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1.
Foods ; 13(2)2024 Jan 19.
Artigo em Inglês | MEDLINE | ID: mdl-38275684

RESUMO

Blueberry fruits have been widely explored for their rich composition of bioactive compounds with recognized health benefits. In contrast, blueberry pruning waste (BPW), generated during the pruning stages of blueberries, has been typically overlooked, even though it can represent a potential source of natural antioxidants. This study aims to characterize the value-added compounds extracted from BPW using green techniques, namely microwave-assisted and subcritical water extraction. The total phenolic content ranged from 157 ± 5 to 335 ± 12 mg GAE/g dw, while the radical scavenging activity determined by a DPPH assay varied from 223 ± 21 to 453 ± 21 mg Trolox equivalents/g dw. Additionally, to ensure the safe application of BPW and its extracts, a screening of pesticides and several environmental contaminants was conducted. Chlorpyrifos-methyl was quantified at a concentration of 4.27 µg/kg in a Bluecrop variety collected in 2019; however, none of the studied compounds were found in the extracts. Despite the presence of a pesticide, this level was below the maximum residue limits for blueberry crops. The results of this study demonstrated the potential of this agro-industrial residue as a natural source of bioactive compounds with high antioxidant activity for food industry applications.

2.
Environ Sci Pollut Res Int ; 31(2): 3152-3168, 2024 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-38085484

RESUMO

The application of sewage sludge (SS) in agriculture, as an alternative to manufactured fertilizers, is current practice worldwide. However, as wastewater is collected from households, industries, and hospitals, the resulting sludge could contaminate land with creeping levels of pharmaceuticals, pesticides, heavy metals, polycyclic aromatic hydrocarbons, and microplastics, among others. Thus, the sustainable management of SS requires the development of selective methods for the identification and quantification of pollutants, preventing ecological and/or health risks. This study presents a thorough evaluation of emerging and priority micropollutants in SS, through the lens of environmental insights, by developing and implementing an integrated analytical approach. A quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method, coupled with gas chromatography and liquid chromatography, was optimized for the determination of 42 organic compounds. These include organophosphorus pesticides, organochlorine pesticides, pyrethroid pesticides, organophosphate ester flame retardants, polybrominated diphenyl ethers, polychlorinated biphenyls, and polycyclic aromatic hydrocarbons. The optimization of the dispersive-solid phase for clean-up, combined with the optimization of chromatographic parameters, ensured improved sensitivity. Method validation included assessments for recovery, reproducibility, limit of detection (LOD), and limit of quantification (LOQ). Recoveries ranged from 59.5 to 117%, while LODs ranged from 0.00700 to 0.271 µg g-1. Application of the method to seven SS samples from Portuguese wastewater treatment plants revealed the presence of sixteen compounds, including persistent organic pollutants. The quantification of α-endosulfan, an organochlorine pesticide, was consistently observed in all samples, with concentrations ranging from 0.110 to 0.571 µg g-1. Furthermore, the study encompasses the analysis of agronomic parameters, as well as the mineral and metal content in SS samples. The study demonstrates that the levels of heavy metals comply with legal limits. By conducting a comprehensive investigation into the presence of micropollutants in SS, this study contributes to a deeper understanding of the environmental and sustainable implications associated with SS management.


Assuntos
Hidrocarbonetos Clorados , Metais Pesados , Praguicidas , Bifenilos Policlorados , Hidrocarbonetos Policíclicos Aromáticos , Esgotos/química , Praguicidas/análise , Compostos Organofosforados , Reprodutibilidade dos Testes , Plásticos , Bifenilos Policlorados/análise , Hidrocarbonetos Clorados/análise , Hidrocarbonetos Policíclicos Aromáticos/análise
3.
Biology (Basel) ; 12(10)2023 Oct 21.
Artigo em Inglês | MEDLINE | ID: mdl-37887061

RESUMO

Cobalt (Co), copper (Cu), manganese (Mn), molybdenum (Mo), and zinc (Zn) are essential trace elements (ETEs) and important cofactors for intermediary metabolism or redox balance. These ETEs are crucial during pregnancy, their role on specific pregnancy outcomes is largely unknown. This prospective study (#NCT04010708) aimed to assess urinary levels of these ETEs in pregnancy and to evaluate their association with pregnancy outcomes. First trimester pregnant women of Porto and Lisbon provided a random spot urine sample, and sociodemographic and lifestyle data. Clinical data were obtained from clinical records. Urinary ETEs were quantified by inductively coupled plasma mass spectrometry (ICP-MS). A total of 635 mother:child pairs were included. Having urinary Zn levels above the 50th percentile (P50) was an independent risk factor for pre-eclampsia (PE) (aOR [95% CI]: 5.350 [1.044-27.423], p = 0.044). Urinary Zn levels above the P50 decreased the risk of small for gestational age (SGA) birth head circumference (aOR [95% CI]: 0.315 [0.113-0.883], p = 0.028), but it increased the risk SGA length (aOR [95% CI]: 2.531 [1.057-6.062], p = 0.037). This study may provide valuable information for public health policies related to prenatal nutrition, while informing future efforts to de-fine urinary reference intervals for ETEs in pregnant women.

4.
Polymers (Basel) ; 15(16)2023 Aug 10.
Artigo em Inglês | MEDLINE | ID: mdl-37631413

RESUMO

Plastic is an indispensable material in modern society; however, high production rates combined with inadequate waste management and disposal have resulted in enormous stress on ecosystems. In addition, plastics can become smaller particles known as microplastics (MPs) due to physical, chemical, and biological drivers. MP pollution has become a significant environmental problem affecting terrestrial and aquatic ecosystems worldwide. Although the topic is not entirely new, it is of great importance to the field of polymers, drawing attention to specific gaps in the existing literature, identifying future areas of research, and improving the understanding of MP pollution and its environmental impacts. Despite progress in this field, problems remain. The lack of standardized methods for MP sampling, separation, extraction, and detection makes it difficult to collect information and establish links between studies. In addition, the distribution and pathways of MPs in ecosystems remain unknown because of their heterogeneous nature and the complex matrices in which they occur. Second, toxicological tests showed that MPs can be ingested by a wide range of organisms, such as Danio rerio and Eisenia fetida, resulting in gut obstruction, physical damage, histological changes, and oxidative stress. The uptake of MP and their toxicological effects depend on their shape, size, concentration, and polymer composition. Furthermore, MPs can enter the food chain, raising concerns regarding potential contaminations for human and environmental health. This review paper sheds light on the pressing issue of MP pollution and highlights the need for interdisciplinary collaboration between scientists, policymakers, and industry leaders.

5.
Polymers (Basel) ; 15(16)2023 Aug 19.
Artigo em Inglês | MEDLINE | ID: mdl-37631527

RESUMO

The constant change in microplastics (MP) due to exposure to environmental conditions leads to physical and chemical changes that enhance their ability to transport other pollutants, increasing the concern about their widespread presence in the environment. This work aimed to simulate the aging process of six MP (polyamide 6, unplasticized polyvinyl chloride, low-density polyethylene, polystyrene, polyethylene-co-vinyl acetate, polypropylene) in freshwater and seawater ecosystems at laboratory scale and evaluate its effects through optical microscope observation, Fourier transform infrared spectroscopy-Attenuated Total Reflectance (FTIR-ATR), Raman spectroscopy, and thermal gravimetric analysis (TGA). Through a combined experimental study of aged MP, the degradation by UV interaction was evidenced by the appearance of new infrared bands in the FTIR spectra assigned to ketones and hydroxyl groups. While Raman analysis and microscope images reveal the appearance of pores, wrinkles, and roughness in the MP surfaces. Variations in the temperature of the maximum weight loss of the MP were observed in the TGA analysis. The adsorption of chlorpyrifos (CPF), a common pesticide widely used in agriculture, by the pristine and aged MP was also studied. The highest affinity for CPF was observed for pristine LDPE and the lowest for PP. The batch adsorption studies revealed an increase in adsorption capacity as a consequence of the aging process for both MP. These results proved that the weathering effects caused changes in the behavior of MP, namely in the interaction with other pollutants.

6.
Foods ; 12(5)2023 Feb 26.
Artigo em Inglês | MEDLINE | ID: mdl-36900510

RESUMO

Global production of exotic fruits has been growing steadily over the past decade and expanded beyond the originating countries. The consumption of exotic and new fruits, such as kiwano, has increased due to their beneficial properties for human health. However, these fruits are scarcely studied in terms of chemical safety. As there are no studies on the presence of multiple contaminants in kiwano, an optimized analytical method based on the QuEChERS for the evaluation of 30 multiple contaminants (18 pesticides, 5 polychlorinated biphenyls (PCB), 7 brominated flame retardants) was developed and validated. Under the optimal conditions, satisfactory extraction efficiency was obtained with recoveries ranging from 90% to 122%, excellent sensitivity, with a quantification limit in the range of 0.6 to 7.4 µg kg-1, and good linearity ranging from 0.991 to 0.999. The relative standard deviation for precision studies was less than 15%. The assessment of the matrix effects showed enhancement for all the target compounds. The developed method was validated by analyzing samples collected from Douro Region. PCB 101 was found in trace concentration (5.1 µg kg-1). The study highlights the relevance of including other organic contaminants in monitoring studies in food samples in addition to pesticides.

7.
Toxics ; 11(2)2023 Jan 27.
Artigo em Inglês | MEDLINE | ID: mdl-36851000

RESUMO

The aims of this study were to characterize the exposure of pregnant women living in Portugal to 3-phenoxybenzoic acid (3-PBA) and to evaluate the association of this exposure with maternal outcomes and newborn anthropometric measures. We also aimed to compare exposure in summer with exposure in winter. Pregnant women attending ultrasound scans from April 2018 to April 2019 at a central hospital in Porto, Portugal, were invited to participate. Inclusion criteria were: gestational week between 10 and 13, confirmed fetal vitality, and a signature of informed consent. 3-PBA was measured in spot urine samples by gas chromatography with mass spectrometry (GC-MS). The median 3-PBA concentration was 0.263 (0.167; 0.458) µg/g creatinine (n = 145). 3-PBA excretion was negatively associated with maternal pre-pregnancy body mass index (BMI) (p = 0.049), and it was higher during the summer when compared to winter (p < 0.001). The frequency of fish or yogurt consumption was associated positively with 3-PBA excretion, particularly during the winter (p = 0.002 and p = 0.015, respectively), when environmental exposure is low. Moreover, 3-PBA was associated with levothyroxine use (p = 0.01), a proxy for hypothyroidism, which could be due to a putative 3-PBA-thyroid hormone antagonistic effect. 3-PBA levels were not associated with the anthropometric measures of the newborn. In conclusion, pregnant women living in Portugal are exposed to 3-PBA, particularly during summer, and this exposure may be associated with maternal clinical features.

8.
J Agric Food Chem ; 71(8): 3898-3905, 2023 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-36792986

RESUMO

A new application of graphene-type materials as an alternative cleanup sorbent in a quick, easy, cheap, effective, rugged, and safe (QuEChERS) procedure combined with GC-ECD/GC-MS/GC-MS/MS detection was successfully used for the simultaneous analysis of 12 brominated flame retardants in Capsicum cultivar samples. The chemical, structural, and morphological properties of the graphene-type materials were evaluated. The materials exhibited good adsorption capability of matrix interferents without compromising the extraction efficiency of target analytes when compared with other cleanups using commercial sorbents. Under optimal conditions, excellent recoveries were obtained, ranging from 90 to 108% with relative standard deviations of <14%. The developed method showed good linearity with a correlation coefficient above 0.9927, and the limits of quantification were in the range of 0.35-0.82 µg/kg. The developed QuEChERS procedure using reduced graphite oxide (rGO) combined with GC/MS was successfully applied in 20 samples, and the pentabromotoluene residues were quantified in two samples.


Assuntos
Capsicum , Retardadores de Chama , Grafite , Resíduos de Praguicidas , Espectrometria de Massas em Tandem , Retardadores de Chama/análise , Capsicum/química , Extração em Fase Sólida/métodos , Verduras , Resíduos de Praguicidas/análise
9.
Nutrients ; 14(21)2022 Oct 26.
Artigo em Inglês | MEDLINE | ID: mdl-36364754

RESUMO

The goal of this work was to examine whether elevated iodine intake was associated with adverse effects on IQ among school-age children in Portugal. In a representative sample of children from the north of the country, IQ percentiles by age (assessed with Raven's Colored Progressive Matrices) were dichotomized to <50 ("below-average" IQs) and ≥50. Morning urine iodine concentrations, corrected for creatinine, were dichotomized to <250 µg/g and ≥250 µg/g, according to the European Commission/Scientific Committee on Food's tolerable upper level of daily iodine intake for young children. Data were examined with Chi-square tests, logistic regression, and GLM univariate analysis. The sample (N = 1965) was classified as generally iodine-adequate (median urinary iodine concentration = 129 µg/L; median iodine-to-creatinine ratio = 126 µg/g) according to the WHO's criteria. A greater proportion of children in the ≥250 µg/g group had below-average IQs, compared to children with less than 250 µg/g (p = 0.037), despite a sizable (though non-significant) proportion of children in the less-than-250 µg/g group also presenting below-average IQs, at the bottom of the iodine distribution (<50 µg/g). The proportion of below-average IQs increased with increasingly elevated iodine concentrations (p = 0.047). The association remained significant after the adjustment for confounders, with the elevated iodine group showing increased odds of having below-average IQs when compared with the non-elevated iodine group (OR 1.55; 95% CI 1.11−2.17; p = 0.011). Consistently, the former group presented a lower mean IQ than the latter (p = 0.006). High iodine intake was associated with lower IQs even in a population classified as iodine-adequate. These results bear on child cognition and on initiatives involving iodine supplementation.


Assuntos
Iodo , Criança , Humanos , Pré-Escolar , Creatinina/urina , Portugal , Iodo/urina , Estado Nutricional , Testes de Inteligência , Iodetos
10.
Polymers (Basel) ; 14(17)2022 Sep 02.
Artigo em Inglês | MEDLINE | ID: mdl-36080721

RESUMO

Microplastics (MP) are spread into all ecosystems and represent a threat to the equilibrium of the environment and human health, not only due to their intrinsic characteristics but also to their action as effective carriers of contaminants, such as pesticides, pharmaceuticals, polychlorinated biphenyls and polycyclic aromatic hydrocarbons. The pesticide α-endosulfan is persistent and spread in the environment. The MP are another possible way of dissemination to be considered in the fate of this pesticide. The adsorption dynamics of α-endosulfan by six different MP (low-density polyethylene­LDPE, polyethylene-co-vinyl acetate, unplasticized polyvinyl chloride, polyamide 6, polystyrene granule, polypropylene granule) with different sizes/shapes and chemical compositions were evaluated. The most critical situation was identified for the system LDPE (particle size < 300 µm). Equilibrium studies (48 h equilibrium time) were performed for distilled, tap and filtered river water. Based on the Langmuir model parameters, the highest maximum adsorption capacity was obtained for distilled water, followed by filtered river and tap waters (i.e., 366 ± 39, 247 ± 38, 157 ± 22 µg/g). The obtained results demonstrate the important role that microplastics may have in the fate and transport of pesticides and their potentially harmful effect on the environment, which requires further investigation.

11.
Toxics ; 10(6)2022 Jun 10.
Artigo em Inglês | MEDLINE | ID: mdl-35736922

RESUMO

In recent decades, citizen awareness of toxic chemicals has been a topic of interest, particularly concerning national and international policy decision makers, expert/scientific platforms, and health protection organizations (WHO, UNEP, CDC, EFSA, IPEN, etc [...].

12.
Artigo em Inglês | MEDLINE | ID: mdl-35565001

RESUMO

Plastics have been one of the most useful materials in the world, due to their distinguishing characteristics: light weight, strength, flexibility, and good durability. In recent years, the growing consumption of plastics in industries and domestic applications has revealed a serious problem in plastic waste treatments. Pollution by microplastics has been recognized as a serious threat since it may contaminate all ecosystems, including oceans, terrestrial compartments, and the atmosphere. This micropollutant is spread in all types of environments and is serving as a "minor but efficient" vector for carrier contaminants such as pesticides, pharmaceuticals, metals, polychlorinated biphenyls (PCBs), and polycyclic aromatic hydrocarbons (PAHs). The need to deeply study and update the evolution of microplastic sources, toxicology, extraction and analysis, and behavior is imperative. This review presents an actual state of microplastics, addressing their presence in the environment, the toxicological effects and the need to understand their extent, their interactions with toxic pollutants, the problems that arise in the definition of analytical methods, and the possible alternatives of treatments.


Assuntos
Microplásticos , Poluentes Químicos da Água , Ecossistema , Monitoramento Ambiental , Plásticos/toxicidade , Águas Residuárias/análise , Poluentes Químicos da Água/análise
13.
Foods ; 11(5)2022 Mar 03.
Artigo em Inglês | MEDLINE | ID: mdl-35267379

RESUMO

Neuroprotection is a need that remains unmet in treating chronic neurodegenerative disorders, despite decades of extensive research. To find new neuroprotective compounds, extracts of Himanthalia elongata (L.) S.F.Gray and of Eisenia bicyclis (Kjellman) Setchell were obtained through subcritical water extraction applying a four-step temperature gradient. The fractions obtained were screened against brain enzymes involved in neurodegenerative etiology, namely in Alzheimer's and Parkinson's diseases, and against reactive oxygen and nitrogen species, all contributing factors to the progression of neurodegeneration. Results showed no significant enzyme inhibition but strong radical scavenging activities, particularly in the fourth fraction, extracted at the highest temperature (250 °C), highlighting their ability to retard oxidative and nitrosative stresses. At higher temperatures, fractions were composed of phenolic compounds and Maillard reaction products, a combination that contributed to their antioxidant activity and, consequently, their neuroprotective properties. All fractions were evaluated for the presence of iodine, 14 organochlorine and 7 organophosphorus pesticides, and pharmaceuticals used in Alzheimer's and Parkinson's diseases (14), psychiatric drugs (8), and metabolites (8). The fractions studied did not present any of the screened contaminants, and only fraction 1 of E. bicyclis should be used with caution due to iodine content.

14.
J Ethnopharmacol ; 290: 115107, 2022 May 23.
Artigo em Inglês | MEDLINE | ID: mdl-35176467

RESUMO

ETHNOPHARMACOLOGICAL RELEVANCE: Alzheimer's disease is the most common form of dementia, but its treatment options remain few and ineffective. To find new therapeutic strategies, natural products have gained interest due to their neuroprotective potential, being able to target different pathological hallmarks associated with this disorder. Several plant species are traditionally used due to their empirical neuroprotective effects and it is worth to explore their mechanism of action. AIM OF THE STUDY: This study intended to explore the neuroprotective potential of seven traditional medicinal plants, namely Scutellaria baicalensis, Ginkgo biloba, Hypericum perforatum, Curcuma longa, Lavandula angustifolia, Trigonella foenum-graecum and Rosmarinus officinalis. The safety assessment with reference to pesticides residues was also aimed. MATERIALS AND METHODS: Decoctions prepared from these species were chemically characterized by HPLC-DAD and screened for their ability to scavenge four different free radicals (DPPH•, ABTS•+, O2•‒ and •NO) and to inhibit enzymes related to neurodegeneration (cholinesterases and glycogen synthase kinase-3ß). Cell viability through MTT assay was also evaluated in two different brain cell lines, namely non-tumorigenic D3 human brain endothelial cells (hCMEC/D3) and NSC-34 motor neurons. Furthermore, and using GC, 21 pesticides residues were screened. RESULTS: Regarding chemical composition, chromatographic analysis revealed the presence of several flavonoids, phenolic acids, curcuminoids, phenolic diterpenoids, one alkaloid and one naphthodianthrone in the seven decoctions. All extracts were able to scavenge free radicals and were moderate glycogen synthase kinase-3ß inhibitors; however, they displayed weak to moderate acetylcholinesterase and butyrylcholinesterase inhibition. G. biloba and L. angustifolia decoctions were the less cytotoxic to hCMEC/D3 and NSC-34 cell lines. No pesticides residues were detected. CONCLUSIONS: The results extend the knowledge on the potential use of plant extracts to combat multifactorial disorders, giving new insights into therapeutic avenues for Alzheimer's disease.


Assuntos
Doença de Alzheimer/patologia , Fármacos Neuroprotetores/farmacologia , Extratos Vegetais/farmacologia , Plantas Medicinais/química , Linhagem Celular , Sobrevivência Celular/efeitos dos fármacos , Colinesterases/efeitos dos fármacos , Relação Dose-Resposta a Droga , Sequestradores de Radicais Livres/metabolismo , Glicogênio Sintase/efeitos dos fármacos , Humanos , Medicina Tradicional Chinesa/métodos , Fármacos Neuroprotetores/efeitos adversos , Resíduos de Praguicidas/análise , Extratos Vegetais/efeitos adversos
15.
Sci Total Environ ; 791: 148395, 2021 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-34412412

RESUMO

Every year, after grape harvesting, high quantities of vine-canes are generated. Due to the high amount of bioactive compounds present in this woody material, several studies reported their potential to be used in different sustainable applications. However, before employing vine-canes in this kind of products, their safety needs to be assessed. A robust method for identification and quantification of 30 environmental contaminants (12 organochloride pesticides (OCPs), 6 organophosphorus pesticides (OPPs), 5 polychlorinated biphenyls (PCBs) and 7 brominated flame retardants (BFRs)) in vine-canes was developed. For that, the extraction and clean-up procedures were optimized, namely the vine-canes size, the QuEChERS (quick, easy, cheap, effective, rugged and safe) composition and the amount of carbon used in the dispersive-solid phase extraction (d-SPE). Suitable analytical parameters were obtained: linearity (r2) >0.99 for all the studied compounds and for the solvent and matrix-matched standards; relative standard deviation (RSD) below 14%; and mean recoveries for two spiking levels (10 and 20 µg/kg) between 75 and 103%, excepting for the PCBs that ranged between 59 and 105%. The limit of detection (LOD) and quantification (LOQ) ranged between 0.38 and 1.09 and 1.26 to 3.64 µg/kg, respectively. Regarding the analysis of 19 vine-cane samples, corresponding to four different varieties (Touriga Nacional, Tinta Roriz, Alvarinho, and Loureiro) collected in four different years in the North of Portugal, five contaminants (aldrin, 2,2-bis(4-chlorophenyl)-1,1-dichloroethylene (p,p'-DDE), α-hexachlorocyclohexane (α-HCH), 2,4,4'-trichlorobiphenyl (PCB28), and 2,2',4,5,5'-pentachlorobiphenyl (PCB101)) were detected. However, only α-HCH (5.85 ± 0.32 to 5.99 ± 0.25 µg/kg) and aldrin (2.44 ± 0.15 µg/kg) were quantified above the LOQ. The screening of environmental contaminants in vine-canes is essential to waste valorization, especially if the goal is to apply them in products for human consumption.


Assuntos
Praguicidas , Bengala , Fazendas , Humanos , Compostos Organofosforados , Portugal
16.
J Chromatogr A ; 1636: 461797, 2021 Jan 11.
Artigo em Inglês | MEDLINE | ID: mdl-33348272

RESUMO

Organochlorine pesticides (OCPs) are synthetic compounds less used nowadays due to their toxicity combined with slow degradation which leads to accumulation in the environment. Gas-diffusion microextraction (GDME) was employed prior to gas chromatography with electron capture detection (GC-ECD) and mass spectrometry (GC-MS). For the first time, the low-cost, eco-friendly GDME system was used to extract the OCPs directly from milk samples and associated with GC-ECD. Parameters that affect GDME's performance (extract volume, extraction time, and temperature) were optimized. The calibration curves of all OCPs (α- and ß-hexachlorocyclohexane, lindane, hexachlorobenzene, p,p'-DDE, aldrin, dieldrin, and α-endosulfan) had coefficients of determination (r2) ranging from 0.991 to 0.995, and limits of detection (LODs) values ranging from 3.7 to 4.8 µg L-1. This method also provided satisfactory values for precision with relative standard deviations (RSDs) lower than 10% and recoveries above 90%. As a proof-of-concept, several commercial milk samples were analyzed, aldrin was found in one of them but below the maximum residue limits.


Assuntos
Elétrons , Cromatografia Gasosa-Espectrometria de Massas/métodos , Hidrocarbonetos Clorados/análise , Leite/química , Praguicidas/análise , Animais , Difusão , Resíduos de Praguicidas/análise , Reprodutibilidade dos Testes
17.
Mikrochim Acta ; 187(3): 184, 2020 02 22.
Artigo em Inglês | MEDLINE | ID: mdl-32088788

RESUMO

An electrochemical magnetic immunosensing strategy was developed for the determination of HER2-ECD, a breast cancer biomarker, and breast cancer cells in human serum. A sandwich assay was performed on carboxylic acid-functionalized magnetic beads (MBs) using a screen-printed carbon electrode (SPCE) as transducer surface. The affinity process was detected using electroactive labels; core/shell streptavidin-modified CdSe@ZnS Quantum Dots (QDs). Cd2+ ions, released from the QDs, were determined by differential pulse anodic stripping voltammetry (DPASV). An assay time of 90 min, with an actual hands-on time of about 20 min, a linear range between 0.50-50 ng·mL-1 of HER2-ECD and a limit of detection of 0.29 ng·mL-1 were achieved. Analysis of live breast cancer cells was also performed using the optimized assay. Breast cancer cell lines SK-BR-3 (a HER2-positive cell line), MDA-MB-231 (a HER2-negative cell line) and MCF-7 (a cell line with low HER2 expression) were tested. The selectivity of the assay towards SK-BR-3 cells was confirmed. A concentration-dependent signal that was 12.5× higher than the signal obtained for the HER2-negative cells (MDA-MB-231) and a limit of detection of 2 cells·mL-1 was obtained. Graphical abstractSchematic representation of the electrochemical immunomagnetic assay for the determination of the breast cancer biomarker HER2-ECD and cancer cells using magnetic beads (MBs), a screen-printed carbon electrode (SPCE) as transducer surface and quantum dots (QD) as electroactive labels.


Assuntos
Biomarcadores Tumorais/sangue , Técnicas Eletroquímicas/métodos , Pontos Quânticos/química , Feminino , Humanos
18.
J Agric Food Chem ; 68(10): 3260-3266, 2020 Mar 11.
Artigo em Inglês | MEDLINE | ID: mdl-32050063

RESUMO

One of the main challenges for analytical laboratories and food safety authorities is the control of food contaminants hazardous to human health. For the first time, a simple, fast, and cost-effective sample preparation method is proposed as an extraction technique to determine 12 brominated flame retardants (BFRs) (seven polybrominated diphenyl ether (PBDE) congeners and five novel BFRs) in Capsicum cultivars. Different QuEChERS and dispersive solid-phase extract (d-SPE) sorbent compositions were evaluated in terms of recovery and matrix effects. The best results were obtained with citrate-buffered version QuEChERS and a cleanup step, with 150 mg of MgSO4, 50 mg of primary secondary amine (PSA), 50 mg of C18, and 5 mg of carbon. The limit of detection (LOD) was between 1.4 and 9.3 µg/kg and R2 > 0.99. Recoveries and matrix effects were between 66 and 104% and 0.58 and 2.18, respectively. The relative standard deviations from repeatability and reproducibility studies and estimation of measurement uncertainty were lower than 20%. Gas chromatography coupled with a mass spectrometer was used to confirm the presence of BFRs in the samples. Novel BFRs were detected lower than the LOD.


Assuntos
Capsicum/química , Retardadores de Chama/análise , Retardadores de Chama/isolamento & purificação , Éteres Difenil Halogenados/química , Éteres Difenil Halogenados/isolamento & purificação , Extração em Fase Sólida/métodos , Contaminação de Alimentos/análise , Frutas/química , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Limite de Detecção , Extração em Fase Sólida/instrumentação
19.
J Chromatogr A ; 1566: 1-12, 2018 Sep 07.
Artigo em Inglês | MEDLINE | ID: mdl-30017087

RESUMO

Magnetic nanoparticles (MNPs) with different sizes and characteristics were synthesized to be used as a QuEChERS sorbents for the determination of seven organophosphorus pesticides (OPPs) in strawberries by gas chromatography analysis with flame photometric and mass spectrometry detection. To achieve the optimum conditions of modified QuEChERS procedure several parameters affecting the cleanup efficiency including the amount of the sorbents and cleanup time were investigated. The results were compared with classical QuEChERS methodologies and the modified QuEChERS procedure using MNPs showed the better performance. Under the optimum conditions of the new methodology, three spiking levels (25, 50 and 100 µg kg-1) were evaluated in a strawberry sample. The results showed that the average recovery was 93% and the relative standard deviation was less than 12%. The enrichment factor ranged from 111 to 145%. The good linearity with coefficients of determination of 0.9904-0.9991 was obtained over the range of 25-250 µg kg-1 for 7 OPPs. It was determined that the MNPs have an excellent function as sorbent when purified even using less amount of sorbents and the magnetic properties allowed non-use of the centrifugation in cleanup step. The new methodology was applied in strawberry samples from conventional and organic farming. The new sorbents were successfully applied for extraction and determination of OPPs in strawberries.


Assuntos
Análise de Alimentos/métodos , Fragaria/química , Cromatografia Gasosa-Espectrometria de Massas , Praguicidas/análise , Microextração em Fase Sólida , Magnetismo
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