Search

The use of fluoroquinolones for the treatment of infections in humans and animals has increased in Argentina, and they can be found in large amounts in water bodies. The present study investigated the occurrence and associated ecological risk of 5 fluoroquinolones in rivers and farm wastewaters of San Luis, Santa Fe, Córdoba, Entre Ríos, and Buenos Aires provinces of Argentina by high‐performance liquid chromatography coupled to fast‐scanning fluorescence detection and ultra–high‐performance liquid chromatography coupled to triple quadrupole mass spectrometry detection. The maximum concentrations of ciprofloxacin, enrofloxacin, ofloxacin, enoxacin, and difloxacin found in wastewater were 1.14, 11.9, 1.78, 22.1, and 14.2 μg L–1, respectively. In the case of river samples, only enrofloxacin was found, at a concentration of 0.97 μg L–1. The individual risk of aquatic organisms associated with water pollution due to fluoroquinolones was higher in bacteria, cyanobacteria, algae, plants, and anurans than in crustaceae and fish, with, in some cases, risk quotients >1. The proportion of samples classified as high risk was 87.5% for ofloxacin, 63.5% for enrofloxacin, 57.1% for ciprofloxacin, and 25% for enoxacin. Our results suggest that the prevalence of fluoroquinolones in water could be potentially risky for the aquatic ecosystem, and harmful to biodiversity. Environ Toxicol Chem 2019;38:2305–2313. © 2019 SETAC. [ABSTRACT FROM AUTHOR]

A low-level data fusion strategy was developed and implemented for data processing of second-order liquid chromatographic data with dual detection, i.e. absorbance and fluorescence monitoring. The synergistic effect of coupling individual information provided by two different detectors was evaluated by analyzing the results gathered after the application of a series of data preprocessing steps and chemometric resolution. The chemometric modeling involved data analysis by MCR-ALS, PARAFAC and N-PLS. Their ability to handle the new data block was assessed through the estimation of the analytical figures of merits achieved in the prediction of a validation set containing fifteen fluorescent and non-fluorescent veterinary active ingredients that can be found in poultry litter. Eventually, the feasibility of the application of the fusion strategy to real poultry litter samples containing the studied compounds was verified. [ABSTRACT FROM AUTHOR]

An efficient generic static headspace gas chromatography (HSGC) method was developed, optimized and validated for the routine determination of several residual solvents (RS) in drug substance, using a strategy with two sets of calibration. Dimethylsulfoxide (DMSO) was selected as the sample diluent and internal standards were used to minimize signal variations due to the preparative step. A gas chromatograph from Agilent Model 6890 equipped with flame ionization detector (FID) and a DB-624 (30 m×0.53 mm i.d., 3.00 µm film thickness) column was used. The inlet split ratio was 5:1. The influencing factors in the chromatographic separation of the analytes were determined through a fractional factorial experimental design. Significant variables: the initial temperature (IT), the final temperature (FT) of the oven and the carrier gas flow rate (F) were optimized using a central composite design. Response transformation and desirability function were applied to find out the optimal combination of the chromatographic variables to achieve an adequate resolution of the analytes and short analysis time. These conditions were 30 °C for IT, 158 °C for FT and 1.90 mL/min for F. The method was proven to be accurate, linear in a wide range and very sensitive for the analyzed solvents through a comprehensive validation according to the ICH guidelines. [ABSTRACT FROM AUTHOR]

Retinoids are known to regulate important processes such as differentiation, development, and embryogenesis of vertebrates: Alteration in endogenous retinoids concentration is linked with teratogenic effects. Retinol (ROH), retinoid acid (RA), and isoform 13-Cis-retinoic acid (13-Cis-RA), in plasma of a native adults frog, Leptodactylus chaquensis from a rice field (RF) and a forest (reference site; RS) were measured. ROH did not vary between treatment sites. RA and 13-Cis-RA activities were higher (93.7 ± 8.6 μg mL −1 and 131.7 ± 11.4 μg mL −1 , respectively) in individuals collected from RF than in those from RS (65.5 ± 8.6 μg mL −1 and 92.2 ± 10.2 μg mL −1 , respectively). The ratios retinoic acid-retinol (RA/ROH) and 13-Cis-RA/ROH revealed significantly higher values in RF than in RS. RA and 13-Cis-RA concentrations in plasma on wild amphibian’s species such as L . chaquensis would be suitable biomarkers of pesticide exposure in field monitoring. Finally, the mechanism of alteration in retinoid metabolites alteration should be further explored both in larvae and adult, considering that the potential exposition and uptake contaminants vary between the double lives of these vertebrates. [ABSTRACT FROM AUTHOR]

The present tutorial aims to review the most frequently reported criteria for the calculation of the limits of detection (LOD) and quantification (LOQ) in univariate calibration, summarizing their fundamentals, advantages, and limitations. The current criteria for estimating LOD and LOQ are based on diverse theoretical and/or empirical assumptions and require different amounts of experimental data, making the calculation rather complex in some cases. Moreover, alternative forms for calculating LOD/LOQ frequently lead to dissimilar results. This scenario might worsen in the case of complex analytical systems. Throughout this tutorial, different forms of calculating LOD/LOQ are illustrated using previously reported experimental datasets in the environmental chemistry field as examples. The influence of the sample matrix during the estimation of LOD/LOQ parameters is investigated through one calibration approache. The discrepancies in the obtained results with different criteria for the calculation of LOD/LOQ are highlighted. Finally, general guidelines and recommendations regarding experimental and data processing issues are proposed, aiming to promote fair criteria for the comparison of different analytical methodologies in terms of prediction ability and detection capability. [Display omitted] • Tutorial for calculation of the limits of detection (LOD) and quantification (LOQ). • The focus of the study is put on complex analytical systems. • Fundamentals, advantages and limitations are discussed. • Frequently, alternative forms for calculating LOD/LOQ lead to dissimilar results. • Different forms of calculation are illustrated, using previously reported experimental datasets. [ABSTRACT FROM AUTHOR]

The ecological risks posed by two β-diketone antibiotics (DKAs, enrofloxacin, ENR and ciprofloxacin, CPX), characterized by their long persistence in aqueous environments and known deleterious effect on model organisms such as zebrafish were analysed using Rhinella arenarum larvae. Sublethal tests were conducted using environmentally relevant concentrations of both ENR and CPX (1–1000 μg L −1 ) under standard laboratory conditions for 96 h. Biological endpoints and biomarkers evaluated were body size, shape, development and growth rates, and antioxidant enzymes (glutathione-S-transferase, GST; Catalase, CAT). Risk assessment was analysed based on ration quotients (RQ). The size and shape measurements of the larvae exposed to concentrations greater than 10 μg L −1 of CPX were lower compared to controls (Dunnett post hoc p < 0.05) and presented signs of emaciation. Concentrations of 1000 μg L −1 of CPX induced GST activity, in contrast with inhibited GST and CAT of larvae exposed to ENR. Risk assessments indicated that concentrations greater than or equal to10 μg L −1 of CPX and ENR are ecotoxic for development, growth, detoxifying, and oxidative stress enzymes. It is suggested that additional risk assessments may provide evidence of bioaccumulation of CPX and ENR in tissues or organs of amphibian larvae by mesocosm sediment test conditions. Finally, intestinal microbiome studies should be considered to establish the mechanisms of action of both antibiotics. [ABSTRACT FROM AUTHOR]