Your browser doesn't support javascript.
loading
Mostrar: 20 | 50 | 100
Resultados 1 - 20 de 313
Filtrar
1.
Pflugers Arch ; 476(8): 1263-1277, 2024 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-38963545

RESUMO

6-Cyanodopamine is a novel catecholamine released from rabbit isolated heart. However, it is not known whether this catecholamine presents any biological activity. Here, it was evaluated whether 6-cyanodopamine (6-CYD) is released from rat vas deferens and its effect on this tissue contractility. Basal release of 6-CYD, 6-nitrodopamine (6-ND), 6-bromodopamine, 6-nitrodopa, and 6-nitroadrenaline from vas deferens were quantified by LC-MS/MS. Electric-field stimulation (EFS) and concentration-response curves to noradrenaline, adrenaline, and dopamine of the rat isolated epididymal vas deferens (RIEVD) were performed in the absence and presence of 6-CYD and /or 6-ND. Expression of tyrosine hydroxylase was assessed by immunohistochemistry. The rat isolated vas deferens released significant amounts of both 6-CYD and 6-ND. The voltage-gated sodium channel blocker tetrodotoxin had no effect on the release of 6-CYD, but it virtually abolished 6-ND release. 6-CYD alone exhibited a negligible RIEVD contractile activity; however, at 10 nM, 6-CYD significantly potentiated the noradrenaline- and EFS-induced RIEVD contractions, whereas at 10 and 100 nM, it also significantly potentiated the adrenaline- and dopamine-induced contractions. The potentiation of noradrenaline- and adrenaline-induced contractions by 6-CYD was unaffected by tetrodotoxin. Co-incubation of 6-CYD (100 pM) with 6-ND (10 pM) caused a significant leftward shift and increased the maximal contractile responses to noradrenaline, even in the presence of tetrodotoxin. Immunohistochemistry revealed the presence of tyrosine hydroxylase in both epithelial cell cytoplasm of the mucosae and nerve fibers of RIEVD. The identification of epithelium-derived 6-CYD and its remarkable synergism with catecholamines indicate that epithelial cells may regulate vas deferens smooth muscle contractility.


Assuntos
Dopamina , Contração Muscular , Ducto Deferente , Masculino , Animais , Ducto Deferente/efeitos dos fármacos , Ducto Deferente/metabolismo , Ducto Deferente/fisiologia , Contração Muscular/efeitos dos fármacos , Ratos , Dopamina/metabolismo , Dopamina/farmacologia , Ratos Wistar , Norepinefrina/farmacologia , Norepinefrina/metabolismo , Músculo Liso/efeitos dos fármacos , Músculo Liso/metabolismo , Músculo Liso/fisiologia , Estimulação Elétrica , Epinefrina/farmacologia , Tirosina 3-Mono-Oxigenase/metabolismo
2.
Rev. Baiana Saúde Pública (Online) ; 47(4): 238-254, 20240131.
Artigo em Inglês | LILACS-Express | LILACS | ID: biblio-1537823

RESUMO

Species of Pithecellobium (Fabaceae) are used in traditional medicine to treat diabetes, cough, bronchitis, and inflammation. This study aims to evaluate the content and determine the antioxidant activity, phenolic compounds content, and cytotoxicity of the extract and the fractions of Pithecellobium diversifolium. This is unprecedented research with an exotic species from the Caatinga, northeastern Brazil, using High-performance Liquid Chromatography-Electrospray Ionization-Mass Spectrometry (HPLC-ESI-MS). The MeOH fractions of leaves and stem barks showed a high content of flavonoids (198.1 ± 106.50 and 542.7 ± 2.52 mg EqQ/g). The CH2Cl2 fraction of peels showed a high content of total phenolic compounds (516.7 ± 3.00 mg EqAG /g). The DPPH test showed that the CH2Cl2 fraction (leaves) held an EC50 of 0.08 ± 0.02, a higher value than that observed for the standards used in the test­Butylated hydroxyanisole (BHA), Butylated hydroxytoluene (BHT), and ascorbic acid. The AcOEt and MeOH fractions of peels presented moderate cytotoxicity with values below 500 µg/mL. The MeOH fraction of leaves showed seven major compounds: myricetin, quercetin, quercetin-arabinofuranoside, apigenin-triglycosides, and apigenin-diglucoside, being the last three unpublished in studies involving the genus. The tests conducted in this study show the potential of P. diversifolium as a promising source of biomolecules with therapeutic applicability.


Espécies de Pithecellobium (Fabaceae) são usadas na medicina tradicional para tratar diabetes, tosse, bronquite e inflamação. Este estudo teve como objetivo avaliar o teor e determinar a atividade antioxidante, o teor de compostos fenólicos e a citotoxicidade do extrato e das frações de Pithecellobium diversifolium, uma pesquisa inédita com uma espécie exótica da Caatinga do Nordeste do Brasil, utilizando a instrumentação Clae-IES. As frações MeOH das folhas e cascas do caule apresentaram alto teor de flavonoides (198,1 ± 106,50 e 542,7 ± 2,52 mg EqQ/g). A fração CH2Cl2 das cascas apresentou um elevado teor de compostos fenólicos totais (516,7 ± 3,00 mg EqAG/g). O teste DPPH mostrou que a fração CH2Cl2 (folhas) apresentou um EC50 de 0,08 ± 0,02, valor superior ao observado para os padrões utilizados no teste ­ Butil hidroxianisol (BHA), Butil hidroxitolueno (BHT) e ácido ascórbico. As frações AcOEt e MeOH das cascas apresentaram citotoxicidade moderada com valores inferiores a 500 µg/mL. A fração MeOH das folhas apresentou sete compostos majoritários: miricetina, quercetina, quercetina-arabinofuranosídeo, apigenina-triglicosídeos e apigenina-diglucosídeo, sendo os três últimos inéditos em estudos envolvendo o gênero. Os testes realizados demonstram o potencial de P. diversifolium, uma promissora fonte de biomoléculas com aplicabilidade terapêutica.


Las especies de Pithecellobium (Fabaceae) se utilizan en la medicina tradicional para tratar diabetes, tos, bronquitis e inflamación. Este estudio tuvo como objetivo evaluar el contenido y determinar la actividad antioxidante, el contenido de compuestos fenólicos y la citotoxicidad del extracto y de las fracciones de Pithecellobium diversifolium, un estudio inédito con una especie exótica de la Caatinga de la región Nordeste de Brasil, que utilizó la instrumentación HPLC-ESI. Las fracciones MeOH de hojas y cortezas de tallo mostraron un alto contenido de flavonoides (198,1 ± 106,50 y 542,7 ± 2,52 mg EqQ/g). La fracción CH2Cl2 de las cortezas presentó un alto contenido de compuestos fenólicos totales (516,7 ± 3,00 mg EqAG/g). El ensayo DPPH mostró que la fracción CH2Cl2 (hojas) tenía EC50 de 0,08 ± 0,02, valor superior a lo observado para los estándares utilizados en el ensayo ­Butilhidroxianisol (BHA), butilhidroxitolueno (BHT) y ácido ascórbico. Las fracciones AcOEt y MeOH de las cortezas presentaron una citotoxicidad moderada con valores inferiores a 500 µ g/mL. La fracción MeOH de las hojas contiene siete compuestos principales: miricetina, quercetina, quercetina-arabinofuranosido, apigenina-triglucósidos y apigenina-diglucósido, de los cuales los tres últimos son inéditos en estudios sobre el género. Las pruebas realizadas demuestran el potencial de P. diversifolium, una fuente prometedora de biomoléculas con aplicabilidad terapéutica.

3.
Braz. J. Pharm. Sci. (Online) ; 60: e23493, 2024. tab, graf
Artigo em Inglês | LILACS | ID: biblio-1533989

RESUMO

Abstract A novel, simple and sensitive high-performance liquid chromatography with fluorescence detection method was developed and validated for the characterization of the preclinical pharmacokinetics of melatonin under pregnant conditions. Plasma samples (25 µL) were treated with 30 µL of ethanol absolute (containing the internal standard, IS). After a centrifugation process, aliquots of supernant (5 µL) were injected into the chromatographic system. Compounds were eluted on a Xbridge C18 (150 mm x 4.6 mm i.d., 5 µm particle size) maintained at 30°C. The mobile phase consisted in a mixture of aqueous solution of 0.4% phosphoric acid and acetonitrile (70:30 v/v). The wavelengths were set at 305 nm (excitation) and 408 nm (emission) and the total analysis time was 8 min/sample. All validation tests were obtained with accuracy and precision, according to FDA guidelines, over the concentration range of 0.005-20 µg/mL. Pharmacokinetic study showed that melatonin systemic exposure increased from day 14, with a significant difference at 19 days of gestation compared to the control group. Our findings suggest a decreased metabolism of melatonin as result of temporary physiological changes that occur throughout pregnancy. However, other maternal physiological changes cannot be ruled out.


Assuntos
Animais , Feminino , Ratos , Plasma , Cromatografia Líquida de Alta Pressão/métodos , Melatonina/agonistas , Gravidez , Farmacocinética
4.
Artigo em Inglês | MEDLINE | ID: mdl-37534825

RESUMO

Sulfite auto-oxidation catalyzed by cobalt complexed with ammonia deposited on silica (CoNSi) was used to generate sulfate radicals. The material was characterized by ATR-FTIR, suggesting that the silica structure did not change, and SEM-EDS, indicating an uniform dispersion of cobalt across the material surface according with XRD results. BET analysis provided information on a mesoporous material (type IV isotherm) with regular morphology (H1 hysteresis). The DSC analysis showed that CoNSi is thermally stable under the studied conditions. Quantitative analysis of Fipronil (FIP) was performed by HPLC-DAD, where the applied method was selective and linear. The Box-Behnken experimental design (BBD) method was used to define the best condition for removing the analyte in water. It was found that in 60 min, 76% removal of 1.8 mg L-1 of FIP was reached by adding 0.30 g of the material and 0.30 g of the sulfite in a solution under stirring, aeration, pH 8.0, and room temperature and protected from radiation. However, analysis of cobalt leaching into the solution by FAAS showed a small amount of the metal (0.44 mg L-1) informing that the synthesis of the material must be improved.

5.
Toxicon X ; 18: 100151, 2023 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-36873112

RESUMO

Venoms from tarantulas contain low molecular weight vasodilatory compounds whose biological action is conceived as part of the envenomation strategy due to its propagative effects. However, some properties of venom-induced vasodilation do not match those described by such compounds, suggesting that other toxins may cooperate with these ones to produce the observed biological effect. Owing to the distribution and function of voltage-gated ion channels in blood vessels, disulfide-rich peptides isolated from venoms of tarantulas could be conceived into potential vasodilatory compounds. However, only two peptides isolated from spider venoms have been investigated so far. This study describes for the first time a subfraction containing inhibitor cystine knot peptides, PrFr-I, obtained from the venom of the tarantula Poecilotheria regalis. This subfraction induced sustained vasodilation in rat aortic rings independent of vascular endothelium and endothelial ion channels. Furthermore, PrFr-I decreased calcium-induced contraction of rat aortic segments and reduced extracellular calcium influx to chromaffin cells by the blockade of L-type voltage-gated calcium channels. This mechanism was unrelated to the activation of potassium channels from vascular smooth muscle, since vasodilation was not affected in the presence of TEA, and PrFr-I did not modify the conductance of the voltage-gated potassium channel Kv10.1. This work proposes a new envenomating function of peptides from venoms of tarantulas, and establishes a new mechanism for venom-induced vasodilation.

6.
Talanta ; 259: 124481, 2023 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-36989967

RESUMO

The concept of Analytical Quality by Design (AQbD) comes as a more robust, economical, and scientifically based alternative for analytical development, to the detriment of OFAT (one factor at a time). This new understanding applicable to analytical development is recommended since regulatory flexibility can be achieved and ensure more reliable results throughout the life of the product. This new approach was applied to develop an analytical procedure indicative of stability for a pharmaceutical product of association of Losartan Potassium and Hydrochlorothiazide, considered a potential first line for the treatment of hypertension. The first stage of the analytical development consisted of defining analytical target profile (ATP), follow by a bibliographic survey of the physicochemical properties of the molecules in question to define an initial method. After defining the initial analytical conditions, statistical tools for design of experiments (DoE) were used for the screening and optimization steps. In the screening stage, the Plackett-Burman design was chosen, using 11 factors and 2 levels, through which it was possible to evaluate numerous variables and determine their significance in relation to the responses. Next, optimization was carried out with the experimental design of a central composite with 4 factors and 5 levels, which allowed modeling a complex response surface and evaluating the phenomena of interactions between the factors. Thus, the optimized analytical conditions were defined, considering a 0.3% formic acid gradient as eluent A and a mixture of acetonitrile and methanol (80:20) as eluent B, X-Bridge C18 chromatographic column (150 mm × 4 .6 mm × 3.5 µm), column temperature of 40°C, flow rate of 1.3 mL/min, injection volume of 10 µL. Through this methodology, it was possible to identify an unknown degradation product of Hydrochlorothiazide, formed by the reaction with lactose (excipient present in the drug formulation), proving that the method can be applicable both to DAD detectors and to spectrometry and mass detectors. It was also proven through the forced degradation study that the method is indicative of stability, in addition to being validated and robust for its purpose.


Assuntos
Hidroclorotiazida , Losartan , Cromatografia Líquida/métodos , Cromatografia Líquida de Alta Pressão/métodos , Incerteza , Espectrometria de Massas em Tandem/métodos , Reprodutibilidade dos Testes
7.
Environ Sci Pollut Res Int ; 30(14): 41014-41027, 2023 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-36626055

RESUMO

In this work, the photolysis of the antibiotic norfloxacin (NOR) and the formation of its photodegradation products were studied using UV and solar radiation. Their extraction was also assessed in Milli-Q water and secondary effluents from a wastewater treatment plant. The photolysis of NOR was chromatographically monitored. The structure of each degradation product is related to the reaction of NOR with reactive oxygen species (ROS), as confirmed using radical quenchers and mass spectrometry. Additionally, the feasibility of extracting NOR and its degradation products was assessed using a commercial solid phase extraction system. Photolysis results showed the formation of five degradation products, generated under exposure to both types of radiation. The decays in NOR concentrations for the solar and UV treatments were adjusted to pseudo first-order kinetics with apparent constant values of ksolar = 1.19 × 10-3 s-1 and kUV = 3.84 × 10-5 s-1. Furthermore, the superoxide radical was the main participant species in the formation of the degradation products P3, P4, and P5. Species P1 and P2 do not need this radical for their formation. The presence of NOR in water opens the possibility of its photolysis by solar radiation. This work contributes to the understanding of the mechanisms that mediate its photodegradation, in addition to studying potential options for its determination and its photodegradation products in the sample treatment.


Assuntos
Antibacterianos , Poluentes Químicos da Água , Humanos , Antibacterianos/química , Norfloxacino/análise , Fotólise , Luz Solar , Cinética , Água/química , Poluentes Químicos da Água/análise , Raios Ultravioleta
8.
Environ Monit Assess ; 195(2): 271, 2023 Jan 06.
Artigo em Inglês | MEDLINE | ID: mdl-36607457

RESUMO

Concerning water resources, several ordinances and legislation determine standards and conditions for the discharge of effluents into water bodies. However, several contaminants are not covered by these guidelines due to little knowledge of their long-term effects and because they are found in low concentrations. These contaminants are called emergent and this category includes drugs, such as anti-inflammatory drugs. The electrocoagulation process associated with advanced oxidation comes up as an alternative to conventional effluent treatment processes, and the objective of this study was to evaluate this process using scrap iron as sacrificial electrodes in the treatment of synthetic effluents containing ibuprofen. High-performance liquid chromatography was used to quantify the drug in synthetic effluents. The Central Rotational Composite Design 24 was used in an experimental design, considering independent variables the concentration of contaminants, applied current, the concentration of the primary oxidizing agent H2O2, and the reaction time. The optimized conditions determined by statistical analysis were drug concentration of 5 mg L-1, H2O2 concentration of 200 mg L-1, current of 5 A, and 150 min. The removals obtained under these conditions were higher than 92% in the aqueous phase, showing that electrocoagulation peroxidation technique has the potential to treat contaminants such as drugs present in effluents and waters.


Assuntos
Eliminação de Resíduos Líquidos , Poluentes Químicos da Água , Eliminação de Resíduos Líquidos/métodos , Ibuprofeno , Peróxido de Hidrogênio/análise , Monitoramento Ambiental , Eletrocoagulação/métodos , Eletrodos , Poluentes Químicos da Água/análise
9.
Food Chem ; 405(Pt B): 134853, 2023 Mar 30.
Artigo em Inglês | MEDLINE | ID: mdl-36435108

RESUMO

Chocolate is widely consumed worldwide and its market grows every year, with emerging demands for new high-quality products. However, this product is susceptible to contamination with polycyclic aromatic hydrocarbons (PAHs), representing a risk for humans. In this study, a methodology for the evaluation of benzo[a]pyrene, benzo[a]anthracene, benzo[b]fluoranthene and chrysene in chocolate by high performance liquid chromatography was validated. The occurrence, dietary exposure, and health risks of 4 PAHs in 38 commercial chocolate samples was investigated. The methodology demonstrated adequate accuracy and precision, with recovery (95.25 %-108.12 %) and relative standard deviation (0.14 %-5.83 %). Benzo[a]pyrene and the ∑4 PAHs concentrations varied between 1.09 and 10.42 µg/kg and 8.38-41.58 µg/kg, respectively. The results of risk assessment suggest low potential health risk for chocolate consumers, considering the margin of exposure (MOE) and the incremental life cancer risk (ILCR) values.


Assuntos
Cacau , Chocolate , Hidrocarbonetos Policíclicos Aromáticos , Humanos , Benzo(a)pireno , Brasil
10.
Sci. agric ; 80: e20220093, 2023. tab, graf
Artigo em Inglês | VETINDEX | ID: biblio-1434393

RESUMO

This study aimed to determine the efficacy of a finishing diet added with sugar beet pulp to reduce backfat skatole of entire male pigs, using the optimised high-performance liquid chromatographic (HPLC) method. The study comprised 72 males Pietrain (Large White × Landrace), divided into two groups of 36 animals each. Pigs in group A (treatment) were fed a supplemented formula (addition of 10 % beet pulp). while animals in group B (control) received a commercial feed, both for a period of 14 days before slaughter. The isocratic HPLC method achieved the chromatographic separation of indolic compounds in approximately 3 min. Skatole was significantly lower ( p = 0.002) in group A, showing that beet root supplementation reduced skatole levels in pig fat. In addition, the optimised HPLC method was reliable, less time-consuming, and showed a resolution suitable for small amounts of skatole.(AU)


Assuntos
Animais , Masculino , Suínos/fisiologia , Cromatografia Líquida de Alta Pressão/veterinária , Escatol/análogos & derivados , Beta vulgaris
11.
Braz. J. Pharm. Sci. (Online) ; 59: e22106, 2023. tab, graf
Artigo em Inglês | LILACS | ID: biblio-1439518

RESUMO

Abstract Guarana (Paullinia cupana) is a native plant from the Amazon whose seeds contain a high concentration of caffeine. Aqueous extract of guarana is widely used in the world. In this study, the objective was to develop and validate a High-Performance Liquid Chromatography method for the determination of caffeine in extracts and commercial beverages based on guarana. A sensitive, simple, and viable high performance liquid chromatographic method without the need of an analyte extraction procedure was developed and validated according to Brazilian and international requirements. The method presented high performance, fulfilling Brazilian and international requirements, in addition to allowing product compliance tests. Results confirmed high selectivity and linearity (>0.999) between 5 to 135 ug/mL, with no significant matrix effect. Detection and quantification limits were 0.02 µg/mL and 2 µg/mL, respectively. Precision was less than 4 %, and accuracy varied from 99.9-120 %. Applicability of the method was demonstrated by conducting a limited evaluation in products containing caffeine. Commercial extracts showed quite different caffeine levels, while carbonated drinks follow Brazilian and American recommendations. Our results indicate that the developed method can be used to evaluate the quality of the guarana extract and of products containing caffeine


Assuntos
Sementes/classificação , Cafeína/agonistas , Extratos Vegetais/análise , Cromatografia Líquida de Alta Pressão/métodos , Paullinia/efeitos adversos , Plantas/classificação , Bebidas/classificação , Gestão da Qualidade Total/normas
12.
Braz. J. Pharm. Sci. (Online) ; 59: e21972, 2023. tab, graf
Artigo em Inglês | LILACS | ID: biblio-1439532

RESUMO

Abstract Brazilian green propolis has been widely used in food and pharmaceutical products due to its valuable source of phenolic compounds and versatile biological activities. The development and validation of analytical methods are extremely useful for the characterization and quality control of products containing propolis. Therefore, the aim of this study was to optimize, validate and investigate the applicability of a reversed-phase HPLC method for analysis of different types of Brazilian green propolis extracts (glycolic and ethanolic). The method showed to be selective for the propolis phenolic markers. The analysis of variance and residues demonstrated that the method had significant linear regression, without lack of fit. It was also a precise, accurate and robust method, which was of utmost importance to analyze both glycolic and ethanolic extracts and at different concentrations. Moreover, as these products can display most complex matrices to analyze, a valid HPLC method can also prove to be specific and versatile.


Assuntos
Própole/análise , Cromatografia Líquida de Alta Pressão/métodos , Preparações Farmacêuticas/administração & dosagem , Compostos Fitoquímicos/análise , Alimentos/classificação
13.
Braz. J. Pharm. Sci. (Online) ; 59: e21626, 2023. tab, graf
Artigo em Inglês | LILACS | ID: biblio-1429969

RESUMO

Abstract n our study, we aimed to validate a method based on liquid chromatography-mass spectrometry (LC-MS) to quantify spironolactone (SPI) and its active metabolite canrenone (CAN) simultaneously in plasma samples to support in vivo experiments. Compounds were separated by using a C18 column with the isocratic elution of a mobile phase composed of 0.1% (v/v) formic acid in methanol-water (60:40 v/v) at a flow rate of 0.4 mL min−1. SPI and CAN were detected in na electrospray interface operating in a positive ionization mode and quantified using the selective ion mode monitoring of mass-charge ratios (m/z) of 439.0 for SPI and 363.1 for CAN. After calculating the matrix effect using theoretical equations, we observed the strong interference of plasma in the equipment-generated signal, which required creating analytical curves using the matrix as a solvent. The method was nevertheless linear (r 2 > 0.999) in a concentration range of 0.4-5.0 µg mL−1, as well as precise, with a coefficient of variation less than 5%. SPI's and CAN's recovery rates from the plasma ranged from 87.4% to 112.1%, while their limits of detection (i.e., 0.07 µg mL−1 and 0.03 µg mL−1, respectively) and quantification (i.e., 0.20 µg mL−1 and 0.08 µg mL−1, respectively) in the presence of plasma contaminants were low. Therefore, the bioanalytical method seems to be feasible for quantifying SPI and CAN in plasma


Assuntos
Plasma , Espectrometria de Massas/métodos , Espironolactona/análise , Canrenona/análise , Cromatografia Líquida/métodos , Farmacocinética , Antagonistas de Androgênios/efeitos adversos
14.
Methods Mol Biol ; 2522: 331-343, 2022.
Artigo em Inglês | MEDLINE | ID: mdl-36125760

RESUMO

Carotenoids are bioactive molecules known to promote human health. Many extreme halophilic archaea synthesize carotenoids, mainly represented by C50 bacterioruberin (BR) and its derivatives. BR has a potent antioxidant capacity, even higher than that of ß-carotene, thus, there is an increasing interest to advance the study of its biological properties as well as to extend its current applications. Here, we describe a procedure to extract and characterize carotenoids (enriched in BR) from haloarchaea using a "hyperpigmented" genetically modified strain of Haloferax volcanii.


Assuntos
Antioxidantes , Haloferax volcanii , Carotenoides , Humanos , beta Caroteno
15.
J Chromatogr A ; 1679: 463397, 2022 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-35973336

RESUMO

A simple, sensitive and reproducible solid-phase extraction method using plastic cartridges containing a monolithic sorbent (m-SPE), coupled to reverse phase liquid chromatography analysis, aiming to determine fifteen polycyclic aromatic hydrocarbons in surface water samples, was developed. The sorbent was easily prepared through a thermal polymerization reaction by using a mixture of n-butyl methacrylate as non-polar monomer and ethylene glycol dimethacrylate as crosslinker contained in a typical Polypropylene syringe cartridge. The effect of different parameters (type of hydrophobic monomer, elution solvent, sample volume, sorbent amount and sorbent load capacity) on the extraction efficiency was optimized. The optimal conditions were achieved by using n-butyl methacrylate as monomer, tetrahydrofurane (THF) as solvent for sorbent cleaning, THF:acetone (1:1) as elution solvent, 25.00 mL of sample volume, 600 µL of the polymerization mixture and 60 µg L-1 as sample loading capacity. Finally, the sorbent charge capacity, the reusability of the cartridges and the extraction efficiency of the m-SPE monolith, as compared with a typical C8 cartridge, were evaluated. Under the optimized experimental conditions, enrichment factors were between 76 and 103, relative recovery factors from 78 to 103%, accuracy values in the range of 58 to 98%, and inter-batch reproducibility values from between 2 and 10%, were obtained. The limits of detection and quantification were obtained by two different procedures: the signal to noise (S/N) ratios (3 and 10, respectively) and the IUPAC convention. The lowest LOD and LOQ values, obtained with the S/N ratios, were between 0.02 and 1.00 µg L-1, respectively whereas with the IUPAC convention the values were between 0.07 and 5 µg L-1. Using this procedure, several PAHs could be detected in the surface water sample taken from a river stream located in La Plata city (Buenos Aires Province, Argentina).


Assuntos
Hidrocarbonetos Policíclicos Aromáticos , Poluentes Químicos da Água , Cromatografia Líquida de Alta Pressão , Limite de Detecção , Polímeros , Reprodutibilidade dos Testes , Extração em Fase Sólida , Solventes , Água
16.
J Tradit Complement Med ; 12(2): 115-122, 2022 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-35528470

RESUMO

Background and aim: This study investigated the effect of Kava extract (Piper methysticum), a medicinal plant that has been worldly used by its anxiolytic effects, on monoamine oxidase (MAO) activity of mice brain after 21 days of treatment as well as anxiolytic and locomotor behavior. Furthermore, the in vitro inhibitory profile of Kava extract on MAO-B activity of mouse brain was evaluated. Experimental procedure: Mice were treated with Kava extract (10, 40, 100 and 400 mg/kg) for 21 days by gavage. After behavioral analysis (plus maze test and open field), MAO activity in different mouse brain structures (cortex, hippocampus, region containing the substantia nigra and striatum) were performed. MAO-B inhibitory profile was characterized in vitro. Results: The treatment with Kava extract (40 mg/kg) increased the percentage of entries of mice into the open arms. Ex vivo analysis showed an inhibition on MAO-B activity caused by Kava extract in cortex (10 mg/kg) and in the region containing the substantia nigra (10 and 100 mg/kg). In vitro, Kava extract also reversibly inhibited MAO-B activity with IC50 = 14.62 µg/mL and, increased Km values at the concentrations of 10 and 30 µg/mL and decreased Vmax value at 100 µg/mL. Conclusion: Kava extract showed different effects on MAO-B isoform depending on the brain structure evaluated. Therefore, the use of Kava extract could be promissory in pathologies where MAO-B is the pharmacological target.

17.
J Tradit Complement Med ; 12(2): 123-130, 2022 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-35528477

RESUMO

BACKGROUND AND AIM: Echinodorus macrophyllus (Kunth.) Micheli is popularly used for acute and chronic inflammatory conditions. The anti-inflammatory activity was previously demonstrated for its flavonoid-enriched fractions. The aim of this work assessed the antinociceptive properties of both aqueous extract and its fractions. EXPERIMENTAL PROCEDURE: The antinociceptive activity was determined by acetic acid-induced writhing, formalin test, tail immersion test, hot-plate test, xylene-induced ear edema methods, and the evaluation of its mechanism was performed in the writhing model. The aqueous extract of Echinodorus macrophyllus (AEEm) was fractionated, yielding Fr20, and Fr40. Fr40 composition was determined by HPLC-DAD-ESI-MS. RESULTS AND CONCLUSION: Fr20 (all doses) and Fr40 (100 mg/kg) reduced the nociception in the tail-flick model. Both fractions increased the percentage of maximum possible effect with 25 mg/kg, in the hot-plate assay, at 60 min, while AEEm reduced pain only with 50 and 100 mg/kg. There was a reduction in xylene-edema index, with Fr40 (25 mg/kg), AEEm (50 mg/kg) and Fr20 (50 mg/kg). All doses of AEEm, Fr20, and Fr40 reduced both phases of the formalin model. In the abdominal contortion model, Fr40 presented the highest activity, reducing 96% of contortions and its antinociceptive mechanism was evaluated. The results indicated the involvement of NO and adrenergic activation pathways. The main components of Fr40 are swertisin, swertiajaponin, isoorientin 7,3'-dimethyl ether, swertisin-O-rhamnoside, isoorientin, isovitexin, isovitexin-Orhamnoside, and isovitexin-7-O-glucoside. The aqueous extract of E. macrophyllus leaves and its fractions exhibited significant analgesic effect, mediated through both peripheral and central mechanisms being considered a potentially antinociceptive drug.

18.
Electrophoresis ; 43(15): 1617-1625, 2022 08.
Artigo em Inglês | MEDLINE | ID: mdl-35507637

RESUMO

The incidence of thrombotic complications in SARS-CoV-2 infections has become a global concern; thus, anticoagulants are an integral part of the treatment. Edoxaban (EDX) is an oral anticoagulant suitable for pharmacologic thromboprophylaxis. Herein, two novel analytical methods for EDX determination in tablets are developed and validated using capillary zone electrophoresis (CZE) and high-performance liquid chromatography (HPLC). Operating conditions such as the electrolyte's concentration and pH value, injection time, volume, and the capillary temperature, were optimized. The methods were successfully validated by establishing the linearity, intra- and inter-day precisions (relative standard deviation [%]), accuracy, and robustness. Adequate separation of excipients and degradation products of EDX generated by stress degradation conditions demonstrated the stability-indicating capability of the methods. The analytical procedures were linear in the range of 25-125 µg/ml (r > 0.999), with the limits of detection and quantification of 3.26 and 10.87 µg/ml for CZE and 0.740 and 2.78 µg/ml for HPLC. Although both methodologies are suitable for determining EDX in tablets, CZE provides a greener alternative due to low-cost analysis using less organic solvents and minimizing waste generation.


Assuntos
COVID-19 , Tromboembolia Venosa , Anticoagulantes , Cromatografia Líquida de Alta Pressão/métodos , Eletroforese Capilar/métodos , Humanos , Piridinas , Reprodutibilidade dos Testes , SARS-CoV-2 , Comprimidos , Tiazóis
19.
Food Chem (Oxf) ; 4: 100068, 2022 Jul 30.
Artigo em Inglês | MEDLINE | ID: mdl-35415675

RESUMO

The effect of abiotic factors, such as weather and climate can alter the properties of vegetable oils. In this work, the effects of the refining process and pre-drying of Moringa oleifera Lam. seeds collected in the dry and rainy seasons (seasonality) were evaluated on the characteristics of the extracted oils. The refined and crude dry season oils had lower acidity and moisture content than the dry and raw rainy season oils. Oleic acid (C18:1) showed the highest concentration in the different Moringa oils studied. The results suggest that dry season oils are more suitable for application as feedstocks in the cosmetic, food, medicinal and pharmaceutical industries. Furthermore, refining proved to be efficient in removing free fatty acids and in lightening the oil.

20.
Colloq. Agrar ; 18(2): 70-78, mar.-abr. 2022. tab
Artigo em Inglês | VETINDEX | ID: biblio-1399125

RESUMO

This work aims to evaluate the effect of industrial treatment with different chemicals and also seed sizes on the physiological behavior of sweet corn in addition to evaluating the content of active ingredients of insecticides before and three months after storage. Four lots of a single sweet corn cross hybrid (L1, L2, L3 and L4) and different sieves (S1, S2 and S3) were carried out in two experiments. Experiment 1: industrial seed treatment, T1 = untreated seeds (control), T2 = Maxim Advanced®, T3 = CruiserⓇ 350 FS and T4 = PonchoⓇ. Experiment 2: quantification of the content of active ingredients, commercial products Cruiser® 350 FS and Poncho and the distribution efficiency was measured by HPLC-UV. The results showed that industrial seed treatment with Maxim Advanced®, CruiserⓇ 350 FS and PonchoⓇ can be carried out three months before sowing without damaging sweet corn seeds. HPLC is efficient to quantify the content of active ingredients in sweet corn seeds treated with Cruiser 350 FS and PonchoⓇ. The industrial seed treatment was calibrated for each batch, which is justified by the different amounts of active ingredient between batches and seed sizes.


Este trabalho tem por objetivo avaliar efeito do tratamento industrial com diferentes produtos químicos e também tamanhos de sementes sobre o comportamento fisiológico do milho doce além de avaliar o teor de ingredientes ativos dos inseticidas antes e três meses após o armazenamento. Quatro lotes de um único híbrido cruzado de milho doce (L1, L2, L3 e L4) e diferentes peneiras (S1, S2 e $3) foram realizados dois experimentos. Experimento 1: tratamento industrial de sementes, T1 = sementes não tratadas (controle), T2 = Maxim Advanced®, T3 = Cruiser 350 FS e T4 = Poncho®. Experimento 2: quantificação do teor de princípios ativos, produtos comerciais CruiserⓇ 350 FS e Poncho e a eficiência de distribuição foi medida por HPLC-UV. Os resultados mostraram que o tratamento de sementes industriais com Maxim Advanced®, CruiserⓇ 350 FS e Poncho® pode ser realizado três meses antes da semeadura sem danificar as sementes de milho doce. A HPLC é eficiente para quantificar o conteúdo de ingredientes ativos em sementes de milho doce tratadas com CruiserⓇ 350 FS e Poncho®. O tratamento industrial de sementes foi calibrado para cada lote, o que se justifica pelas diferentes quantidades de ingrediente ativo entre os lotes e os tamanhos das sementes.


Assuntos
Sementes/classificação , Resíduos de Praguicidas/análise , Cromatografia Líquida de Alta Pressão , Zea mays/fisiologia
SELEÇÃO DE REFERÊNCIAS
DETALHE DA PESQUISA