquida para a quantificação destes compostos na matriz cabelo. Métodos: As amostras foram lavadas, em ciclos consecutivos de diclorometano, água desionizada e metanol de modo a remover contaminantes depositados externamente. Depois de feita a secagem, com ajuda de uma tesoura, as amostras foram cortadas em fragmentos de cerca de 1-3mm. Cinquenta miligramas de cabelo foram incubados com NaOH (1 M) a 45 °C, durante a noite. Seguido este passo, foi feita uma neutralização com HCl (10 M) e, por fim, as amostras foram extraídas através do processo MEPS, usando um enchimento constituído por C8-SCX. Os compostos foram analisados por LC-MS/MS em modo MRM. Resultados e discussão: O procedimento final demonstrou bons resultados de recuperação (15-59% para todos os analitos), com linearidade para todos os analitos de 0,03 a 2,5 pg/mg, excepto para a pentedrona, cuja gama de linearidade foi de 0,1 a 2,5 pg/mg. Conclusão: Este trabalho permitiu otimizar a metodologia de MEPS para a determinação de 7 catinonas sintéticas em amostras de cabelo. O método foi considerado adequado para a análise destes compostos em cabelo, com valores de recuperação e linearidade satisfatórios.
- 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
- 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.