RESUMO
Abstract Chronic type 2 diabetes mellitus (T2DM) and its associated diseases are major concern among human population and also responsible for significant mortality rate. Hence, the present study aims to evaluate and correlate the invertase inhibition, antioxidant activity and control against DFU causing bacterial pathogens by Pandanus odoratissimus flowers. Two dimensional preparative thin layer chromatography (2D PTLC) was adopted to purify the phenolic acid component and LC-MS2 was done to predict the phenolic acid structures. Standard spectrophotometry methods were adopted to investigate the in vitro invertase inhibitory and antioxidant (CUPRAC and ABTS) activities. Agar well diffusion and broth dilution assays were used to record the antibacterial property against DFU causing pathogens isolated from clinical samples. Statistical analyses were used to validate the experiments. A new and novel diferuloyl glycerate related phenolic acid (m/z 442) purified from PTLC eluate has recorded satisfactory cupric ion reducing power (ED50= 441.4±2.5 µg), moderate ABTS radical scavenging activity (IC50= 450.3±10 µg; 32.5±1.5%), and a near moderate, in vitro, invertase mixed type inhibition (24.5±4.5%; Ki: 400 µg). Similarly, bacterial growth inhibitory kinetics has showed a significant inhibition against E. coli and S. aureus.
Assuntos
Humanos , Masculino , Feminino , Técnicas In Vitro/métodos , Pé Diabético/patologia , Pandanaceae/efeitos adversos , Flores/classificação , beta-Frutofuranosidase/isolamento & purificação , Diabetes Mellitus Tipo 2/patologia , Espectrofotometria/métodos , Cromatografia em Camada Fina/instrumentação , Antioxidantes/efeitos adversosRESUMO
Thin-layer chromatography (TLC) is a classic method for the separation and analysis of complex mixtures. Biological assays, chemical derivatisation and spectroscopy techniques are compatible with TLC and provide extra information about isolated compounds. However, coupling TLC to mass spectrometry is hampered by the difficulty to desorb the analytes from the silica surfaces. In this study, we used a multimodal ion source for laser desorption (LD) and low-temperature plasma (LTP) post-ionisation. Efficient desorption was reached by covering the TLC plates with activated carbon. Regions of interest can be analysed by spots, by lines or by area. We show the separation of methylxanthines from coffee, tea and cocoa preparations by TLC, with subsequent mass spectrometry imaging (MSI). Using a lateral resolution of 400 µm × 400 µm, allowed the acquisition of 21 895 spectra in 2.4 h (2.5 pixels per s). Further, we demonstrate the possibility of direct mass fragmentation studies and quantification. We mounted the system on an Open LabBot with a theoretical lateral resolution of 12.5 µm and performed the visualisation of ions of interest and the pixel-wise review of mass spectra with our free software RmsiGUI (). This non-proprietary and modular platform enables the cost-efficient adaption of the system and further development by the community.
Assuntos
Cromatografia em Camada Fina/instrumentação , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por Matriz/métodos , Xantinas/análise , Cacau/química , Café/química , Temperatura Baixa , Limite de Detecção , Chá/química , Xantinas/isolamento & purificaçãoRESUMO
Echinodorus grandiflorus e Echinodorus macrophyllus, conhecidas como chapéu-de-couro, são empregadas de forma indistinta como anti-inflamatório. O objetivo deste trabalho foi realizar análises físico-químicas de três amostras (A, B e C) de folhas de chapéu-de-couro (E. grandiflorus) provenientes de fornecedores de São Paulo buscando avaliar a qualidade e autenticidade destas amostras considerando a Farmacopéia Brasileira, 5ª edição, como referência. Verificou-se que as amostras estavam de acordo com as especificações farmacopeicas em relação às características organolépticas, material estranho, umidade, cinzas totais, cinzas sulfatadas (exceto amostras A e B) e teores de derivados de ácido o-hidroxicinâmico (exceto amostra A). Na descrição macro e microscópica foram identificadas estruturas características de E. grandiflorus. Após análise dos perfis cromatográficos por cromatografia em camada delgada de sílica (CCDS) constatou-se a presença de ácido caféico, isoorientina e swertiajaponina, conforme a monografia da espécie. A amostra C foi a única droga vegetal aprovada segundo os critérios da Farmacopeia Brasileira, evidenciando-se a necessidade da realização do controle de qualidade de matérias-primas vegetais para garantir a obtenção de fitoterápicos seguros e eficazes.
Echinodorus grandiflorus and Echinodorus macrophyllus, known as "chapéu-de-couro", have been differently used as anti-inflammatory agents. The aim of the present study was to carry out physicochemical analyses of three leaf samples (A, B and C) from "chapéu-de-couro" (E. grandiflorus) obtained from suppliers in São Paulo to assess the quality and the authenticity of these samples according to the Brazilian Pharmacopoeia (BP) 5th edition. All samples were in agreement with the specifications of the Pharmacopoeia considering their organoleptic characteristics, foreign material, humidity, total ash and sulfated ash (except for samples A and B), as well as the levels of o-hydroxycinnamic acid derivatives (except for sample A). Macroscopic and microscopic analysis of the samples revealed structures typical of E. grandiflorus. Analysis of chromatographic profiles by thin-layer chromatography (TLC) on silica gel indicated the presence caffeic acid, isoorientin and swertiajaponin, which are in accordance with the monography for this species. Sample C was the only plant drug approved according to the criteria of the Brazilian Pharmacopoeia, evidencing the need of quality control of raw plant material to ensure the production of safe and effective phytomedicines.
Assuntos
Cromatografia em Camada Fina/instrumentação , Alismataceae/efeitos adversos , Folhas de Planta/químicaRESUMO
Avaliou-se a cromatografia em camada delgada (CCD) como método de diagnóstico toxicológico para os casos de intoxicação por aldicarb em cães e gatos, utilizando-se 50 amostras de conteúdo gástrico obtidas durante a necropsia e 50 amostras de alimentos utilizados como iscas para intoxicar criminalmente os animais. Todas as amostras resultaram positivas para o aldicarb, mostrando ser a CCD uma técnica qualitativa eficiente, rápida e de baixo custo, com uso potencial na toxicologia veterinária forense
The present study concerns about the identification of aldicarb residues using thin-layer chromatography (TLC) in 50 samples of gastric content obtained from the necropsy of dogs and cats and 50 samples of foods suspected of being used as baits. All samples resulted positive for aldicarb showing that the TLC is an efficient, fast and not expensive qualitative method for the detection of aldicarb, being useful for this purpose in the forensic veterinary toxicology
Assuntos
Animais , Gatos , Cães , Aldicarb/intoxicação , Gatos , Cromatografia em Camada Fina/instrumentação , Cromatografia em Camada Fina/métodos , Cromatografia em Camada Fina/veterinária , Cães , Conteúdo GastrointestinalRESUMO
Avaliou-se a cromatografia em camada delgada (CCD) como método de diagnóstico toxicológico para os casos de intoxicação por aldicarb em cães e gatos, utilizando-se 50 amostras de conteúdo gástrico obtidas durante a necropsia e 50 amostras de alimentos utilizados como iscas para intoxicar criminalmente os animais. Todas as amostras resultaram positivas para o aldicarb, mostrando ser a CCD uma técnica qualitativa eficiente, rápida e de baixo custo, com uso potencial na toxicologia veterinária forense(AU)
The present study concerns about the identification of aldicarb residues using thin-layer chromatography (TLC) in 50 samples of gastric content obtained from the necropsy of dogs and cats and 50 samples of foods suspected of being used as baits. All samples resulted positive for aldicarb showing that the TLC is an efficient, fast and not expensive qualitative method for the detection of aldicarb, being useful for this purpose in the forensic veterinary toxicology(AU)