Emerging contaminants (ECs) have been studied extensively because of the various damages they can cause to the environment, especially due to the non-treated domestic effluents, which contaminate the ...water bodies. Therefore, it is important to evaluate alternatives to remove these compounds. The objective of this work was to evaluate the potential of a new biosorbent from chitosan modified with vanillin (CTSV) to remove isoniazid, cortisol, bisphenol A, 17α-ethinylestradiol, and triclosan by competitive adsorption studies. Structural characterization of the biosorbents was performed by Fourier transform infrared spectroscopy, thermogravimetry, Brunauer-Emmett-Teller, zeta potential, scanning electron microscopy, and
1
H nuclear magnetic resonance. The adsorption for ECs were carried out in an aqueous medium, and quantitative analyzes were performed by HPLC. The effect of pH was evaluated in the pH range 5 to 10 and indicated that better results were found in pH 9 and 8 for CTS and CTSV, respectively. The salt concentrations effect was evaluated in 0.0 to 1.0 mol L
−1
and revealed better adsorption conditions in 0.7 mol L
−1
of NaCl. The adsorption kinetics pointed to an equilibrium condition reached quickly (with adjustment of data R
2
> 0.969) with adequacy to pseudo–second-order model for both biosorbents and ECs. The linear isothermal model was suitable for the adsorption isothermal data and distribution constant (
K
D
) showed the highest values for 17α-ethinylestradiol (0.067 L g
−1
) and triclosan (0.197 L g
−1
) in CTSV adsorption. Thus, the results indicated that CTSV performed well in removal for the tested ECs, being an interesting alternative, due to the ease of obtaining and abundance of reagents employed in its preparation.
Graphical abstract
This paper proposes an innovative sub-minute capillary zone electrophoresis method and a simple sample preparation procedure for simultaneous nitrate and nitrite determination. The novelty of the ...method is the simplicity of execution and the capacity to separate the analytes in less than 0.5min. The BGE is composed of 10mmolL−1 perchloric acid and 40mmolL−1 β-alanine at pH 3.96. Thiocyanate was used as an internal standard. The method was validated following the Eurachem guidelines and applied to the analysis of 14 baby food samples. Of these samples, one had nitrate levels above that permitted by Brazilian legislation (250mgkg−1) and for all samples the nitrite concentrations were under the limit of quantification. The good analytical performance verified for this method indicates that it is suitable for implementation in food laboratories for the routine determination of nitrate and nitrite as an alternative to the official method provided by the AOAC.
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•A sub-minute CZE method was developed for the determination of nitrate and nitrite.•The CZE method was applied in the analysis of baby foods.•Sample preparation step was simple and effective to extract the analytes.•Analytical validation was performed according to the Eurachem guidelines.•The CZE method showed good analytical performance to the analysis of baby foods.
•A rapid CZE method for the analysis ofcitrate, phosphate and sulfitewas developed.•The analytes were separated in less than 3.5 min.•Seafood samples were analyzed by the validated CZE ...method.•In-house method validation was performed to confirm the fitness-for-purpose.
Since seafood is susceptible to decomposition, additives may be used to maintain its quality. However, some additives may be improperly used to disguise spoilage, thus resulting in food fraud. Market growth demands faster and more reliable quality control tools that incorporate the most common additives in a single analysis. This study developed a rapid analytical method for the determination of citrate, phosphate and sulfite in seafood by capillary zone electrophoresis with indirect UV–Vis detection. Electrophoretic separation was achieved in less than 3.5 min. The background electrolyte consisted of 20 mmol L−1 of benzenesulfonic acid and 45 mmol L−1 of aminocaproic acid. After validation, the method was applied for 24 seafood real samples. Citrate was found in five samples. Four samples presented higher phosphate and sulfite concentrations than those permitted by Brazilian legislation. Good analytical performance indicates that the method is a viable alternative for food control in routine analysis.
A simple and green sample preparation protocol using dispersive pipette extraction (DPX) followed by identification and quantification by high-performance liquid chromatography (HPLC) is proposed for ...the determination of 11 polyphenols, including phenolic acids and flavonoids, in grape juice. Sample preparation variables by DPX, including extraction phase, sample volume, pH, desorption solvent, salt concentration, time and cycles of extraction and desorption, were evaluated and optimized using univariate and multivariate designs. The analytical performance was satisfactory, with coefficient of determination greater than or equal to 0.9621, precisions with values lower than 20%, and recoveries ranging from 80 to 120%, demonstrating good method trueness. In addition, the method proved to be robust and showed no matrix effect. Finally, the method was applied to determine polyphenols in three grape juice samples. The major compounds determined in the samples were chlorogenic acid (70.84–120.70 mg L
−1
) and gallic acid (69.62–96.08 mg L
−1
). Finally, the green character of this method was evaluated using the tools Green Analytical Procedure Index (GAPI), Analytical Greenness Metric (AGREE), and Analytical Greenness Metric for Sample Preparation (AGREEprep). According to the metrics, an excellent green character was determined, emphasizing the minimization of sample (160 μL) and solvent (200 μL) volumes, as well as the short extraction time (< 5 min).
Graphical Abstract
The juçara palm tree produces a small spherical and black-purple fruit similar to açaí. It is rich in phenolic compounds, especially anthocyanins. A clinical trial evaluated the absorption and ...excretion of the main bioactive compounds in urine and the antioxidant capacity in serum and erythrocytes of 10 healthy subjects after juçara juice intake. Blood samples were collected before (0.0 h) and 0.5 h, 1 h, 2 h, and 4 h after a single dose (400 mL) of juçara juice, while urine was collected at baseline and 0-3 and 3-6 h after juice intake. Seven phenolic acids and conjugated phenolic acids were identified in urine deriving from the degradation of anthocyanins: protocatechuic acid, vanillic acid, vanillic acid glucuronide, hippuric acid, hydroxybenzoic acid, hydroxyphenylacetic acid, and ferulic acid derivative. In addition, kaempferol glucuronide was also found in urine as a metabolite of the parent compound in juçara juice. Juçara juice caused a decrease in the total oxidant status of serum after 0.5 h in comparison to baseline values (
< 0.05) and increased the phenolic acid metabolites excretion. This study shows the relationship between the production of metabolites of juçara juice and the total antioxidant status in human serum, indicating evidence of its antioxidant capacity.
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•SFE and SWE in single or combined mode allow extraction of value-added compounds.•SFE modifies the cell wall, and the oil fraction is rich in fatty acids.•PCA is used to correlate ...phenolic compounds with extraction methods.•Vanillic acid is the major phenolic compound quantified in all extracts.•First report of detection of 29 new phenolic compounds from soursop seed extracts.
Soursop (Annona muricata L.) seeds, which is a residue obtained from juice agro-industries, were subjected to supercritical fluid extraction (SFE) and subcritical water extraction (SWE) in single or combined mode to extract the potential value-added compounds. Different extraction methods were evaluated in terms of the extraction yield, phenolics content, antioxidant activity (DPPH, ABTS, and FRAP), and Maillard reaction products. The extracts were analyzed using SEM, GC-MS, and LC-MS/MS techniques. The temperature and a combination of high-pressure techniques positively affected the overall results (SFE + SWE), affording nonpolar and polar extracts rich in phenolics and antioxidant compounds. SEM analysis showed that the use of SFE caused modifications in the cell wall, and the oil fraction was rich in fatty acids. Twenty-nine compounds associated with soursop seed extracts were detected for the first time using LC-MS/MS, showing the potential of the raw material as well as promoting resource re-utilization in circular economy.
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.
The aim of this study was to develop a simple and rapid method of capillary electrophoresis using a short end multiple injection in free solution to determine simultaneously the biological sample ...volume and analytes concentration. The method consists of a sequence of injection steps with an internal standard as the reference for correction of the volume of sample collected. The procedure was applies in the determination of NO
3
− and SCN in saliva samples. The background electrolyte was composed of 12
mM tris(hydroxymethyl)aminomethane and 8.5
mM sulfuric acid, at pH 2.5. The internal standard used was BrO
3
−. A fused silica capillary (48.5
cm total length, 8.5
cm effective length and 75
μm i.d.) coated with chitosan was used in a short-end injection configuration. Modification of the electroosmotic flow (EOF) using dynamic coating resulted in a controlled and stable EOF, contributing to the rapid separation of anions (0.36
min) in co-electroosmotic mode. The validation of the method for correcting the volume of saliva collected with a swab showed a difference of less than 3.5% compared with the predicted value and a correlation of 0.999. The limits of detection for NO
3
− and SCN
− were 0.13 and 0.23
mg
L
−1, respectively. The inter-day precision of the method determined for both analytes was less than 5% and the recovery ranged between 97 and 102%.
The dataset showed in this manuscript belongs to the investigation of the Southern-Brazilian geopropolis of stingless bees. Stingless bees are native species of insects from tropical areas; they ...produce honey, pollen and geopropolis that is composed of a mix of vegetal extracts, digestive enzymes, and mostly by soil. Used in folk medicine as antiseptic, antioxidant and antimicrobial agent, the composition is due to bee species, climate changes, local flora, and soil type. Moreover, the complex chemical content gives to the geopropolis a bioactive potential, with scavenging characteristics that is important to avoid free radical damages in the human health.
Regarding the importance of exploring new natural matrices sources with bioactive potential, the first approach of chemical characterization of geopropolis is indispensable. Thus, ten samples of Southern-Brazilian geopropolis were analyzed and the bioactive responses obtained were discussed in the accompanying article titled “Southern-Brazilian geopropolis: A potential source of polyphenolic compounds and assessment of mineral composition”. Furthermore, the physicochemical analysis of moisture and ash content, the yield of extraction, the reducing activity and free radical scavenging potential of ethanolic extracts, the antimicrobial activity, and the analysis of HPLC-ESI-MS/MS chromatograms are the main data presented in brief. The data can guide scientists in order to know methods and data for these samples.
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.
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