Percorrer por autor "Delerue-Matos, Cristina"
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- Adulteration of Brain Health (Cognitive, Mood, and Sleep Enhancement) Food Supplements by the Addition of Pharmaceutical Drugs: A Comprehensive Review of Analytical Approaches and TrendsPublication . Paiva, Rafael; Correia, Manuela; Delerue-Matos, Cristina; Amaral, Joana S.In recent years, the consumption of dietary supplements has grown worldwide, particularly in developed regions. However, this growing market has also become a prime target for adulteration practices, with some manufacturers illegally adding pharmaceuticals into plant-based food supplements (PFS) to enhance their effects. While extensive research has focused on detecting adulterant drugs in PFS tailored for improving sexual performance, weight loss, and muscle building, less attention has been given to supplements intended for mood enhancement, sleep aid, and cognitive function (nootropics). Nonetheless, recent reports indicate an increasing level of adulteration within this group of PFS. Therefore, this review aims at providing a comprehensive overview on the adulteration of PFS tailored for brain health, with a focus on the analytical techniques utilized for detection while also presenting data on consumption patterns and the prevalence of reported adulterants. Considering that the detection of such fraudulent practices primarily relies on chromatographic techniques coupled with mass spectrometry (MS), the developments in this field comprising either targeted or untargeted analysis of pharmaceutical adulterants are discussed.
- Analysis of pharmaceutical adulterants in plant food supplements by UHPLC-MS/MSPublication . Paíga, Paula; Rodrigues, Manuela J.E.; Correia, Manuela; Amaral, Joana S.; Oliveira, Beatriz; Delerue-Matos, CristinaA method based on the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was successfully developed and validated for the analysis of 26 pharmaceutical compounds belonging to different therapeutic classes (anorexics, stimulants, anxiolytics, antidepressants and laxatives), which are all prone to be illegally added into weight-loss plant food supplements (PFS) for their pharmacological activity. Internal standard calibration with six isotopically labelled compounds rendered good linearity in the range of 5 to 1000 μg/l, depending on the compound, and good sensitivity with limits of quantification in the range of 0.02–9.80 μg/l. Recoveries were assessed for all the 16 samples analysed and were found between 70% and 120% for over 90% of the analytes. The average recovery value was 90.8%, for the different studied matrices (liquids, liquid ampoules, tablets and capsules), with RSD values lower than 10% for all forms. The changes introduced to the QuEChERS procedure maintained the good performance characteristics of the extraction method while preserving the chromatographic system for the introduction of unwanted matrix compounds. Synephrine was the only compound detected and quantified in one sample, but at a very low concentration (768 μg/l) and its presence may be due to the plant extracts used in the formulation, as synephrine is known to be a natural constituent of Citrus aurantium amara. Despite none of the 16 evaluated samples were found to be adulterated by the illegal addition of the drugs included in this work, the developed methodology can be very useful for monitoring the adulteration of weight-loss PFS.
- Antioxidant, photoprotective and inhibitory activity of tyrosinase in extracts of Dalbergia ecastaphyllumPublication . Morais, Daniel Vieira; Costa, Maria Angélica Carvalho; Bárbara, Marivalda; Silva, Fabiane de Lima; Moreira, Manuela M.; Delerue-Matos, Cristina; Dias, L.G.; Estevinho, Leticia M.; Carvalho, Carlos Alfredo Lopes deDalbergia ecastaphyllum is a native Brazil plant with importance for beekeeping, and widely used in folk medicine. For the first time, the extracts of this plant were assessed for the presence of hydrophilic and lipophilic antioxidants, as well as inhibition of tyrosinase, free radicals scavenging and sunscreen protection. The antioxidant activity was evaluated by free radical scavenging (DPPH) andβ-carotene bleaching assay. The tyrosinase inhibitory activity was evaluated and calculated the EC50. The photoprotective activity was measured using different concentrations of D. ecastaphyllum extracts. The Sun Protection Factor (SPF) of the samples was higher than 6, and the sample from Ilhe ´us showed the most pronounced photoprotective effect. Sample from Canavieiras presented the highest antioxidant activity by free radical scavenging DPPH andβ-carotene bleaching method, with 92.41% and 48.34%, respectively. All samples inhibited the tyrosinase, especially the sample from Prado that was most effective (124.62μg.mL-1). Significant negative correlation was found between flavonoid contents and inhibition of tyrosinase. The overall results provide relevant information about the Dalbergia ecastaphyllum species, indicating as potential material to cosmetic and pharmaceutical industry.
- Assessment of plant food supplements adulteration with psychopharmaceutical drugsPublication . Rodrigues, Manuela J.E.; Paíga, Paula; Santos, Lúcia H.M.L.M.; Amaral, Joana S.; Oliveira, Beatriz; Correia, Manuela; Delerue-Matos, CristinaThe purpose of this study was to compare three different extraction methods (two based on ethanol extraction and one on the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERs) method) to assess the possible addition of psychopharmaceutical drugs (fluoxetine, sertraline, citalopram, venlafaxine, paroxetine, trazodone, and diazepam) as adulterants in St. John's wort (Hypericum perforatum) based plant food supplements (PFS). Methodology: Analysis was performed in a Nexera Ultra-High Performance Liquid Chromatograph (UHPLC) coupled to a triple-quadrupole mass spectrometer (LCMS-8030 Shimadzu) with an electrospray ionization source (ESI), operating in positive ion mode, using a Kinetex C18 fused core column (150 × 2.10 mm i.d.; 1.7 m) (Phenomenex). Multiple reaction monitoring mode (MRM) was selected and pharmaceuticals were quantified by internal standard calibration method. Calibration curves were constructed in the range 10 – 1000 g/L. The three different extraction methods were compared based on the analysis of spiked samples.
- Background concentrations of polycyclic aromatic hydrocarbons metabolites in Portuguese firemenPublication . Oliveira, Mónica; Slezakova, Klara; Fernandes, Adília; Vaz, Josiana A.; Delerue-Matos, Cristina; Pereira, Maria do Carmo; Morais, SimonePolycyclic aromatic hydrocarbons (PAHs) are ubiquitous environmental pollutants produced by the incomplete combustion of organic materials. PAHs may pose risks to human health as many of the individual compounds are cytotoxic and mutagenic to both lower and higher organisms, being some of them regarded as carcinogenic. Pyrene is by far the most characterized PAH in all sample matrices, and is classified as PAH marker of exposure while benzo(a)pyrene is considered the biomarker of carcinogenic exposure to PAHs. Among the 16 PAHs established by US EPA as priority pollutants, naphthalene, acenaphthene, fluorene, and phenanthrene are also found in almost all the matrices. Workers from industrial settings where airborne PAH levels are high such as coke works and the primary aluminium industry, show excess rates of cancers. Firemen are also exposed to high concentrations of PAHs during firefighting; however their biomonitoring is difficult and epidemiological studies are scarce. During the last decade, the urinary 1-hydroxypyrene has been used as a biomarker of environmental and occupational exposure to PAHs. Still no standard reference or occupational guidelines are available for any urinary PAH metabolite. Within the present work, sixty healthy and no smoking Portuguese firemen from ten Portuguese corporations from the district of Bragança (North of Portugal) were evaluated regarding their levels of the most important urinary hydroxyl- PAHs:
- Biomonitoring of firefighters occupational exposure to polycyclic aromatic hydrocarbons during the 2014 hot seasonPublication . Oliveira, Mónica; Slezakova, Klara; Fernandes, Adília; Vaz, Josiana A.; Teixeira, João Paulo Fernandes; Delerue-Matos, Cristina; Pereira, Maria do Carmo; Morais, SimoneHuman biomonitoring is an important tool in environmental medicine that is used to assess the level of internal exposure to environmental pollutants. Firefighters are one of the most exposed and least studied occupations. During fire suppression, firefighters are heavily exposed to a wide range of chemicals. Polycyclic aromatic hydrocarbons (PAH) are ubiquitous environmental pollutants that are considered as the largest known group of carcinogens due to their cytotoxic and mutagenic properties. Smoke and ashes released during a fire are important sources of PAH. Firefighters can be also exposed to PAH through smoking, via polluted ambient air, water, soil, and through consumption of food. Metabolites of PAH (OH-PAHs), such as 1-hydroxynaphthalene (1OHNapt), 1-hydroxyacenaphthene(1OHAce), 1-hydroxypyrene (1OHPy) and 3-hydroxybenzo[a]pyrene (3OHB[a]P) have been used as biological markers for measurements of human internal exposure to PAH. The present work aims to quantify the urinary metabolites of PAH, namely 1OHNapt, 1OHAce, 1OHPy and 3OHB[a]P in study population of firefighters. Firemen exposed to fires that occurred during 2014 season were asked to fill a post-fire questionnaire and to collect urinary samples. A control study population group was selected to collect samples of urines during the pre-fires season (winter). Among all participating firemen only healthy no-smoking subjects were considered. OH-PAHs were analysed by high-performance liquid chromatography with fluorescence detection. Overall, 1OHNapt and 1OHAce were the most abundant OH-PAHs in firemen urine samples, accounting for approximately 90% of the total OH-PAHs. The urinary OH-PAHs in exposed firefighters were higher than those of control group. Data collected with the individual questionnaire were further used to analyse the concentrations of OH-PAH between (and within) control and exposed groups of firemen. Additionally, 1OHPy concentrations in the exposed firefighters will be compared with the available proposed guidelines.
- Biomonitoring of firefighters occupational exposure to polycyclic aromatic hydrocarbons during the 2014 hot seasonPublication . Oliveira, Mónica; Slezakova, Klara; Fernandes, Adília; Vaz, Josiana A.; Teixeira, João Paulo Fernandes; Delerue-Matos, Cristina; Pereira, Maria do Carmo; Morais, SimoneHuman biomonitoring is an important tool in environmental medicine that is used to assess the level of internal exposure to environmental pollutants. Firefighters are one of the most exposed and least studied occupations. During fire suppression, firefighters are heavily exposed to a wide range of chemicals. Polycyclic aromatic hydrocarbons (PAHs) are ubiquitous environmental pollutants that are considered as the largest known group of carcinogens due to their cytotoxic and mutagenic properties (IARC 2010, WHO 2013). Smoke and ashes released during a fire are important sources of PAHs. Firefighters can be also exposed to PAHs through smoking, via polluted ambient air, water, soil, and through consumption of food. Metabolites of PAHs (OH-PAHs), such as 1-hydroxynaphthalene (1OHNapt), 1-hydroxyacenaphthene(1OHAce), 1-hydroxypyrene (1OHPy) and 3-hydroxybenzo[a]pyrene (3OHB[a]P) have been used as biological markers for measurements of human internal exposure to PAHs. The present work aims to quantify the urinary metabolites of PAHs, namely 1OHNapt, 1OHAce, 1OHPy and 3OHB[a]P in study population of firefighters. Firemen exposed to fires that occurred during 2014 season were asked to fill a post-fire questionnaire and to collect urinary samples. A control study population group was selected to collect samples of urines during the pre-fires season (winter). Among all participating firemen only healthy no-smoking subjects were considered. OH-PAHs were analysed by high-performance liquid chromatography with fluorescence detection
- Dalbergia ecastaphyllum leaf extracts: in vitro inhibitory against enzymes related to metabolic syndrome, inflammation and neurodegenerative diseasesPublication . Morais, Daniel Vieira; Moreira, Manuela M.; Silva, Fabiane de Lima; Costa, Maria Angélica Carvalho; Delerue-Matos, Cristina; Carvalho, Carlos Alfredo Lopes de; Estevinho, Leticia M.For the first time, the anti-hemolytic activity and the enzyme inhibitory activities of Dalbergia ecastaphyllum leaves extracts were tested against α-amylase, α-glucosidase, lipase, acetylcholinesterase, butyrylcholinesterase, tyrosinase and hyaluronidase. The phenolic profile of the obtained extracts was also investigated by high-performance liquid chromatography with photodiode array detection (HPLC-PAD). The extracts showed inhibitory activity against all enzymes evaluated, with the highest inhibitory activity reported for the enzyme hyaluronidase (28.28 ± 2.43 to 72.19 ± 1.40 μg mL-1). The obtained extracts also demonstrate anti-hemolytic activity (52.22 ± 1.62 to 71.17 ± 1.82%). Among the phenolic compounds identified, protocatechuic, vanillic and β-resorcylic acids were the most abundant (1.13 ± 0.06 to 2.53 ± 0.06, 0.90 ± 0.06 to 2.19 ± 0.06 and 1.03 ± 1.62 to 22.11 ± 1.62 mg L-1, respectively). In the statistical analysis, a significant correlation was found between the flavonoids content and all enzymes inhibitory activities. The present study showed that D. ecastaphyllum leaves extracts may have the potential to be used in the therapeutic treatment of several diseases such as Alzheimer, Parkinson, type 2 diabetes mellitus, hyperglycemia, and pigmentation, as well as those associated with oxidative stress.
- Deteção remota apoiada por veículos aéreos não tripulados (VANT) aplicada à monitorização de áreas sujeitas a incêndios florestaisPublication . Barroso, Ana; Royer, Ana Carolina; Alves, Leonardo Kipper; Piovesan, Eloiza de Lima; Fernandes, M.; Teixeira, Bruno Rafael Silva; Alves, Diogo; Santos, Patrícia; Fonseca, Felícia; Pamplona, Jorge Manuel; Carvalho, Manuela; Henriques, Renato; Hernández, Zulimar; Delerue-Matos, Cristina; Figueiredo, Tomás de; Valente, TeresaOs incêndios florestais, nas últimas décadas, têm aumentado em termos de frequência, intensidade e extensão. Em consequência, têm também crescido as preocupações pelos efeitos ambientais negativos destes eventos, nomeadamente nas propriedades dos solos. A gravidade das modificações depende, entre outros aspetos, da intensidade e/ou severidade do fogo, topografia local e tipo de vegetação. A monitorização das áreas ardidas é pois essencial para compreender a evolução das propriedades do solo e sua interação com a vegetação, bem como as tendências de recuperação ao longo do tempo. É neste contexto que se reforça a utilidade das técnicas de deteção remota, proporcionando ferramentas eficazes para o acompanhamento de áreas florestais queimadas. Mais frequentemente, esta monitorização faz-se com recursamento ao processamento de imagens de satélite, antes e pós incêndio. As aplicações mais comuns referem o mapeamento ara obtenção de modelos digitais de superfície (MDS) e cálculo de índices de vegetação (NDVI) ou de áreas ardidas (NBR) e volume de biomassa. No entanto, as imagens de satélite apresentam algumas limitações, nomeadamente quanto à resolução espacial e temporal, condicionando assim a qualidade dos dados. Estas limitações são ultrapassadas com a utilização de veículos aéreos não tripulados (VANT), que possibilitam uma maior resolução espacial. No presente trabalho mostra-se um caso de aplicação deste tipo de tecnologia numa área situada no Parque Natural de Montesinho (Aveleda, Bragança, Portugal). São apresentados os resultados de levantamentos fotogramétricos, realizados antes e após um fogo controlado, que proporcionaram imagens obtidas com um VANT Dji Phantom 4RTK. O tratamento dos dados resultantes dos voos permitiu a obtenção de ortofotomapas e MDS, abrindo a possibilidade de estimar o volume de biomassa e avaliar a evolução do processo de revegetação natural. A realização de voos de pormenor, em pequenas secções da parcela, permite ainda um acompanhamento de elevada resolução do efeito do fogo em termos de perda de solo por erosão.
- Determination of psychopharmaceutical adulterants in plant food supplements using UHPLC-MS/MSPublication . Rodrigues, Manuela J.E.; Paíga, Paula; Santos, Lúcia H.M.L.M.; Amaral, Joana S.; Oliveira, Beatriz; Correia, Manuela; Delerue-Matos, CristinaIn the last decades, medicinal plants and derived products have become increasingly available on the EU market as components of formulations sold as plant food supplements (PFS). Such products are legally considered as foods under the Directive 2002/46/EC [l] and do not require any kind of authorization to be placed on the market. The legal responsibility for its safety relies on the business operators. Among the several issues that may aíFect the safety of PFS, adulterations including the addition of illegal substances represent an increasing public health concern. In this context, the adulteration by the addition of psychopharmaceuticals should be investigated. Chromatographic methods, especially LC, coupled to various detectors are commonly used for the detection of fraudulent addition of pharmaceuticals in complex mixtures such as PFS. Among them, LC-MS/MS provides accurate and sensitive detectíon ofthe target compounds [2]. The purpose of this study was to assess the presence of psychopharmaceutical adulterants namely, fluoxetine, sertraline, citalopram, venlafaxine, paroxetine, trazodone, and diazepam in St. Johns wort (Hypericum perforatum) based PFS since this plant and/or extracts are traditionally used for its antidepressive properties. Analysis was performed in a Nexera Ultra-High Performance Liquid Chromatograph coupled to a triple-quadrupole mass spectrometer (LCMS-8030 Shimadzu) with an electrospray ionization source (ESI), operating in positive ion mode, using a Kinetex C18 fused core column (150 x 2.10 mm i.d.; 1.7 [im) (Phenomenex). Multiple reaction monitoring mode (MRM) was selected and pharmaceuticals were quantified by internai standard calibration method. Prior to analysis PFS samples were extracted with methanol. The methodology was applied to a set of20 St. Johns wort based PFS commercially available in the Portuguese market.