Abstract Myrcia splendens is popularly known as “guamirim-de-folha-miúda”, and its occurrence ranges from Mexico to southern Brazil. The aim of this work was to identify and quantify phenolic compounds in the crude hydroalcoholic (EBH), ethyl acetate (EBAE) and dichloromethane (EBDM) extracts using the HPLC-ESI- MS/MS. In total, 15 compounds, including protocatecuic acid, syringic acid, p-coumaric acid, salicylic acid, isoquercetin, ellagic acid, ferulic acid, umbelliferone, coniferaldehyde, sinapaldehyde, carnosol, gallic acid, syringaldehyde, umbelliferone, coniferaldehyde, myricetin and kaempferol were identified. Ellagic acid was the major compound in all extracts.
Resumo Myrcia splendens é conhecida popularmente por “guamirim-de-folha-miúda”, e sua ocorrência vai desde o México até o sul do Brasil. Poucos estudos sobre sua composição química existem na literatura, sendo assim, este trabalho teve por objetivo identificar e quantificar substâncias fenólicas nos extratos brutos hidroalcoólico (EBH), acetato de etila (EBAE) e diclorometano (EBDM) através da técnica de HPLC-ESI-MS/MS. Ao total, 15 substâncias foram identificadas, incluindo ácido protocatecuico, ácido siríngico, ácido p-cumárico, ácido salicílico, isoquercetina, ácido elágico, ácido ferúlico, umbeliferona, coniferaldeído, sinapaldeído, carnosol, ácido gálico, siringaldeído, coniferaldeído, miricetina e kaempferol. O ácido elágico foi a substância majoritária em todos os extratos.
Extracts of black mulberry leaves present phytochemicals such as phenolic compounds and minerals. These substances have been studied because they show several health benefits. In this work we report the influence of drying temperature, infusion temperature and extraction time by means of factorial design monitoring the total phenolic content (CFT) of aqueous extracts of leaves of Morus nigra L. The concentrations of CFT, flavonoids, flavonols and antioxidant activity of the extracts were determined by spectrophotometry. The identification and quantification of phenolic compounds were performed by LC-ESI-MS / MS. The determination of the mineral concentration in the black mulberry leaves was performed by ICP-MS. The Pareto and surface response graphs suggested that the most efficient extractions occurred for leaves drying at lower temperatures and using higher infusion temperatures, extraction time did not show significant influence. The extracts presented concentration of CFT from 16.96 ± 0.15 to 5.73 ± 0.33 mg GAE g-1. The analyzes by LC-ESI-MS / MS allowed to identify phenolic substances not yet reported in the literature to date. In addition 10 mineral elements were determined in the black mulberry leaves at mg kg-1 concentrations range.
This paper describes the use of a multiple-injection capillary electrophoresis method as a fast strategy to determine the antinitrosating capacity of nine commercial teas through nitrite quantification. The method consists of the injection of the sample followed by the injection of the control solution, employing a fused-silica capillary of 32.0 cm total length (23.5 cm effective length, 50 µm internal diameter) with background electrolyte composed of 4.0 g L-1 β-alanine and 1.5 g L-1 perchloric acid (pH 3.79) and sodium thiocyanate was used as the internal standard. Before the injections the tea samples were maintained by 1 h of incubation, at 37 °C, with sodium nitrite in perchloric acid medium (pH 2.3). In order to avoid nitrite oxidation and nitrate formation, ultra-pure nearly oxygen-free water was used to prepare the solutions. Black tea, green tea and white tea, obtained from Camellia sinensis, showed greater antinitrosating capacity (96, 93 and 89%, respectively).
A simple strategy using an atomic absorption spectrometer (AAS) for the direct determination of molecular compounds is proposed. The determination of caffeine and propranolol employing atomic absorption instrumentation was conducted, monitoring the emission lines of Fe (271.9 nm) and Mg (285.2 nm), respectively, using a quartz cuvette (1.0 cm) positioned in the burner head. Samples or standards were inserted into the cuvette in order to obtain the absorbance measurements. The parameters of merit were evaluated and the limits of detection were 0.46 and 0.56 mg L-1 for caffeine and propranolol, respectively, with a coefficient of determination R2 > 0.999. The methods developed were applied to the determination of caffeine and propranolol in real samples of beverages and pharmaceutical formulations, respectively. To evaluate the accuracy of the proposed methodologies the results obtained by atomic absorption spectrometer were compared with those obtained by molecular absorption spectrophotometry (UV-Vis) and high performance liquid chromatography (HPLC) or capillary electrophoresis (CE).
In this work, a new adsorbent was prepared by microencapsulation of sulfoxine into chitosan microspheres by the spray drying technique. The new adsorbent was characterized by Raman spectroscopy, scanning electron microscopy and microanalysis of energy dispersive X-rays. The Cu(II) adsorption was studied as a function of pH, time and concentration. The optimum pH was found to be 6.0. The kinetic and equilibrium data showed that the adsorption process followed the pseudo second-order kinetic model and the Langmuir isotherm model over the entire concentration range. An increase of 8.0% in the maximum adsorption capacity of the adsorbent (53.8 mg g-1) was observed as compared to chitosan glutaraldehyde cross-linked microspheres.
The aim of this study was to impregnate the chelating agent 3,3-bis-N,N,bis-(carboxymethyl)aminomethyl-o-cresolsulfonephthalein in chitosan and to investigate the adsorption of Cu(II) ions. The chemical modification was confirmed by FTIR spectrometry, thermogravimetric analysis (TGA) and energy dispersive x-ray spectroscopy (EDX). The adsorption studies were carried out with Cu(II) ions in a batch process and were shown to be dependent on pH. The adsorption kinetics was tested using three models: pseudo first-order, pseudo second order and intraparticle diffusion. The experimental kinetics data were best fitted with the pseudo second-order model (R² = 0.999), which provided a rate constant, k2, of 1.21 x 10-3 g mg-1 min-1. The adsorption rate depended on the concentration of Cu(II) ions on the adsorbent surface and on the quantity of Cu(II) ions adsorbed at equilibrium. The Langmuir isotherm model provided the best fit for the equilibrium data in the concentration range investigated, with the maximum adsorption capacity being 81.0 mg of Cu(II) per gram of adsorbent, as obtained from the linear equation of the isotherm. Desorption tests revealed that around 90% of the adsorbed metal was removed, using EDTA solution as the eluent. This result suggests that the polymeric matrix can be reused.