Search Results (7)

Objective: We set out to evaluate the persistence of sulfachloropyridazine, oxytetracycline, and enrofloxacin in broiler chicken litter following therapeutic oral treatment and its association with the isolation of Escherichia coli resistant to these antimicrobials. Methods: Forty broiler chickens were raised under controlled conditions and divided into three experimental groups, each treated with a different antimicrobial, in addition to an untreated/control group. Litter samples were collected post treatment, analyzed by UPLC-MS/MS, and processed for the isolation of E. coli. The antimicrobial susceptibility of E. coli was assessed using the Kirby–Bauer disk diffusion method. Results: Chemical analysis detected concentrations of antimicrobials throughout post treatment, reaching maxima of 42,910.14 μg kg⁻¹, 92,712 μg kg⁻¹, and 9567 μg kg⁻¹ for sulfachloropyridazine, oxytetracycline plus 4-epi-oxytetracycline, and enrofloxacin plus ciprofloxacin, respectively. It was estimated that the concentrations of sulfachloropyridazine, oxytetracycline, and enrofloxacin would persist in broiler litter for 61, 244, and 514 days, respectively. A very strong association was observed between the presence of antimicrobial residues and the antimicrobial resistance of E. coli (p-value < 0.0001, and Cramer’s coefficient of 0.47), and an independence between the level of residue concentration and susceptibility (p-value 0.5262). Conclusions: The persistence of antimicrobial residues contributes to the selection of resistant bacteria, regardless of persistent antimicrobial concentrations. These findings highlight the need for stricter regulations on poultry litter management, including residue thresholds and resistance monitoring, to minimize environmental and public health risks. Proper treatment of poultry litter is essential to ensure its sustainable and safe re-use in agricultural systems. Full article

A diatomite-modified Fe₂O₃ (Fe₂O₃/Dia) catalyst was prepared to catalyze the ozonation degradation of sulfachloropyridazine sodium (SPDZ). The chemical oxygen demand (COD) was used as the index of pollutant degradation. The catalytic ozonation experiment showed that the COD removal rate of SPDZ was 87% under Fe₂O₃/Dia catalysis, which was much higher than that obtained when using Fe₂O₃ as the catalyst. The characteristics of the Fe₂O₃/Dia catalyst were investigated, and the successful synthesis of the Fe₂O₃/Dia composite catalyst was proved by XRD, XPS, SEM, FTIR, BET and other characterization methods. The catalytic mechanism of degradation by ozone with Fe₂O₃/Dia was analyzed. According to free-radical trapping experiments and an in situ electron paramagnetic spectrometer characterization analysis, the main oxidizing species in the catalytic Fe₂O₃/Dia ozone system is ·OH. The intermediates in the degradation process of SPDZ were detected and analyzed in detail by liquid chromatography-coupled mass spectrometry. The degradation mechanism and three degradation paths of SPDZ were proposed. Full article

Oxytetracycline (OTC), enrofloxacin (EFX), and sulfachloropyridazine (SCP) are critically important antimicrobials (AMs) in both human and veterinary medicine, where they are widely used in farm animals. Lettuce has become a matrix of choice for studying the presence of residues of these AMs in plants, as the concentrations of residues detected in lettuce can range from ng to mg. While several analytical methodologies have been developed for the purpose of detecting AMs in lettuce, these currently do not detect both the parent compound and its active metabolites or epimers, such as in the case of ciprofloxacin (CFX) and 4-epi-oxitetracycline (4-epi-OTC), which also pose a risk to public health and the environment due to their AM activity. In light of this situation, this work proposes an analytical method that was developed specifically to allow for the detection of OTC, 4-epi-OTC, EFX, CFX, and SCP in a lettuce matrix. This method uses acetonitrile, methanol, 0.5% formic acid, and McIlvaine-EDTA buffer as extraction solvents, and dispersive solid-phase extraction (dSPE) for the clean-up. The analytes were detected using a liquid chromatography technique coupled to mass spectrometry (HPLC-MS/MS). Parameters such as the specificity, linearity, recovery, precision, limit of detection, and limit (LOD) of quantification (LOQ) were calculated according to the recommendations established in the European Union decision 2021/808/EC and VICH GL2: Validation of analytical procedures. The LOQ for the analytes OTC, 4-epi-OTC, CFX, and SCP was 1 μg·kg⁻¹, whereas for EFX, it was 5 μg·kg⁻¹ dry weight. All calibration curves showed a coefficient of determination (R²) of >0.99. The recovery levels ranged from 93.0 to 110.5% and the precision met the acceptance criteria, with a coefficient of variation of ≤14.02%. Therefore, this methodology allows for the precise and reliable detection and quantification of these analytes. The analysis of commercial samples confirmed the suitability of this method. Full article

Biological activated carbon (BAC) biofilter coupling ultrafiltration (UF) is a promising process for the treatment of river water contaminated by pharmaceutical and personal care products (PPCPs). However, the pilot-scale study should be conducted to reveal the long-term removal performance and the respective contributions of BAC and UF. In this study, a BAC-UF system with treatment capacity of 0.16 m³ h⁻¹ was operated for 130 days. The water quality was analyzed in terms of COD_Mn, UV₂₅₄, NH₄⁺-N, and PPCPs. The results showed that both BAC and UF were related to the removal of organic matter (COD_Mn and UV₂₅₄), achieving the removals of 56.00% and 55.25%, respectively. Similarly, BAC and UF were both relevant to the removal effects of ammonia nitrogen, nitrite, and nitrate. Moreover, the BAC-UF process was featured with a high efficiency in the removal of PPCPs, and the average removal of total PPCPs reached 47.84%, especially anhydroerythromycin, sulfachloropyridazine, sulfadiazine, trimethoprim, and caffeine. Besides, it was found that the BAC unit played a key role in PPCPs removal and the UF unit also degraded them by the biomass on UF membranes. Therefore, this study proved the removal performance of BAC-UF for treating popular pollutants from river water, and the BAC-UF process in this work can be considered as a feasible method of producing clean drinking water. Full article

Tetracyclines, sulphonamides, and quinolones are families of antimicrobials (AMs) widely used in the poultry industry and can excrete up to 90% of AMs administrated, which accumulate in poultry litter. Worryingly, poultry litter is widely used as an agriculture fertilizer, contributing to the spread AMs residues in the environment. The aim of this research was to develop a method that could simultaneously identify and quantify three AMs families in poultry litter by high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS). Samples of AMs free poultry litter were used to validate the method according to 657/2002/EC and VICH GL49. Results indicate that limit of detection (LOD) ranged from 8.95 to 20.86 μg kg⁻¹, while limits of quantitation (LOQ) values were between 26.85 and 62.58 µg kg⁻¹ of tetracycline, 4-epi-tetracycline, oxytetracycline, 4-epi-oxytetracycline, enrofloxacin, ciprofloxacin, flumequine, sulfachloropyridazine, and sulfadiazine. Recoveries obtained ranged from 93 to 108%. The analysis of field samples obtained from seven commercial poultry flocks confirmed the adequacy of the method since it detected means concentrations ranging from 20 to 10,364 μg kg⁻¹. This provides us an accurate and reliable tool to monitor AMs residues in poultry litter and control its use as agricultural fertilizer. Full article

The largest wastewater treatment plant in Jordan was monitored in the summer to determine the removal of pharmaceuticals and personal care products (PPCPs). Grab samples were collected from the influent and effluent of As-Samra Wastewater Treatment Plant (WWTP). Liquid chromatography and tandem mass spectrometry (LC–MS/MS) were utilized to determine the concentrations of 18 compounds of pharmaceuticals and personal care products (PPCPs). The results showed that 14 compounds were detected in the collected samples from the influent and effluent of As-Samra WWTP. These compounds are 1,7-dimethylxanthine, amphetamine, acetaminophen, caffeine, carbamazepine, cimetidine, cotinine, diphenhydramine, methylenedioxymethamphetamine (MDMA), morphine, phenazone, sulfamethazine, sulfamethoxazole, thiabendazole, and trimethoprim. However, four compounds were below the detection limit (<0.005 µg/L), namely cimetidine, methylenedioxyamphetamine (MDA), methamphetamine, and sulfachloropyridazine. Among PPCPs, the highest estimated average concentrations in raw wastewater were caffeine, acetaminophen, 1,7-dimethylxanthine, cotinine, and carbamazepine sampled during the summer, at an estimated concentration of 155.6 µg/L, 36.7 µg/L, 10.49 µg/L, and 1.104 µg/L, respectively. However, the highest estimated average concentrations in treated wastewater were for carbamazepine, sulfamethoxazole, caffeine, cotinine, and acetaminophen, at 0.856 µg/L, 0.096 µg/L, 0.086 µg/L, 0.078 µg/L, and 0.041 µg/L, respectively. In general, the results showed that some compounds in the collected samples of wastewater in Jordan have concentrations exceeding the values reported in the literature. The removal efficiency rates of 1,7-dimethylxanthine, acetaminophen, caffeine, cotinine, morphine, and trimethoprim were higher than 95%, while those of carbamazepine, sulfamethazine, and sulfamethoxazole were lower than 22.5%. Moreover, diphenhydramine and thiabendazole had negative removal efficiency rates. The removal efficiency rates of the PPCPs in As-Samra WWTP were generally consistent with those of indicator compounds reported in the literature for conventional WWTPs. Full article

Tetracyclines, sulfonamides and amphenicols are broad spectrum antimicrobial drugs that are widely used in poultry farming. However, a high proportion of these drugs can be excreted at high concentrations in droppings, even after the end of a therapy course. This work intended to assess and compare concentrations of florfenicol (FF), florfenicol amine (FFa), chlortetracycline (CTC), 4-epi-chlortetracycline (4-epi-CTC), and sulfachloropyridazine (SCP) in broiler chicken droppings. To this end, 70 chickens were housed under controlled environmental conditions, and assigned to experimental groups that were treated with therapeutic doses of either 10% FF, 20% CTC, or 10% SCP. Consequently, we implemented and designed an in-house validation for three analytical methodologies, which allowed us to quantify the concentrations of these three antimicrobial drugs using liquid chromatography coupled to mass spectrometry (LC-MS/MS). Our results showed that FF and FFa concentrations were detected in chicken droppings up to day 10 after ceasing treatment, while CTC and 4-epi-CTC were detected up to day 25. As for SCP residues, these were detected up to day 21. Noticeably, CTC showed the longest excretion period, as well as the highest concentrations detected after the end of its administration using therapeutic doses. Full article