Solidified floating organic drop microextraction (SFODME) for the simultaneous analysis of three non-steroidal anti-inflammatory drugs in aqueous samples by HPLC

In this work, a liquid-liquid microextraction methodology using solidified floating organic drop (SFODME) was combined with liquid chromatography and UV/Vis detection to determine non-steroidal anti-inflammatory drugs (NSAIDs) naproxen (NPX), diclofenac (DCF), and mefenamic acid (MFN) in tap water, surface water, and seawater samples. Parameters that can influence the efficiency of the process were evaluated, such as the type and volume of the extractor and dispersive solvents, effect of pH, agitation type, and ionic strength. The optimized method showed low detection limits (0.09 to 0.25 μg L-1), satisfactory recovery rates (90 to 116%), and enrichment factors in the range between 149 and 199. SFODME showed simplicity, low cost, speed, and high concentration capacity of the analytes under study. Its use in real samples did not demonstrate a matrix effect that would compromise the effectiveness of the method, being possible to apply it successfully in water samples with different characteristics.publishe

Producing magnetic nanocomposites from paper sludge for the adsorptive removal of pharmaceuticals from water: a fractional factorial design

In view of a simple after-use separation, the potentiality of producing magnetic activated carbon (MAC) by intercalation of ferromagnetic metal oxide nanoparticles in the framework of a powder activated carbon (PAC) produced from primary paper sludge was explored in this work. The synthesis conditions to produce cost effective and efficient MACs for the adsorptive removal of pharmaceuticals (amoxicillin, carbamazepine, and diclofenac) from aqueous media were evaluated. For this purpose, a fractional factorial design (FFD) was applied to assess the effect of the most significant variables (Fe3+ to Fe2+ salts ratio, PAC to iron salts ratio, temperature, and pH), on the following responses concerning the resulting MACs: Specific surface area (SBET), saturation magnetization (Ms), and adsorption percentage of amoxicillin, carbamazepine, and diclofenac. The statistical analysis revealed that the PAC to iron salts mass ratio was the main factor affecting the considered responses. A quadratic linear regression model A = f(SBET, Ms) was adjusted to the FFD data, allowing to differentiate four of the eighteen MACs produced. These MACs were distinguished by being easily recovered from aqueous phase using a permanent magnet (Ms of 22-27 emu g-1), and their high SBET (741-795 m2 g-1) were responsible for individual adsorption percentages ranging between 61% and 84% using small MAC doses (35 mg L-1).publishe

Catálogo Taxonômico da Fauna do Brasil: setting the baseline knowledge on the animal diversity in Brazil

The limited temporal completeness and taxonomic accuracy of species lists, made available in a traditional manner in scientific publications, has always represented a problem. These lists are invariably limited to a few taxonomic groups and do not represent up-to-date knowledge of all species and classifications. In this context, the Brazilian megadiverse fauna is no exception, and the Catálogo Taxonômico da Fauna do Brasil (CTFB) (http://fauna.jbrj.gov.br/), made public in 2015, represents a database on biodiversity anchored on a list of valid and expertly recognized scientific names of animals in Brazil. The CTFB is updated in near real time by a team of more than 800 specialists. By January 1, 2024, the CTFB compiled 133,691 nominal species, with 125,138 that were considered valid. Most of the valid species were arthropods (82.3%, with more than 102,000 species) and chordates (7.69%, with over 11,000 species). These taxa were followed by a cluster composed of Mollusca (3,567 species), Platyhelminthes (2,292 species), Annelida (1,833 species), and Nematoda (1,447 species). All remaining groups had less than 1,000 species reported in Brazil, with Cnidaria (831 species), Porifera (628 species), Rotifera (606 species), and Bryozoa (520 species) representing those with more than 500 species. Analysis of the CTFB database can facilitate and direct efforts towards the discovery of new species in Brazil, but it is also fundamental in providing the best available list of valid nominal species to users, including those in science, health, conservation efforts, and any initiative involving animals. The importance of the CTFB is evidenced by the elevated number of citations in the scientific literature in diverse areas of biology, law, anthropology, education, forensic science, and veterinary science, among others

Ultrasound-assisted dispersive liquid-liquid microextraction for determination of enrofloxacin in surface waters

This work describes the development of an HPLC-FLD methodology for the separation of five fluoroquinolones (ciprofloxacin, enrofloxacin, sarafloxacin, norfloxacin and levofloxacin) followed by optimization of the DLLME process for the clean-up and preconcentration of enrofloxacin in samples of seawater and river water. The mobile phase used for the chromatographic separation consisted of methanol: phosphate buffer (NaHPO4 H2O 0.04 M pH 3 with H3PO4 85 %), gradient eluted at a ratio of 20:80 (v:v). The mobile phase flow was maintained at 1.2 mL min-1. For the ultrasonic-assisted dispersive liquid liquid microextraction (UA-DLLME), the following conditions were used: 8 mL of sample with pH adjusted to 8, extraction solvent: 500 μL of chloroform, dispersive solvent: 500 μL of acetonitrile; samples were vortexed and sonicated for 2 minutes, each. The enrichment factor (EF) was 54.7 and the recovery was 70 %, achieving a limit of detection (LOD) of 0.11 μg L-1. Repeatability and intermediate reproducibility presented values of relative standard deviation (RSD) lower than 2 %. Finally, the optimized method was applied to the analysis of water and enrofloxacin was detected in both water samples with a concentration of 0.20 μg L-1 in the river and 0.12 μg L-1 in the seawater. However, recovery tests performed to evaluate the water matrices' effects on the extraction performance, presented recoveries of 72±6.1 for river water and 27±8.3 for seawater. These results demonstrate that hereby developed method is only suitable for water samples with a low salinity content.publishe

Multivariable optimization of activated carbon production from microwave pyrolysis of brewery wastes - Application in the removal of antibiotics from water

This study aimed at optimizing the one-step chemical activation and microwave pyrolysis of an agro-industrial waste to obtain a microporous activated carbon (AC) with superior textural and adsorptive properties by a fast, low-reagent and low-energy process. Spent brewery grains were used as precursor, and the antibiotics sulfamethoxazole (SMX), trimethoprim (TMP) and ciprofloxacin (CIP) were considered as target adsorbates. A fractional factorial design was applied to evaluate the effect of the main factors affecting the preparation of AC (activating agent, activating agent:precursor ratio, pyrolysis temperature and residence time) on relevant responses. Under optimized conditions (K2CO3 activation, pyrolysis at 800 °C during 20 min and a K2CO3:precursor ratio of 1:2), a microporous AC with specific surface area of 1405 m2 g-1 and large adsorption of target antibiotics (82-94%) was obtained and selected for further studies. Equilibrium times up to 60 min and maximum Langmuir adsorption capacities of 859 µmol g-1 (SMX), 790 µmol g-1 (TMP) and 621 µmol g-1 (CIP) were obtained. The excellent textural and adsorptive properties of the selected material were achieved with a very fast pyrolysis and low load of activating agent, highlighting the importance of optimization studies to decrease the environmental and economic impact of waste-based AC.This work was developed within the scope of the project CICECO - Aveiro Institute of Materials (UIDB/50011/2020 & UIDP/50011/2020). We acknowledge financial support to CESAM by FCT/MCTES (UIDP/50017/2020+UIDB/50017/2020+LA/P/0094/2020), through national funds. Érika M.L. Sousa thanks to Fundação para a Ciência e Tecnologia (FCT) for her PhD grant (2020.05390. BD). Paula Ferreira is thankful to FCT for the Investigator Program (IF/00300/2015). María V. Gil acknowledges support from a Ramón y Cajal grant (RYC-2017-21937) of the Spanish government and the Spanish State Research Agency, co-financed by the European Social Fund (ESF).Peer reviewe

Determination of three estrogens in environmental water samples using dispersive liquid-liquid microextraction by high-performance liquid chromatography and fluorescence detector

In this work the dispersive liquid-liquid microextraction technique (DLLME) is presented as an important alternative to the classical extraction methods and was used to extract and concentrate before estrogen quantification by HPLC in environmental water samples. For the evaluation of the analytical methodology, the following conditions were used: sample volume: 8 mL; extraction solvent: 200 μL of chlorobenzene; dispersive solvent: 2000 μL of acetone. The enrichment factor (EF) was 140 for Estrone, 202 for 17β-estradiol (E2) and 199 for 17α-ethinylestradiol (EE2). Limit of detection was 20 ng L-1 for E1, 3.1 ng L-1 for E2, 2.7 ng L-1 for EE2. Repeatability and intermediate reproducibility presented values of relative standard deviation lower than 10%. Finally, recovery tests were performed to evaluate the water matrices effects on the extraction performance, resulting in recoveries between 76% and 110% in surface water and between 84% and 109% in wastewater.publishe

Producing Efficient Adsorbents from Kraft Lignin for the Removal of Contaminants from Water—A Full Factorial Design

This work aimed at optimizing the preparation of activated carbon (AC) from Kraft lignin for the adsorption of methylene blue (MB) and amoxicillin (AMX) from water. A full factorial design of three factors (precursor:activating agent (H3PO4) ratio, pyrolysis temperature, and residence time) at two levels was used to optimize the AC production. Eight AC products were obtained and evaluated considering the following responses: product yield, specific surface area (SBET), energy consumption, and adsorptive removal of the contaminants under study. The produced AC presented satisfactory SBET, ranging between 750 and 1335 m2 g−1, and efficient adsorption of MB and AMX from water, achieving up to 99% removal under the studied experimental conditions (100 mg L−1 of MB and AMX solution and material dose of 1 g L−1). Statistical analysis showed that product yield and energy consumption for AC production were influenced by temperature and residence time. The determination of a desirability function indicated a precursor/H3PO4 ratio of 1:2, pyrolysis at 700 °C, and residence time of 60 min as the optimal production conditions. The optimized AC presented SBET 1335 m2 g−1 and maximum adsorption capacity of 210 and 280 mg g−1 for MB and AMX, respectively

Fecal Microbiota Transplant in a Pre-Clinical Model of Type 2 Diabetes Mellitus, Obesity and Diabetic Kidney Disease

Diabetes mellitus (DM) burden encompasses diabetic kidney disease (DKD), the leading cause of end-stage renal disease worldwide. Despite compelling evidence indicating that pharmacological intervention curtails DKD progression, the search for non-pharmacological strategies can identify novel targets for drug development against metabolic diseases. One of those emergent strategies comprises the modulation of the intestinal microbiota through fecal transplant from healthy donors. This study sought to investigate the benefits of fecal microbiota transplant (FMT) on functional and morphological parameters in a preclinical model of type 2 DM, obesity, and DKD using BTBRob/ob mice. These animals develop hyperglycemia and albuminuria in a time-dependent manner, mimicking DKD in humans. Our main findings unveiled that FMT prevented body weight gain, reduced albuminuria and tumor necrosis factor-α (TNF-α) levels within the ileum and ascending colon, and potentially ameliorated insulin resistance in BTBRob/ob mice. Intestinal structural integrity was maintained. Notably, FMT was associated with the abundance of the succinate-consuming Odoribacteraceae bacteria family throughout the intestine. Collectively, our data pointed out the safety and efficacy of FMT in a preclinical model of type 2 DM, obesity, and DKD. These findings provide a basis for translational research on intestinal microbiota modulation and testing its therapeutic potential combined with current treatment for DM