Luciano Vitali

N-nitrosamines (NAs) have recently been identified as contaminants in various matrices, including processed meat products. These compounds exhibit high carcinogenic potential, raising significant concerns regarding their presence. In this context, the present study proposes the use of solid-phase microextraction (SPME) in the Headspace ( HS ), a technique that offers higher efficiency and a greener profile compared to conventional extraction methods, enabling the achievement of low detection limits when combined with gas chromatography coupled to flame ionization detection (GC/FID). Instrumental parameters were optimized to ensure suitable separation and detection of N-nitrosodiethylamine (NDEA) and N-nitrosodimethylamine (NDMA). The optimization of the HS -SPME parameters revealed that the PDMS/Car/DVB fiber, sample solution at pH 7, ionic strength adjusted to 30% NaCl, extraction temperature of 35 °C, and extraction time of 60 min were optimal conditions. The analytical parameters of the developed method were evaluated, yielding excellent selectivity and limits of detection of 4 and 38 µg kg⁻ ¹ for NDEA and NDMA, respectively. The method exhibited precision with RSDs from 2.6% to 14.4%, with the higher value attributed to the manual nature of the SPME process for NDMA, and accuracy, with recoveries between 92.3% and 111.5%, thereby confirming the effectiveness of the developed method for the determination of NAs. The proposed approach provides an efficient and sustainable alternative to more costly conventional methods. The developed method was applied to two commercial sausage samples purchased from different local markets, and no detectable levels of the evaluated NAs were found. The proposed approach provides an efficient and sustainable alternative to more costly conventional methods. Graphical Abstract

The genus Myrcia from the Myrtaceae family contains species with therapeutic properties, such as reducing glycemia and oxidative stress. This study investigated the effects of the hydroalcoholic extract of Myrcia tijucensis in an animal model of Type 1 diabetes induced by alloxan. The objective was to evaluate its antidiabetic and antioxidant activities, as well as its effects on pancreatic islets. Chromatographic analysis by HPLC–MS/MS revealed, for the first time in the genus Myrcia , the presence of phenolic acids such as vanillic acid, syringic acid, vanillin, p ‐coumaric acid, and salicylic acid. The extract demonstrated potent inhibition of the α‐glucosidase enzyme (IC ₅₀ = 0.17 ± 0.01 mg/mL), suggesting a hypoglycemic mechanism. At the biological level, treatment with the extract significantly reduced oxidative stress, as evidenced by a decrease in thiobarbituric acid reactive substances (TBA‐RS) and normalization of antioxidant enzymes such as superoxide dismutase (SOD) and glutathione peroxidase (GSH‐Px). Additionally, an improvement in the architecture of pancreatic islets was observed, with an increase in islet diameter in treated groups, suggesting potential cellular regeneration. Altogether, the extract of M. tijucensis has proven promising for studies in adjunctive therapy for Type 1 diabetes, helping to control glycemia, reduce oxidative stress, and preserve pancreatic islets.

The aim of this study was to characterize the phytochemical profile and potential antiaging and wound‐healing activities of 70% hydroalcoholic crude extract (CHE) from Myrcia neoobscura leaves and its fractions—insoluble (IF), ethyl acetate (EAF), and aqueous (AF)—for use in phytocosmetics for skin application. CHE and its fractions showed high concentrations of total phenolics, including flavanols and flavonoids. Ten phenolic compounds were identified, with gallic acid as the major, followed by chlorogenic and p ‐coumaric acids. Catechin, isoorientin, taxifolin, resveratrol, naringenin, and eriodictyol were reported for the first time in the genus. CHE and AF showed the best results in antioxidant assays. In antiglycation activity, EAF showed the highest oxidative glycation inhibition, comparable to quercetin. CHE and AF exhibited the strongest collagenase and elastase inhibition. CHE, IF, and EAF showed the highest SPF. CHE promoted 81.86% fibroblast migration in 24 h, indicating strong wound‐healing potential. CHE maintained cellular viability in the MTT assay. In the HET‐CAM assay and agarose overlay assays, CHE and fractions were classified as non to mildly irritating. These results suggest potential antiaging applications, mainly attributed to the phenolic profile.

A new analytical method was developed for the determination of 14 multiclass emerging organic contaminants in surface waters using LC-MS, and Dispersive Liquid–Liquid Microextraction (DLLME) for extraction. Different Natural Deep Eutectic Solvents (NADESs) composed of terpenes and organic acids were tested as extraction solvents and characterized by Fourier Transform Infrared Spectroscopy (FTIR), Hydrogen Nuclear Magnetic Resonance Spectroscopy (¹H-NMR), Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), density, and viscosity, eliminating the need to use traditional chlorinated solvents. NADES produced with butyric acid and thymol showed the best results and was selected for application for the first time in the extraction of emerging organic contaminants of different classes in water samples. Vortex was used as the dispersion mode, eliminating the use of the dispersion solvent. Chromatographic conditions and sample preparation were optimized using multivariate experimental designs. The optimized chromatographic conditions included the column oven temperature, mobile phase modifiers, and stationary phase type. The optimized conditions for sample preparation included the extraction temperature and pH, salting out effect, and extraction solvent volume. The analytical performance was evaluated through repeatability and intermediate precision tests, with RSD values below 20%, and recoveries between 70 and 120%. The coefficient of determination was greater than 0.98 for all analytes. LOQs varied between 1.5 and 35 μg L⁻¹. DLLME is a simple technique, it does not require expensive and specific equipment. Furthermore, replacing traditional chlorinated solvents with NADES makes the procedure more environmentally friendly. The method presented here can be applied to a wide range of analytes for the analysis of fresh, brackish, and salt waters. Up to the present moment, this is the first study using NADES based thymol and butyric acid for the determination of multiclass emerging contaminants in surface waters samples.

This study expands and shows the versatility of applications in hydrophilic interaction chromatography coupled with triple quadrupole mass spectrometry (HILIC-MS/MS) using a FRULIC-N column to determine 31 phenolic compounds in beverage industry residues (coffee, apple juice, beer, and wine). Optimization, via Doehlert design, determined the acetonitrile proportion (50-90%) and pH (3.0-7.0) in the mobile phase (MP). A 22 factorial design assessed the concentration of ammonium acetate (10-110 mmol L-1) in the MP and column temperature (20-60 °C). Injection volume (5-45 µL) was univariately optimized. Separations at 60 °C reduced chromatographic run time to less than 11 min. Gradient elution (500 µL min-1) employed an MP comprising acetonitrile and ammonium acetate (110 mmol L-1, pH 7). Validation demonstrated average coefficient of determination (R2 ) 0.9707, limit of detection 0.001-0.503 mg L-1 and quantification 0.004-1.524 mg L-1, precision < 12.2%, recovery 92.4-110.8%. The method was applied to five residues, indicating its viability for determining phenolics in beverage production residues.

Faced with the global challenge of water treatment, the investigation of the removal of endocrine disruptor compounds (EDCs) in aquatic environments is essential to protect human and animals health. In this study, a novel nanocomposite was prepared from biochar from agricultural waste (corn cob) and maghemite (γ-Fe2O3) nanoparticles, named PCCN, to remove four EDCs (triclosan, 17α-ethinylestradiol, methylparaben, and bisphenol A) from aqueous solutions by adsorption. For the characterization of PCCN, the advanced techniques Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmett-Teller analysis (BET), pH of point of zero charge (pHpzc), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and thermogravimetry (TGA) were employed. Competitive adsorption equilibrium studies of EDCs were performed with PCCN and compared to unmodified biochar (PCC). The pH effect showed that optimal adsorption of EDCs was at pH 8.0 for PCC and pH 6.0 for PCCN. The salt concentration did not influence EDCs in the adsorption. In the adsorption isotherm, the results fitted the Freundlich isotherm model (R2 > 0.903) and the adsorption kinetics were well described by the pseudo-second-order model (R2 > 0.985). Furthermore, the desorption studies indicated that the PCCN can be reused. Thus, the investigation suggests PCCN has promising potential in the removal of EDCs from wastewater.