Browsing by Author "Morais, Simone"
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- Adsorptive stripping voltammetric determination of venlafaxine in urine with a mercury film microelectrodePublication . Morais, Simone; Ryckaert, Christine P. M. C. A.; Delerue-Matos, CristinaAn adsorptive stripping voltammetric procedure for the determination of the antidepressant venlafaxine in urine using a mercury film microelectrode wasdeveloped. The method is based on controlled adsorptive accumulation of the drug at the potential of 1.00V (vs. Ag/AgCl) in the presence of 1.25 x10 -2 molL- 1 borate buffer (pH 8.7). Urine samples were analyzed directly after performing a ten-fold dilution with the supporting electrolyte but without other pretreatment. The limit of detection obtained for a 30 s collection time was 0.693x 10- 6 mol L -1. Recovery experimentsgave good results at the 10 -6 mol L- 1 level (bias less 5% were obtained).
- Agar extraction from integrated multitrophic aquacultured Gracilaria vermiculophylla: Evaluation of a microwave-assisted process using response surface methodologyPublication . Sousa, Ana M. M.; Alves, V. D.; Morais, Simone; Delerue-Matos, Cristina; Gonçalves, Maria PilarMicrowave-assisted extraction (MAE) of agar from Gracilaria vermiculophylla, produced in an integrated multitrophic aquaculture (IMTA) system, from Ria de Aveiro (northwestern Portugal), was tested and optimized using response surface methodology. The influence of the MAE operational parameters (extraction time, temperature, solvent volume and stirring speed) on the physical and chemical properties of agar (yield, gel strength, gelling and melting temperatures, as well as, sulphate and 3,6-anhydro-Lgalactose contents) was evaluated in a 2^4 orthogonal composite design. The quality of the extracted agar compared favorably with the attained using traditional extraction (2 h at 85ºC) while reducing drastically extraction time, solvent consumption and waste disposal requirements. Agar MAE optimum results were: an yield of 14.4 ± 0.4%, a gel strength of 1331 ± 51 g/cm2, 40.7 ± 0.2 _C gelling temperature, 93.1 ± 0.5ºC melting temperature, 1.73 ± 0.13% sulfate content and 39.4 ± 0.3% 3,6-anhydro-L-galactose content. Furthermore, this study suggests the feasibility of the exploitation of G. vermiculophylla grew in IMTA systems for agar production.
- Air pollution from traffic emissions in Oporto, Portugal: health and environmental implicationsPublication . Slezakova, Klara; Castro, Dionísia; Begonha, Arlindo; Delerue-Matos, Cristina; Alvim-Ferraz, Maria da Conceição M.; Morais, Simone; Pereira, Maria do CarmoAir pollution represents a serious risk not only to environment and human health, but also to historical heritage. In this study, air pollution of the Oporto Metropolitan Area and its main impacts were characterized. The results showed that levels of CO, PM10 and SO2 have been continuously decreasing in the respective metropolitan area while levels of NOx and NO2 have not changed significantly. Traffic emissions were the main source of the determined polycyclic aromatic hydrocarbons (PAHs; 16 PAHs considered by U.S. EPA as priority pollutants, dibenzo[a,l]pyrene and benzo[j]fluoranthene) in air of the respective metropolitan area. The mean concentration of 18 PAHs in air was 69.9±39.7 ng m−3 with 3–4 rings PAHs accounting for 75% of the total ΣPAHs. The health risk analysis of PAHs in air showed that the estimated values of lifetime lung cancer risks considerably exceeded the health-based guideline level. Analytical results also confirm that historical monuments in urban areas act as passive repositories for air pollutants present in the surrounding atmosphere. FTIR and EDX analyses showed that gypsum was the most important constituent of black crusts of the characterized historical monument Monastery of Serra do Pilar classified as “UNESCO World Cultural Heritage”. In black crusts, 4–6 rings compounds accounted approximately for 85% of ΣPAHs. The diagnostic ratios confirmed that traffic emissions were the major source of PAHs in black crusts; PAH composition profiles were very similar for crusts and PM10 and PM2.5.
- Alzheimer’s disease: Development of a sensitive label-free electrochemical immunosensor for detection of amyloid beta peptidePublication . Carneiro, Pedro; Loureiro, Joana; Delerue-Matos, Cristina; Morais, Simone; Pereira, Maria do CarmoIn this work, a highly sensitive label-free immunosensor for detection of the main biomarker of Alzheimer’s disease (AD), amyloid beta 1–42 (Aβ (1–42)), is presented. A gold electrode was modified with a mercaptopropionic acid (MPA) self-assembled monolayer, electrodeposited gold nanoparticles (AuNPs) and a monoclonal antibody mAb DE2B4 to recognize Aβ; all the relevant experimental variables were optimized. Antibodies were functionalized through chemical modification (thiolation) to promote the antibody immobilization on the AuNPs surface with proper orientation which enabled the direct detection of Aβ(1–42). Scanning electron microscopy, square-wave voltammetry and electrochemical impedance spectroscopy were used to characterize the construction of the biosensor. Using the proposed immunosensor, Aβ(1–42) was specifically detected within the linear range of 10–1000 pg mL−1 with a 5.2 pg mL−1 and 17.4 pg mL−1 detection and quantification limit, respectively; recovery values for the tested spiking levels ranged from 90.3 to 93.6%. The immunosensor enables rapid, accurate, precise, reproducible and highly sensitive detection (14.6%reduction mL pg−1) of Aβ with low-cost and opens the possibilities for diagnostic ex vivo applications and research-based in vivo studies.
- Alzheimer’s disease: Development of a sensitive label-freeelectrochemical immunosensor for detection of amyloid beta peptidePublication . Carneiro, Pedro; Loureiro, Joana; Delerue-Matos, Cristina; Morais, Simone; Pereira, Maria do CarmoIn this work, a highly sensitive label-free immunosensor for detection of the main biomarker of Alzheimer’s disease (AD), amyloid beta 1–42 (A (1–42)), is presented. A gold electrode was modified with a mercaptopropionic acid (MPA) self-assembled monolayer, electrodeposited gold nanoparticles (AuNPs) and a monoclonal antibody mAb DE2B4 to recognize A ; all the relevant experimental variables were optimized. Antibodies were functionalized through chemical modification (thiolation) to promote the antibody immobilization on the AuNPs surface with proper orientation which enabled the direct detection of A (1–42). Scanning electron microscopy, square-wave voltammetry and electrochemical impedance spectroscopy were used to characterize the construction of the biosensor. Using the pro-posed immunosensor, A (1–42) was specifically detected within the linear range of 10–1000 pg mL−1 with a 5.2 pg mL−1 and 17.4 pg mL−1 detection and quantification limit, respectively; recovery values for the tested spiking levels ranged from 90.3 to 93.6%. The immunosensor enables rapid, accurate, precise, reproducible and highly sensitive detection (14.6%reduction mL pg−1) of A with low-cost and opens the possibilities for diagnostic ex vivo applications and research-based in vivo studies.
- Analysis of PCBs in soils and sediments by microwave-assisted extraction, headspace-SPME and high resolution gas chromatography with ion-trap tandem mass spectrometryPublication . Herbert, Paulo; Morais, Simone; Paíga, Paula; Alves, Arminda; Santos, LúciaA procedure for the determination of seven indicator PCBs in soils and sediments using microwave-assisted extraction (MAE) and headspace solid-phase microextraction (HS-SPME) prior to GC-MS/MS is described. Optimization of the HS-SPME was carried out for the most important parameters such as extraction time, sample volume and temperature. The adopted methodology has reduced consumption of organic solvents and analysis runtime. Under the optimized conditions, the method detection limit ranged from 0.6 to 1 ng/g when 5 g of sample was extracted, the precision on real samples ranged from 4 to 21% and the recovery from 69 to 104%. The proposed method, which included the analysis of a certified reference material in its validation procedure, can be extended to several other PCBs and used in the monitoring of soil or sediments for the presence of PCBs.
- Analysis of polycyclic aromatic hydrocarbons in fish: evaluation of a quick, easy, cheap, effective, rugged, and safe extraction methodPublication . Ramalhosa, Maria João; Paíga, Paula; Morais, Simone; Delerue-Matos, Cristina; Oliveira, M. Beatriz P. P.QuEChERS method was evaluated for extraction of 16 PAHs from fish samples. For a selective measurement of the compounds, extracts were analysed by LC with fluorescence detection. The overall analytical procedure was validated by systematic recovery experiments at three levels and by using the standard reference material SRM 2977 (mussel tissue). The targeted contaminants, except naphthalene and acenaphthene, were successfully extracted from SRM 2977 with recoveries ranging from 63.5–110.0% with variation coefficients not exceeding 8%. The optimum QuEChERS conditions were the following: 5 g of homogenised fish sample, 10 mL of ACN, agitation performed by vortex during 3 min. Quantification limits ranging from 0.12– 1.90 ng/g wet weight (0.30–4.70 µg/L) were obtained. The optimized methodology was applied to assess the safety concerning PAHs contents of horse mackerel (Trachurus trachurus), chub mackerel (Scomber japonicus), sardine (Sardina pilchardus) and farmed seabass (Dicentrarchus labrax). Although benzo(a)pyrene, the marker used for evaluating the carcinogenic risk of PAHs in food, was not detected in the analysed samples (89 individuals corresponding to 27 homogenized samples), the overall mean concentration ranged from 2.52 l 1.20 ng/g in horse mackerel to 14.6 ± 2.8 ng/ g in farmed seabass. Significant differences were found between the mean PAHs concentrations of the four groups.
- Analysis of polycyclic aromatic hydrocarbons in atmospheric particulate samples by microwaveassisted extraction and liquid chromatographyPublication . Castro, Dionísia; Slezakova, Klara; Oliva-Teles, Maria Teresa; Delerue-Matos, Cristina; Alvim-Ferraz, Maria da Conceição M.; Morais, Simone; Pereira, Maria do CarmoA methodology based on microwave-assisted extraction (MAE) and LC with fluorescence detection (FLD) was investigated for the efficient determination of 15 polycyclic aromatic hydrocarbons (PAHs) regarded as priority pollutants by the US Environmental Protection Agency and dibenzo(a,l)pyrene in atmospheric particulate samples. PAHs were successfully extracted from real outdoor particulate matter (PM) samples with recoveries ranging from 81.4±8.8 to 112.0±1.1%, for all the compounds except for naphthalene (62.3±18.0%) and anthracene (67.3±5.7%), under the optimum MAE conditions (30.0 mL of ACN for 20 min at 110ºC). No clean-up steps were necessary prior to LC analysis. LOQs ranging from 0.0054 ng/m3 for benzo( a)anthracene to 0.089 ng/m3 for naphthalene were reached. The validated MAE methodology was applied to the determination of PAHs from a set of real world PM samples collected in Oporto (north of Portugal). The sum of particulate-bound PAHs in outdoor PM ranged from 2.5 and 28 ng/m3.
- Analysis of polycyclic aromatic hydrocarbons in fish: optimisation and validation of microwave-assisted extractionPublication . Ramalhosa, Maria João; Paíga, Paula; Morais, Simone; Sousa, Ana M. M.; Gonçalves, Maria Pilar; Delerue-Matos, Cristina; Oliveira, M. Beatriz P. P.An accurate and sensitive method for determination of 18 polycyclic aromatic hydrocarbons (PAHs) (16 PAHs considered by USEPA as priority pollutants, dibenzo[a,l]pyrene and benzo[j]fluoranthene) in fish samples was validated. Analysis was performed by microwave-assisted extraction and liquid chromatography with photodiode array and fluorescence detection. Response surface methodology was used to find the optimal extraction parameters. Validation of the overall methodology was performed by spiking assays at four levels and using SRM 2977. Quantification limits ranging from 0.15–27.16 ng/g wet weight were obtained. The established method was applied in edible tissues of three commonly consumed and commercially valuable fish species (sardine, chub mackerel and horse mackerel) originated from Atlantic Ocean. Variable levels of naphthalene (1.03–2.95 ng/g wet weight), fluorene (0.34–1.09 ng/g wet weight) and phenanthrene (0.34–3.54 ng/g wet weight) were detected in the analysed samples. None of the samples contained detectable amounts of benzo[a]pyrene, the marker used for evaluating the occurrence and carcinogenic effects of PAHs in food.
- Anodic adsorptive stripping voltammetric determination of atrazine in spiked soil samples with a gold microelectrodePublication . Morais, Simone; Tavares, Oriza; Paíga, Paula; Delerue-Matos, CristinaMicrowave-assisted solvent extraction was combined with anodic adsorptive stripping voltammetry at a gold microelectrode to extract and quantify the herbicide atrazine in spiked soil samples. A systematic study of the experimental parameters affecting the stripping response was carried out by square-wave voltammetry. The voltammetric procedure is based on controlled adsorptive accumulation of atrazine at the potential of 0.35V (versus Ag/AgCl) in the presence of Britton–Robinson buffer pH (2.0). The limit of detection obtained for a 30 sec collection time was 4.3x10-7 mol L-1. Recovery experiments, at the 1µgg-1 level of spiking, gave good results for the global procedure, and the values found were comparable to those obtained by HPLC.