Your browser doesn't support javascript.
loading
Mostrar: 20 | 50 | 100
Resultados 1 - 20 de 199
Filtrar
1.
Mycotoxin Res ; 2024 May 16.
Artigo em Inglês | MEDLINE | ID: mdl-38753281

RESUMO

Poultry farming has developed into one of Algeria's most productive industrial farming because of the growing demand for sources of protein among Algerian society. Laying hen feed consists mainly of cereals, which can be contaminated with molds and subsequently with their secondary metabolites known as mycotoxins. These later can pose a serious danger to the production and quality of eggs in the commercial layer industry. This work focuses on the detection of emerging mycotoxins, mainly enniatins (ENNs) and beauvericin (BEA), in poultry feed and eggs from different locations in Algeria. Two different QuEChERS-based extractions were established to extract ENNs and BEA from chicken feed and eggs. The determination of mycotoxin occurrence was achieved by a UHPLC-MS/MS method using 0.1% (v/v) formic acid in water and MeOH as mobile phase, an ESI interface operating in positive mode, and a triple quadrupole mass spectrometer operating in MRM for the detection. Matrix-matched calibration curves were carried out for both matrices, obtaining good linearity (R2 > 0.99). The method performance was assessed in terms of extraction recovery (from 87 to 107%), matrix effect (from - 47 to - 86%), precision (RSD < 15%), and limits of quantitation (≤ 1.1 µg/kg for feed and ≤ 0.8 µg/kg for eggs). The analysis of 10 chicken feed samples and 35 egg samples composed of a 10-egg pool each showed that ENN B1 was the most common mycotoxin (i.e., found in 9 feed samples) with contamination levels ranging from 3.6 to 41.5 µg/kg, while BEA was detected only in one feed sample (12 µg/kg). However, eggs were not found to be contaminated with any mycotoxin at the detection limit levels. Our findings indicate that the searched mycotoxins are present in traces in feed and absent in eggs. This can be explained by the application of a mycotoxin binder. However, this does not put a stop on the conduction of additional research and ultimately setting regulations to prevent the occurrence of emerging mycotoxins.

2.
Int J Biol Macromol ; 262(Pt 2): 130132, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38354919

RESUMO

Inhibition of SARS-CoV-2 membrane fusion is a highly desired target to combat COVID-19. The interaction between the spike's heptad repeat (HR) regions 1 (HR1) and 2 (HR2) is a crucial step during the fusion process and these highly conserved HR regions constitute attractive targets for fusion inhibitors. However, the relative importance of each subregion of the long HR1-HR2 interface for viral inhibition remains unclear. Here, we designed, produced, and characterized a series of chimeric miniproteins that mimic two different half subdomains of HR1. The proteins were designed as single polypeptide chains that spontaneously fold into antiparallel trimeric helical bundles aimed at structurally imitate the molecular surface of each HR1 half subregion. All the miniproteins folded stably as helical structures and could bind complementary HR2 peptides with moderate affinity. However, only the miniproteins mimicking the N-terminal HR1 half subdomain, but not those imitating C-terminal one, could inhibit cell infection by SARS-COV-2 real viruses in cell cultures. Most interestingly, the inhibitory activity of the miniproteins correlated with their structural stability, but not with their relative binding affinity for HR2 peptides. These results are highly relevant for designing more focused and active fusion inhibitors targeting the highly conserved HR2 region of the Spike.


Assuntos
COVID-19 , SARS-CoV-2 , Humanos , SARS-CoV-2/metabolismo , Sequência de Aminoácidos , Proteínas do Envelope Viral/química , Glicoproteína da Espícula de Coronavírus/genética , Glicoproteína da Espícula de Coronavírus/metabolismo , Peptídeos/química , Antirretrovirais/farmacologia , Fusão de Membrana
3.
Angew Chem Int Ed Engl ; 63(11): e202400261, 2024 Mar 11.
Artigo em Inglês | MEDLINE | ID: mdl-38246884

RESUMO

The formation of highly organized metal-DNA structures has significant implications in bioinorganic chemistry, molecular biology and material science due to their unique properties and potential applications. In this study, we report on the conversion of single-stranded polydeoxycytidine (dC15 ) into a Pd-DNA supramolecular structure using the [Pd(Aqa)] complex (Aqa=8-amino-4-hydroxyquinoline-2-carboxylic acid) through a self-assembly process. The resulting Pd-DNA assembly closely resembles a natural double helix, with continuous [Pd(Aqa)(C)] (C=cytosine) units serving as palladium-mediated base pairs, forming interbase hydrogen bonds and intrastrand stacking interactions. Notably, the design of the [Pd(Aqa)] complex favours the interaction with cytosine, distinguishing it from our previously reported [Pd(Cheld)] complex (Cheld=chelidamic acid). This finding opens possibilities for creating heteroleptic Pd-DNA hybrids where different complexes specifically bind to nucleobases. We confirmed the Pd-DNA supramolecular structural assembly and selective binding of the complexes using NMR spectroscopy, circular dichroism, mass spectrometry, isothermal titration calorimetry, and DFT calculations.


Assuntos
DNA , Paládio , Pareamento de Bases , Paládio/química , DNA/química , Citosina/química
4.
J Chromatogr A ; 1717: 464666, 2024 Feb 22.
Artigo em Inglês | MEDLINE | ID: mdl-38266594

RESUMO

Cyanotoxins constitute a group of toxic secondary metabolites, the presence of which in any water body poses a major health risk. Moreover, advanced organisms such as edible plants exposed to these toxins, are a possible pathway for human exposure. Green analytical chemistry is demanding environmentally friendly analytical techniques. In this sense, we propose the use of capillary electrophoresis coupled to tandem mass spectrometry (CE-MS/MS) to determine a mixture of eight cyanotoxins belonging to three different classes: cyclic peptides (microcystin-LR, microcystin-RR and nodularin), alkaloids (cylindrospermopsin and anatoxin-a) and three isomeric non-protein amino acids (ß-methylamino-l-alanine, 2,4-diaminobutyric acid and N-(2-aminoethyl)glycine). Separation was achieved by using an acidic background electrolyte consisting of 2 M formic acid and 20% acetonitrile in water. Parameters affecting MS/MS detection and the sheath-liquid interface were also studied. Finally, a combination of pH-junction, field-amplified sample stacking (FASS) and acid barrage as online preconcentration strategies, was employed to improve sensitivity and efficiency. The online preconcentration applied, in combination with a dual cartridge solid-phase extraction (SPE) system, allows to obtain limits of detection in the very low range of µg·L-1 for these multiclass cyanotoxins in reservoir water samples (from 0.005 to 0.10 µg·L-1). Furthermore, for the first time cyanotoxins are analysed in spinach samples through CE-MS/MS using the same SPE procedure, following lyophilisation and solid-liquid extraction with 6 mL 80 % aqueous MeOH.


Assuntos
Spinacia oleracea , Espectrometria de Massas em Tandem , Humanos , Espectrometria de Massas em Tandem/métodos , Água , Cromatografia Líquida de Alta Pressão , Toxinas de Cianobactérias , Microcistinas/análise , Eletroforese Capilar
5.
Am J Infect Control ; 52(4): 400-409, 2024 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-37422066

RESUMO

BACKGROUND: To analyze whether the application of topical formulas as cosmetics or sunscreens could affect the skin thermographic readings in terms of infection control in pandemic situations. METHODS: The temperature of the skin of the dorsal region of the back and the face of 20 volunteers was followed after the application of 6 different types of gels, sunscreens, and make-up under controlled temperature and humidity conditions. High-resolution thermographic images were analyzed to calculate the temperature of treated skin compared to skin free of topical products. RESULTS: The application of hydroalcoholic gel resulted in a mean drop of more than 2°C just after 1 minute followed by organic sunscreens until 1.7°C. Recovery was observed progressively until minute 9. Color make-up type formulas, rich in iron oxide as well as sunscreens with mineral filters had little or no effect on the skin thermal response. CONCLUSIONS: It is possible to alter the skin temperature almost immediately by using hydroalcoholic gels and sunscreen cosmetics. So, it is possible to produce false negative data in the readings of patients screened thermically.


Assuntos
Cosméticos , Protetores Solares , Humanos , Pele , Géis , Raios Ultravioleta
6.
Dis Colon Rectum ; 67(4): 514-522, 2024 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-38100620

RESUMO

BACKGROUND: Aggressive angiomyxoma is a very rare mesenchymal tumor most commonly found in the pelvic and perineal regions. Although many are estrogen and progesterone hormone receptor positive, the pathogenesis is unknown. Due to its rarity, there is a paucity of literature relating to this pathology. This article presents a case series on the management of aggressive angiomyxoma of the pelvis. OBJECTIVE: To present a 35-year experience managing aggressive angiomyxoma of the pelvis. DESIGN: This was a retrospective single-system analysis. SETTINGS: This study was conducted at a quaternary referral academic health care system. PATIENTS: All patients treated for aggressive angiomyxoma of the pelvis. INTERVENTIONS: All patients underwent surgical or medical management of their disease. MAIN OUTCOME MEASURES: The primary outcomes were disease recurrence and mortality. Secondary outcomes included risk factors for recurrence. RESULTS: A total of 32 patients (94% women) were identified with a median follow-up of 65 months. Thirty patients (94%) underwent operative resection and 2 patients were treated solely with medical management. Fifteen achieved an R0 resection (negative microscopic margins) at the index operation, of which 4 (27%) experienced tumor recurrence. There were no mortalities. No risk factors for disease recurrence were identified. LIMITATIONS: Limitations to our study include its nonrandomized retrospective nature, single health care system experience, and small patient sample size. CONCLUSIONS: Aggressive angiomyxoma is a rare, slow-growing tumor with locally invasive features and a high potential for recurrence even after resection with negative margins. Imaging modalities such as CT or MRI should be obtained to aid in diagnosis and surgical planning. Workup should be paired with preoperative biopsy and testing for hormone receptor status, which can increase diagnostic accuracy and guide medical treatment. Close posttreatment surveillance is imperative to detect recurrence. See Video Abstract . ANGIOMIXOMA AGRESIVO DE PELVIS EXPERIENCIA DE AOS: ANTECEDENTES:El angiomixoma agresivo es un tumor mesenquimal muy raro que se encuentra más comúnmente en las regiones pélvica y perineal. Aunque muchos son positivos para los receptores hormonales como el estrógeno y la progesterona, la patogénesis es aún desconocida. Debido a su rareza, existe escasa literatura relacionada con esta patología. Este artículo presenta una serie de casos sobre el tratamiento del angiomixoma agresivo de pelvis.OBJETIVO:Presentar una experiencia de 35 años en el manejo del angiomixoma agresivo de pelvis.DISEÑO:Este fue un análisis retrospectivo de sistema único.AJUSTES:Este estudio se llevó a cabo en un sistema de salud académico de referencia de nivel cuaternario.PACIENTES:Todos los pacientes tratados por angiomixoma agresivo de pelvis.INTERVENCIONES:Todos los pacientes se sometieron a tratamiento quirúrgico y/o médico de su enfermedad.PRINCIPALES MEDIDAS DE RESULTADO:Los resultados primarios fueron la recurrencia de la enfermedad y la mortalidad. Los resultados secundarios incluyeron factores de riesgo de recurrencia.RESULTADOS:Se identificaron un total de 32 pacientes (94% mujeres) con una mediana de seguimiento de 65 meses. Treinta (94%) fueron sometidos a resección quirúrgica y dos fueron tratados únicamente con tratamiento médico. Quince lograron una resección R0 (márgenes microscópicos negativos) en la operación inicial, de los cuales cuatro (27%) experimentaron recurrencia tumoral. No hubo mortalidades. No se identificaron factores de riesgo para la recurrencia de la enfermedad.LIMITACIONES:Las limitaciones de nuestro estudio incluyen su naturaleza retrospectiva no aleatoria, la experiencia de un solo sistema de atención médica y el tamaño pequeño de la muestra de pacientes.CONCLUSIONES:El angiomixoma agresivo es un tumor raro, de crecimiento lento, con características localmente invasivas y un alto potencial de recurrencia incluso después de una resección con márgenes negativos. Se deben obtener modalidades de imágenes como CT y/o MRI para la ayuda diagnóstica y la planificación quirúrgica. El estudio debe combinarse con una biopsia preoperatoria y pruebas del estado de los receptores hormonales, que pueden aumentar la precisión del diagnóstico y guiar el tratamiento médico. Es imperativa una estrecha vigilancia posterior al tratamiento para detectar recurrencia. (Traducción-Dr Osvaldo Gauto ).


Assuntos
Mixoma , Pelve , Humanos , Feminino , Masculino , Estudos Retrospectivos , Pelve/patologia , Períneo/patologia , Imageamento por Ressonância Magnética , Mixoma/diagnóstico , Mixoma/cirurgia , Mixoma/patologia
7.
Foods ; 12(24)2023 Dec 13.
Artigo em Inglês | MEDLINE | ID: mdl-38137267

RESUMO

Consumption of fried foods is associated with a higher risk of cardiovascular and other diseases; therefore, consumers are looking to reduce fat intake. We evaluated the effect of high-protein breaders and fiber on oil absorption and quality attributes in chicken nuggets, using flour blends (wheat, chickpea, coconut, oil-quinoa-chia), soy protein concentrate, and brewers' spent grain. We evaluated the chemical composition, water and oil retention capacity (ORC), viscosity profile, and flour particle size distribution, along with the developed breaders (Formulation 1 and 2) and a commercial breader (CB), in addition to texture, color, fat, and moisture contents of the fried chicken nuggets prepared with the developed breaders and the CB. The total dietary fiber content (TDF) of the nuggets breaded with only Formulation-1 and CB was determined. Nuggets breaded with Formulation-1 showed lower (p ≤ 0.05) ORC, better moisture retention (67.6%), and more TDF (4.5% vs. 2.3%, p ≤ 0.05) compared to CB-breaded nuggets. Nuggets with Formulation-1 showed the expected texture and color characteristics for fried products. Formulation-1 has the potential to be used as a breader due to its moisture, reduced ORC, and the texture and color it imparts to the fried nuggets, providing higher amounts of nutrients and possible health benefits.

8.
Artigo em Inglês | LILACS-Express | LILACS | ID: biblio-1535963

RESUMO

We describe the first case in our environment of endoscopic ultrasound (EUS)-assisted transgastric endoscopic retrograde cholangiopancreatography in a patient with gastric bypass surgery. The procedure was performed with a side-viewing duodenoscope through a jejunogastrostomy using apposing stents, placed with EUS assistance, and a standard technique and instruments.


Se describe el primer caso en nuestro medio de colangiopancreatografía retrógrada endoscópica transgástrica asistida por endosonografía en una paciente con cirugía de baipás gástrico. El procedimiento se realizó con duodenoscopio de visión lateral a través de una yeyunogastrostomía por stent de aposición, emplazado con asistencia endosonográfica y con una técnica e instrumental estándar.

9.
Am J Bot ; 110(11): e16249, 2023 11.
Artigo em Inglês | MEDLINE | ID: mdl-37792319

RESUMO

PREMISE: Bryophytes form a major component of terrestrial plant biomass, structuring ecological communities in all biomes. Our understanding of the evolutionary history of hornworts, liverworts, and mosses has been significantly reshaped by inferences from molecular data, which have highlighted extensive homoplasy in various traits and repeated bursts of diversification. However, the timing of key events in the phylogeny, patterns, and processes of diversification across bryophytes remain unclear. METHODS: Using the GoFlag probe set, we sequenced 405 exons representing 228 nuclear genes for 531 species from 52 of the 54 orders of bryophytes. We inferred the species phylogeny from gene tree analyses using concatenated and coalescence approaches, assessed gene conflict, and estimated the timing of divergences based on 29 fossil calibrations. RESULTS: The phylogeny resolves many relationships across the bryophytes, enabling us to resurrect five liverwort orders and recognize three more and propose 10 new orders of mosses. Most orders originated in the Jurassic and diversified in the Cretaceous or later. The phylogenomic data also highlight topological conflict in parts of the tree, suggesting complex processes of diversification that cannot be adequately captured in a single gene-tree topology. CONCLUSIONS: We sampled hundreds of loci across a broad phylogenetic spectrum spanning at least 450 Ma of evolution; these data resolved many of the critical nodes of the diversification of bryophytes. The data also highlight the need to explore the mechanisms underlying the phylogenetic ambiguity at specific nodes. The phylogenomic data provide an expandable framework toward reconstructing a comprehensive phylogeny of this important group of plants.


Assuntos
Briófitas , Hepatófitas , Filogenia , Briófitas/genética , Plantas/genética , Hepatófitas/genética
11.
J Chromatogr A ; 1706: 464239, 2023 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-37541059

RESUMO

Cationic, anionic, zwitterionic and, partially polar metabolites are very important constituents of blood serum. Several of these metabolites underpin the core metabolism of cells (e.g., Krebs cycle, urea cycle, proteins synthesis, etc.), while others might be considered ancillary but still important to grasp the status of any organism through blood serum analysis. Due to its wide chemical diversity, modern metabolomics analysis of serum is still struggling to provide a complete and comprehensive picture of the polar metabolome, due to the limitations of each specific analytical method. In this study, two metabolomics-based analytical methods using the most successful techniques for polar compounds separation in human serum samples, namely hydrophilic interaction liquid chromatography (HILIC) and capillary electrophoresis (CE), are evaluated, both coupled to a high-resolution time-of-flight mass spectrometer via electrospray ionization (ESI-Q-TOF-MS). The performance of the two methods have been compared using five terms of comparison, three of which are specific to metabolomics, such as (1) compounds' detectability (2) Pezzatti score (Pezzatti et al. 2018), (3) intra-day precision (repeatability), (4) ease of automatic analysis of the data (through a common deconvolution alignment and extrapolation software, MS-DIAL, and (5) time & cost analysis. From this study, HILIC-MS proved to be a better tool for polar metabolome analysis, while CE-MS helped identify some interesting variables that gave it interest in completing metabolome coverage in metabolomics studies. Finally, in this framework, MS-DIAL demonstrates for the first time its ability to process CE data for metabolomics, although it is not designed for it.


Assuntos
Metabolômica , Soro , Humanos , Cromatografia Líquida/métodos , Eletroforese Capilar/métodos , Interações Hidrofóbicas e Hidrofílicas , Metaboloma , Metabolômica/métodos
12.
Angew Chem Int Ed Engl ; 62(41): e202307884, 2023 Oct 09.
Artigo em Inglês | MEDLINE | ID: mdl-37604782

RESUMO

Triangulenes are a class of open-shell triangular graphene flakes with total spin increasing with their size. In the last years, on-surface-synthesis strategies have permitted fabricating and engineering triangulenes of various sizes and structures with atomic precision. However, direct proof of the increasing total spin with their size remains elusive. In this work, we report the combined in-solution and on-surface synthesis of a large nitrogen-doped triangulene (aza-[5]-triangulene) on a Au(111) surface, and the detection of its high-spin ground state. Bond-resolved scanning tunneling microscopy images uncovered radical states distributed along the zigzag edges, which were detected as weak zero-bias resonances in scanning tunneling spectra. These spectral features reveal the partial Kondo screening of a high-spin state. Through a combination of several simulation tools, we find that the observed distribution of radical states is explained by a quintet ground state (S=2), instead of the quartet state (S=3/2) expected for the neutral species. This confirms that electron transfer to the metal substrate raises the spin of the ground state. We further provide a qualitative description of the change of (anti)aromaticity introduced by N-substitution, and its role in the charge stabilization on a surface, resulting in an S=2 aza-triangulene on Au(111).

13.
Sports (Basel) ; 11(6)2023 Jun 13.
Artigo em Inglês | MEDLINE | ID: mdl-37368568

RESUMO

The purpose of this paper was to conduct a systematic review and meta-analysis of studies examining the differences in the mean propulsive velocities between men and women in the different exercises studied (squat, bench press, inclined bench press and military press). Quality Assessment and Validity Tool for Correlational Studies was used to assess the methodological quality of the included studies. Six studies of good and excellent methodological quality were included. Our meta-analysis compared men and women at the three most significant loads of the force-velocity profile (30, 70 and 90% of 1RM). A total of six studies were included in the systematic review, with a total sample of 249 participants (136 men and 113 women). The results of the main meta-analysis indicated that the mean propulsive velocity is lower in women than men in 30% of 1RM (ES = 1.30 ± 0.30; CI: 0.99-1.60; p < 0.001) and 70% of 1RM (ES = 0.92 ± 0.29; CI: 0.63, 1.21; p < 0.001). In contrast, for the 90% of the 1RM (ES = 0.27 ± 0.27; CI: 0.00, 0.55), we did not find significant differences (p = 0.05). Our results support the notion that prescription of the training load through the same velocity could cause women to receive different stimuli than men.

14.
J Agric Food Chem ; 71(26): 10178-10189, 2023 Jul 05.
Artigo em Inglês | MEDLINE | ID: mdl-37347990

RESUMO

The increased consumption of blue-green algae (BGA)-based dietary supplements has raised concern about their food safety, especially about cyanotoxin presence. The hyphenation of liquid chromatography with ion mobility mass spectrometry represents a relevant tool to screen several compounds in a large variety of food matrices. In this work, ultrahigh-performance liquid chromatography coupled to traveling wave ion mobility spectrometry/quadrupole time-of-flight mass spectrometry (UHPLC-TWIMS-QTOF) was employed to establish the first comprehensive TWIMS-derived collision cross section database (TWCCSN2) for phycotoxins. The database included 20 cyanotoxins and 1 marine toxin. Accurate m/z, retention times, and TWCCSN2 values were obtained for 81 adducts in positive and negative electrospray (ESI+/ESI-) modes. Reproducibility and robustness of the TWCCSN2 measurements were determined to be independent of the matrix. A screening was carried out on 19 commercial BGA dietary supplements of different composition. Cyanotoxins were confidently identified in five samples based on retention time, m/z, and TWCCSN2.


Assuntos
Toxinas de Cianobactérias , Toxinas Marinhas , Reprodutibilidade dos Testes , Espectrometria de Massas/métodos , Cromatografia Líquida
16.
Plant Foods Hum Nutr ; 78(2): 314-319, 2023 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-36913108

RESUMO

Wheat-flour (WF) tortillas are among the popular flatbreads used in northern Mexico to prepare 'burritos', which are widely accepted in the USA and other countries but have low nutritional quality. Therefore, to increase the protein and fiber contents, we replaced 10 or 20% of the WF with coconut (Cocos nucifera, variety Alto Saladita) flour (CF) and evaluated the effects on the dough rheology and quality of the composite tortillas. There were differences in the optimum mixing times among the doughs. The protein, fat, and ash contents of the tortillas increased (p < 0.05) with increasing CF content. The carbohydrate content was unchanged (p > 0.05), but the 20% CF tortillas contained more fiber than the control tortilla. Tortilla firmness increased (p < 0.05) and extensibility decreased (p < 0.05) with increasing CF content. The 80:20 blended tortillas showed the highest firmness (7.9 N), whereas the control and 90:10 blended tortillas did not differ (p > 0.05) in firmness. There were no differences (p > 0.05) in extensibility between the composite tortillas. The physicochemical properties of the tortillas indicated that the 20% CF-containing tortilla was a more nutritious option to the wheat flour tortilla due to its higher dietary fiber and protein contents, in addition to the slight reduction seen in extensibility compared to the WF tortilla.


Assuntos
Farinha , Triticum , Triticum/química , Cocos , Pão , Reologia
17.
Crit Rev Anal Chem ; : 1-29, 2023 Mar 20.
Artigo em Inglês | MEDLINE | ID: mdl-36940156

RESUMO

Neonicotinoids (NNIs) are neuro-active and systemic insecticides widely used to protect crops from pest attack. During the last decades, there has been an increase concern about their uses and toxic effects, especially to beneficial and non-target insects such as pollinators. To assess potential health hazards and the environmental impacts derived from NNIs uses, a great variety of analytical procedures for the determination of their residues and their metabolites at trace level in environmental, biological and food samples have been reported. Due to the complexity of the samples, efficient sample pretreatment methods have been developed, which include mostly clean-up and preconcentration steps. On the other hand, among the analytical techniques used for their determination, high-performance liquid chromatography (HPLC) coupled to ultraviolet (UV) or mass spectrometry (MS) detection is the most widely used, although capillary electrophoresis (CE) has also been employed in the last years, considering some improvements in sensitivity when coupling with new MS detectors. In this review, we present a critical overview of analytical methods based on HPLC and CE reported in the last decade, discussing relevant and innovative sample treatments for the analysis of environmental, food and biological samples.

18.
Toxins (Basel) ; 15(2)2023 02 04.
Artigo em Inglês | MEDLINE | ID: mdl-36828442

RESUMO

In recent years, the consumption of blue-green algae (BGA) dietary supplements is increasing because of their health benefits. However, cyanobacteria can produce cyanotoxins, which present serious health risks. In this work we propose hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry (HILIC-MS/MS) to determine cyanotoxins in BGA dietary supplements. Target toxins, including microcystin-leucine-arginine (MC-LR) and microcystin-arginine-arginine (MC-RR), nodularin, anatoxin-a and three non-protein amino acids, ß-N-methylamino-L-alanine (BMAA), 2,4-diaminobutyric acid (DAB) and N-(2-aminoethyl)glycine (AEG), were separated using a SeQuant ZIC-HILIC column. Cyanotoxin extraction was based on solid-liquid extraction (SLE) followed by a tandem-solid phase extraction (SPE) procedure using Strata-X and mixed-mode cation-exchange (MCX) cartridges. The method was validated for BGA dietary supplements obtaining quantification limits from 60 to 300 µg·kg-1. Nine different commercial supplements were analyzed, and DAB, AEG, and MCs were found in some samples, highlighting the relevance of monitoring these substances as precaution measures for the safe consumption of these products.


Assuntos
Cianobactérias , Microcistinas , Microcistinas/análise , Espectrometria de Massas em Tandem/métodos , Toxinas de Cianobactérias , Cromatografia Líquida/métodos , Cianobactérias/química , Suplementos Nutricionais/análise , Arginina , Interações Hidrofóbicas e Hidrofílicas , Cromatografia Líquida de Alta Pressão/métodos
19.
Methods Mol Biol ; 2551: 15-28, 2023.
Artigo em Inglês | MEDLINE | ID: mdl-36310193

RESUMO

Amyloid aggregation is a hallmark in many neuropathologies and other diseases of tremendous impact. It is increasingly evident that neuronal death associated with Alzheimer's disease (AD) is mainly produced by oligomers of the amyloid-ß (Aß) peptide. Yet little is known about the detailed structural and biophysical mechanisms of their formation. This lack of complete understanding comes from the labile nature and handling complexity of the oligomers. Consequently, providing reproducible and robust protocols for oligomer preparation is of particular importance.In this study, we describe detailed methods for the preparation and isolation of micellar oligomers of Aß that evolve towards larger and more stable oligomers enriched in beta-sheet structure and able to acquire a higher capacity to fibrillate. We also describe briefly some biophysical experiments allowing oligomer characterization.


Assuntos
Doença de Alzheimer , Peptídeos beta-Amiloides , Humanos , Peptídeos beta-Amiloides/química , Fragmentos de Peptídeos/química , Amiloide
20.
Talanta ; 253: 123946, 2023 Feb 01.
Artigo em Inglês | MEDLINE | ID: mdl-36167011

RESUMO

Enniatins (ENN) and beauvericin (BEA) are emerging mycotoxins that have been traditionally determined by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). However, to the best of our knowledge, no analytical methods based on capillary electrophoresis (CE)-MS/MS have been reported so far. Due to their non-polar nature, in this work, a non-aqueous CE (NACE) method coupled to quadrupole time-of-flight-MS is proposed for the first time to identify and quantify these mycotoxins. Determination was achieved in 4 min under optimum conditions: 40 mM ammonium acetate in 80:20 (v/v) acetonitrile-methanol (buffer), 30 kV (voltage), 80 cm (capillary length), 20 °C (capillary temperature) and 50 mbar × 30 s (injection). Higher selectivity can be achieved when compared with LC due to the formation of exclusive CE adducts such as [M + CH3CH2NH3]+. "All Ions" acquisition mode was selected as it allows the quantification of the usual ENNs, as well as the identity confirmation of less common ENNs. The method was validated for wheat samples, obtaining limits of quantification from 4.0 to 8.3 µg/kg depending on the emerging mycotoxin, recovery values higher than 87.4%, and intra- and inter-day precision values (RSDs) lower than 15.1% in all cases. Finally, 29 wheat samples were analyzed, finding 26 samples with concentrations of enniatin B higher than the limit of quantification (7.5-1480 µg/kg), 20 for enniatin B1 (5.2-550 µg/kg), 7 for enniatin A (10-55 µg/kg), 4 for enniatin A1 (12.6-77 µg/kg) and 5 for BEA (9.2-16.4 µg/kg). Moreover, two other ENNs were tentatively identified.


Assuntos
Micotoxinas , Cromatografia Líquida , Espectrometria de Massas em Tandem , Eletroforese Capilar
SELEÇÃO DE REFERÊNCIAS
DETALHE DA PESQUISA
...