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Antibiotics are among the emerging contaminants of greatest concern to the scientific community. However, the occurrence and behaviour of their metabolites in soils have been scarcely studied. To address this research gap, this study investigates the occurrence, sorption, dissipation kinetics, and environmental risk of highly important antibiotics (sulfamethazine, sulfadiazine, sulfamethoxazole, trimethoprim) and their main metabolites in Mediterranean agricultural soils. Batch experiments were conducted under natural conditions for 120 days. Five different dissipation kinetics models were applied to elucidate antibiotics degradation. The sorption isotherms were evaluated by three different models. Most of the antibiotics and metabolites tested showed a good fit with the Linear Isotherm model (R 2 >0.96) and biphasic dissipation kinetic models (R 2 >0.90). The dissipation and the endpoints values (DT 50 and DT 90 ) depended on the soil type properties. A Lixisol soil demonstrated reduced degradation of the investigated compounds. Trimethoprim showed the highest persistence, followed by sulfamethazine, sulfamethoxazole, and sulfadiazine. Parent compounds exhibited lower degradation rates than their metabolites. Remaining antibiotic concentrations were found to be below the predicted no-effect concentration in soil, suggesting that they may not pose a risk to terrestrial biota. This study provides valuable insights into the behaviour of these antibiotics and their metabolites in soil., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier B.V. All rights reserved.)

Antibiotics are a group of drugs used for the treatment of bacterial diseases. They are used in both human and veterinary medicine and, although they are not permitted, they are sometimes used as growth promoters. The present research compares two extraction techniques: ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) in order to evaluate their efficiency in the determination of 17 usually prescribed antibiotics in human nails. The extraction parameters were optimized using multivariate techniques. Once both techniques were compared, MAE was selected as optimal due to its greater experimental practicability together with the better extraction efficiencies it provides. Target analytes were detected and quantified by ultra-high performance liquid chromatography with tandem mass spectrometry detection (UHPLC-MS/MS). The run time was 20 min. The methodology was then successfully validated, obtaining acceptable analytical parameters according to the guide used. Limits of detection were between 0.3 and 3 ng g -1 and limits of quantification were in the range from 1.0 to 4.0 ng g -1 . Recovery percentages ranged from 87.5% to 114.2%, and precision (in terms of standard deviation) was less than 15% in all cases. Finally, the optimized method was applied to nails taken from 10 volunteers and the results revealed the presence of one or more antibiotics in all the samples examined. The most commonly found antibiotic was sulfamethoxazole, followed by danofloxacin and levofloxacin. The results demonstrated, on the one hand, the presence of these compounds in the human body and, on the other hand, the suitability of nails as a non-invasive biomarker of exposure., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Due to the growing trend of organic food, there is still concern over the use of chemicals and pesticides in agriculture. In recent years, several procedures have been validated for the control of pesticides in food. In the present research, a comprehensive two-dimensional liquid chromatography coupled with tandem mass spectrometry is proposed for the first time for a multi-class analysis of 112 pesticides in corn-based products. Notably, a "reduced" QuEChERS-based method as extraction and clean-up procedure prior to the analysis, was successfully employed. Limits of quantification values were lower than the ones fixed by the European legislation; intra-day and inter-day precision were lower than 12.9% and 15.1%, respectively (at the 500 μg/kg concentration levels). Over 70% of the analytes provided recoveries between 70% and 120% range (at 50, 500 and 1000 µg/kg concentration levels) with standard deviation values below 20%. In addition, matrix effect values were in the range between 13% to 161%. The method was applied to the analysis of real samples, and three pesticides were detected at trace levels in both samples. The findings of this work pave the way for the treatment of complex matrices such as corn products., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Personal care products (PCPs) and cosmetics are indispensable product in our daily routine. Their widespread use makes them a potential route of exposure for certain contaminants to which human would not be normally exposed. One of these contaminants includes endocrine disrupting chemicals, molecules capable of mimicking the body's natural hormones and interfering with the endocrine system. Some of them are ingredients included in the product's formulation, such as UV-filters (sunscreens), phthalates (plasticizers and preservatives), synthetic musks (fragrances), parabens and other antimicrobial agents (antimicrobial preservatives). Others are non-intended added substances that may result from the manufacturing process or migration from the plastic packaging, as with bisphenols and perfluorinated compounds. Some of these endocrine disruptors have been restricted or even banned in cosmetics and PCPs given the high risk they pose to health. Thus, the development of fast, sensitive and precise methods for the identification and quantification of these compounds in cosmetics is a substantial need in order to ensure consumer safety and provide insight into the real risk of human exposure. The present work aims at reviewing the more recently developed analytical methods published in the literature for the determination of endocrine disrupting chemicals in cosmetics and PCPs using chromatographic techniques, with a focus on sample treatment and the quality of analytical parameters., (Copyright © 2021 Elsevier B.V. All rights reserved.)

Rapid industrialization has resulted in a progressive increase in human exposure to hazardous chemicals. The present work develops and validates a new method to determinate 18 endocrine disrupting chemicals (EDCs) in human nail samples. In contrast to other common biological samples, nail sampling is non-invasive and since they take several months to grow out, they are well suited for measuring and reflecting the cumulative exposure to harmful substances in the long term. A digestion of samples with a 0.04 M solution of sodium hydroxide is carried out followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), working in multiple-reaction-monitoring (MRM) mode. The compounds were separated in 8 min. Multivariate optimization strategies were used for the optimization of the parameters that affects the digestion procedure. The validation was developed using a matrix-matched calibration and a recovery assay with spiked samples. The limits of detection and quantification ranged from 0.3 to 1.2 ng g -1 and from 1 to 5 ng g -1 , respectively. Recovery rates for spiked samples were between 88% and 113% and the relative standard deviation (% RSD) was lower than 12.7% for all studied EDCs. The method was applied for the analysis of these compounds in human nail samples from volunteers. All samples tested positive for several of the analyzed EDCs., (Copyright © 2019 Elsevier B.V. All rights reserved.)

Emerging contaminants are a heterogeneous group of chemicals that includes daily personal care products and pharmaceuticals (PPCPs), flame retardants, endocrine disrupting chemicals (EDCs) and nanoparticles (NPs). The present work is an overview focused in the research published in the scientific literature for the determination of this type of pollutants in sewage sludge samples in the last 5 years. Instrumental and sample preparation methods for the detection and quantification of the analytes of interest are reviewed, with an emphasis on the sample treatment techniques. Liquid chromatography (LC) and gas chromatography (GC) coupled to mass spectrometry are generally employed as the analytical technique of preference. Sample preparation techniques include conventional methods such as Soxhlet, solid-phase extraction (SPE), pressurized liquid extraction (PLE) or ultrasound-assisted extraction (UAE), but also other recent techniques, including novel microextraction techniques such as microextraction by packed sorbent (MEPS) or solid-phase microextraction (SPME)., (Copyright © 2018 Elsevier B.V. All rights reserved.)