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Microbial communities play an important role in water quality regulation and biogeochemical cycles in lakes, and their community structure and function are affected by environmental factors. Therein, antibiotics affect the abundance, diversity, composition, and function of microbial communities. In this study, Baiyangdian Lake was selected as the study area. Sediment samples of 16 sites were collected in August 2018 and April 2019, respectively. Ultra-high performance liquid chromatography-mass spectrometry （HPLC-MS/MS） was used to determine the content of typical antibiotics-quinolones （QNs） in sediment. Through high-throughput sequencing technology, the structure and function of microbial communities was analyzed in the sediments to explore the spatiotemporal variation. Thereinto, redundancy analysis （RDA） was used to identify the key influencing factors of spatiotemporal variation of microbial communities. The results showed that： ① From August to April, the average ω （QNs） showed an increasing trend, and its mean value changed from 3.91 ng·g -1 to 6.34 ng·g -1 , with significant seasonal differences in oxolinic acid （OXO） and total QNs content （ P < 0.05）. ② In terms of temporal variation, the dominant bacteria were Proteobacteria and Chloroflexi. The relative abundance of Proteobacteria showed a decreasing trend, whereas Chloroflexi showed an increasing trend； at the genus level, the dominant bacteria genera in August were norank_ f__Anaerolineaceae and Thiobacilus , and the dominant bacteria genera in April were Acinetobacter and norank_ f_Anaerolineaceae, and the dominant bacteria genera had significant seasonal differences （ P < 0.05）. ③ In terms of temporal variation, the index of Simpson, Chao, Ace, and OTU number all showed an increasing trend, and the seasonal differences were significant （ P < 0.05）. ④ In terms of spatial variation, there were no significant spatial differences among functional genes of COG. In terms of temporal variation, there were significant seasonal differences in functional genes of energy production and conversion, carbohydrate transport and metabolism, transcription, cell wall/membrane/envelope biogenesis, and signal transduction mechanisms （ P < 0.01 and P < 0.05）. ⑤ Microbial community structure and functional genes were significantly correlated with QNs （ P < 0.01 and P < 0.05）, and QNs were the main influencing factors. Therefore, QNs were the main factor affecting the changes in microbial community structure and functional genes in sediments of Baiyangdian Lake. Thus, comprehensive control of antibiotic pollution in sediments should be further strengthened.

Yancheng coastal wetland, the largest coastal wetland in the west coast of the Pacific Ocean and the margin of the Asian continent, has significant environmental, economic and social effects on local human beings. The extensive contamination and potential risk of quinolone antibiotics (QNs) on local aquaculture and human health are still not clear until now. In this study, 52 surface sediment samples were collected to investigate the contamination status and polluted sources, and evaluate ecological risks of QNs in the south of Yancheng coastal wetland. The total contents of QNs ranged from 0.33 to 21.60 ng/g dw (mean value of 4.51 ng/g dw), following the detection frequencies of QNs ranging from 19.23 to 94.23%. The highest content of QNs occurred around an aquaculture pond dominated by flumequine. The total organic carbon contents of sediment were positively correlated with sarafloxacin and lomefloxacin (p < 0.05), indicating the enhanced absorption of these QNs onto sediments. Partial QNs, such as lomefloxacin, enrofloxacin, sarafloxacin and flumequine, presented the homology features originating from the emission of medical treatment and aquaculture. There was no potential risk of QNs to human beings but a potential risk to aquatic organisms (algae > plant > invertebrate). Totally, the management and protection of Yancheng coastal wetland should be of concern with aquaculture as the important industry., (© 2024. The Author(s), under exclusive licence to Springer Nature B.V.)

Background: Antibiotics residues can accelerate the growth of drug-resistant bacteria and harm the ecological environment. Under the effect of enrichment and biomagnification, the emergence of drug-resistant pathogenic bacteria may eventually lead to humans being ineffective to drugs in the face of bacterial or fungal disease infections in the future. It is urgent to develop an efficient separation medium and analytical method for simultaneous extraction and determination of antibiotics in the water environment., Results: This work doped 2,6-Di-O-methyl-β-cyclodextrin, randomly methyl-β-cyclodextrin, 2-hydroxypropyl-β-cyclodextrin with thymol:fatty acid respectively to construct non-covalent interaction-dominated pH-responsive ternary supramolecular deep eutectic solvents (SUPRADESs), which can undergo a hydrophilic/hydrophobic transition with aqueous phase to achieve an efficient microextraction. Semi-empirical method illustrated that SUPRADESs have a wide range of hydrogen bond receptor sites. We developed a SUPRADES-based analytical method combined with liquid chromatography-triple quadrupole mass spectrometry for the extraction and determination of trace quinolones and sulfonamides in wastewater. The overall limits of detection of the method were 0.0021-0.0334 ng mL -1 and the limits of quantification were 0.0073-0.1114 ng mL -1 . The linearity maintained good in the spiked level of 0.01-100 ng mL -1  (R 2  > 0.99). The overall enrichment factors of the method were 157-201 with lower standard deviations (≤8.7)., Significance: The method gave an extraction recovery of 70.1-115.3 % for 28 antibiotics in livestock farming wastewater samples from Zhejiang, China, at trace levels (minimum 0.5 ng mL -1 ). The results demonstrated that inducing the phase transition between SUPRADES and aqueous phase by adjusting pH for extraction is a novel and efficient pretreatment strategy. To our knowledge, this is the first application of cyclodextrin-based ternary SUPRADESs with pH-responsive reversible hydrophobicity-hydrophilicity transition behavior in wastewater analysis., 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 Elsevier B.V. All rights reserved.)

There is a large surface-groundwater exchange downstream of wastewater treatment plants (WWTPs), and antibiotics upstream may influence sites downstream of rivers. Thus, samples from 9 effluent-receiving urban rivers (ERURs) and 12 groundwater sites were collected in Shijiazhuang City in December 2020 and April 2021. For ERURs, 8 out of 13 target quinolone antibiotics (QNs) were detected, and the total concentration of QNs in December and April were 100.6-4,398 ng/L and 8.02-2,476 ng/L, respectively. For groundwater, all target QNs were detected, and the total QNs concentration was 1.09-23.03 ng/L for December and 4.54-170.3 ng/L for April. The distribution of QNs was dissimilar between ERURs and groundwater. Most QN concentrations were weakly correlated with land use types in the system. The results of a positive matrix factorization model (PMF) indicated four potential sources of QNs in both ERURs and groundwater, and WWTP effluents were the main source of QNs. From December to April, the contribution of WWTP effluents and agricultural emissions increased, while livestock activities decreased. Singular value decomposition (SVD) results showed that the spatial variation of most QNs was mainly contributed by sites downstream (7.09%-88.86%) of ERURs. Then, a new method that combined the results of SVD and PMF was developed for a specific-source-site risk quotient (SRQ), and the SRQ for QNs was at high level, especially for the sites downstream of WWTPs. Regarding temporal variation, the SRQ for WWTP effluents, aquaculture, and agricultural emissions increased. Therefore, in order to control the antibiotic pollution, more attention should be paid to WWTP effluents, aquaculture, and agricultural emission sources for the benefit of sites downstream of WWTPs., 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. Published by Elsevier B.V.)

This study aimed to present a selective and effective method for analyzing quinolones (QNs) in food matrix. Herein, a NiFe 2 O 4 -based magnetic sodium disulfonate covalent organic framework (NiFe 2 O 4 /COF) was prepared using a simple solvent-free grinding method, and was adopted as a selective adsorbent for magnetic solid phase extraction of QNs. Coupled with UHPLC-Q-Orbitrap HRMS, an efficient method for simultaneous detection of 18 kinds of QNs was established. The method exhibited good linearity (0.01-100 ng g -1 ), high sensitivity (LODs ranging from 0.0011 to 0.0652 ng g -1 ) and precision (RSDs below 9.5%). Successful extraction of QNs from liver and kidney samples was achieved with satisfactory recoveries ranging from 82.2% to 108.4%. The abundant sulfonate functional groups on NiFe 2 O 4 /COF facilitated strong affinity to QNs through electrostatic and hydrogen bonding interactions. The proposed method provides a new idea for the extraction of contaminants with target selectivity., Competing Interests: Declaration of competing interest The authors declare that none of the work presented in this study may have been impacted by any known competing financial interests or personal ties., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Quinolones, a widely used class of antibiotics, present significant environmental and health concerns if they excessively remain in the environment and in food. Aptamers specific to quinolones can be applied as bioreceptors for the detection of quinolone residues in the environment and food. The quinolone family contains dozens of different individuals that share the same core structure coupled with various substituents at six different positions. The diversity and complexity of the substitution sites make it a challenge to choose a set of representative molecules that encompass all the desired sites and preserve the core molecular framework for the screening of quinolone-specific aptamers via systematic evolution of ligands by exponential enrichment (SELEX). To address this challenge, we introduce a novel parallel-series strategy guided by Liebig's law for isolating quinolone-specific cross-reactive aptamers by using the library-immobilized SELEX method. Through this approach, we successfully identified 5 aptamers (Apt.AQ01-Apt.AQ05) with high binding affinity and excellent specificity to 24 different quinolone individuals. Among them, Apt.AQ03 showcased optimal performance with affinities ranging from 0.14 to 1.07 μM across the comprehensive set of 24 quinolones, exhibiting excellent specificity against nontarget interferents. The binding performance of Apt.AQ03 was further characterized with microscale thermophoresis, circular dichroism spectra, and an exonuclease digestion assay. By using Apt.AQ03 as a bioreceptor, a fluorescence resonance energy transfer (FRET) aptasensor was developed for the detection of 24 quinolones in milk, achieving a remarkable detection limit of 14.5-21.8 ng/mL. This work not only establishes a robust and effective strategy for selecting cross-reactive aptamers applicable to other small-molecule families but also provides high-quality aptamers for developing various high-throughput and reliable methods for the detection of multiple quinolone residues in food.

To establish infections in human hosts, Pseudomonas aeruginosa must overcome innate immune-generated oxidative stress, such as the hypochlorous acid (HOCl) produced by neutrophils. We set out to find specific biomarkers of oxidative stress through the development of a protocol for the metabolic profiling of P. aeruginosa cultures grown in the presence of different oxidants using a novel ionization technique for mass spectrometry, laser desorption rapid evaporative ionization mass spectrometry (LD-REIMS). We demonstrated the ability of LD-REIMS to classify samples as untreated or treated with a specific oxidant with 100% accuracy and identified a panel of 54 metabolites with significantly altered concentrations after exposure to one or more of the oxidants. Key metabolic changes were conserved in P. aeruginosa clinical strains isolated from patients with cystic fibrosis lung infections. These data demonstrated that HOCl stress impacted the Pseudomonas quinolone signal (PQS) quorum sensing system. Ten 2-alkyl-4-quinolones (AHQs) associated with the PQS system were significantly lower in concentration in HOCl-stressed P. aeruginosa cultures, including 2-heptyl-3-hydroxy-4(1H)-quinolone (PQS), the most active signal molecule of the PQS system. The PQS system regulates the production of virulence factors, including pyocyanin and elastase, and their levels were markedly affected by HOCl stress. No pyocyanin was detectable and elastase concentrations were reduced by more than 75% in cultures grown with sub-lethal concentrations of HOCl, suggesting that this neutrophil-derived oxidant may disrupt the ability of P. aeruginosa to establish infections through interference with production of PQS-associated virulence factors., Importance: This work demonstrates that a high-throughput ambient ionization mass spectrometry method can be used successfully to study a bacterial stress response. Its application to the opportunistic pathogen Pseudomonas aeruginosa led to the identification of specific oxidative stress biomarkers, and demonstrated that hypochlorous acid, an oxidant specifically produced by human neutrophils during infection, affects quorum sensing and reduces production of the virulence factors pyocyanin and elastase. No pyocyanin was detectable and elastase levels were reduced by more than 75% in bacteria grown in the presence of hypochlorous acid. This approach has the potential to be widely applicable to the characterization of the stress responses of bacteria., Competing Interests: The authors declare no conflict of interest.

A rapid multi-residue LC-MS/MS method for the identification and determination of banned veterinary drugs in honey was developed. A total of 31 investigated veterinary drugs belonging to 4 classes including nitrofurans metabolites, nitroimidazoles, amphenicols, and quinolones were quantified by LC-MS/MS with ESI using one single injection. The sample preparation included treatment with 5-nitro-2-furaldehyde (5-NFA) in a thermostated ultrasonic bath (80 °C, 0.5М НСl, 20 min) to liberate matrix-bound residues of nitrofurans. Magnetic hypercrosslinked polystyrene (HCP/Fe 3 O 4 ) was proposed for the solid-phase extraction and clean-up of target analytes prior to LC-MS/MS analysis. To evaluate and validate the performance of method, the criteria of the Decision (EC) no 2002/657 were applied. The LOQs of the examined analytes range from 0.3 to 1 μg kg -1 , which indicates good sensitivity to quantify the target compounds in honey. The recoveries of veterinary drugs from 1 g of honey with 50 mg of the sorbent are 97-109% for nitrofuran metabolites, 84-115% for nitroimidazoles, 86-103% for amphenicols, and 97-118% for quinolones. The relative standard deviations of intra-day and inter-day precision analyses (RSD) are less than 16%. This methodology was applied to real honey samples and trace levels of some veterinary drugs were detected., 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.)

Quinolones are potent antibacterial drugs extensively utilized for treating bacterial infections in poultry. However, the presence of quinolone antibiotic residues in milk is a matter of concern due to potential health risks and adverse effects on milk quality. This review provides an overview of current analytical strategies for the determination of quinolone residues in milk. Various sample preparation techniques, such as liquid-phase extraction, solid-phase extraction and QuEChERS, are discussed, along with detection methods including instrument-based detection, immune-based detection, and microbial detection. The advantages and limitations of each method are highlighted, as well as their applicability in different stages of milk production. Additionally, recent advancements in sample preparation and detection methods are presented. This comprehensive review aims to contribute to the development of accurate and reliable methods for the detection of quinolone residues in milk, ensuring the safety and quality of dairy 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 Ltd. All rights reserved.)

Although veterinary antibiotics are essential in preventing and treating clinical diseases in cattle, the frequent use of antibiotics leads to antibiotic residues in milk and dairy products, consequently threatening human health. The massive milk consumption makes it necessary to assess antibiotic pollution and health impact comprehensively. Hence, we conducted a systematic review to evaluate antibiotics in milk and dairy products and their potential health risk. We searched four databases using multiple keyword combinations to retrieve 1582 pieces of literature and finally included eighteen articles to analyze antibiotic residues in milk and dairy products. These studies detected seven antibiotics in different regions of China. Quinolones and β-lactam antibiotics exceeded the MRL for raw and commercial milk. The maximum levels of sulfonamides and tetracyclines were detected in the same raw milk sample, exceeding the MRL. The estimated THQ and HI values in milk and dairy products are less than 1 for adults, indicating negligible noncarcinogenic health risk of antibiotics through consuming milk and dairy products. Children face higher health risks than adults, with the HI and THQ of quinolones exceeding 1. It is worth noting that quinolones accounted for nearly 89% of health risks associated with all antibiotics. Finally, we put forward possible research directions in the future, such as specific health effects of total dietary exposure to low levels of antibiotics. In addition, policymakers should effectively improve this problem from the perspectives of antibiotic use supervision, antibiotic residue analysis in food, and continuous environmental monitoring and control., (© 2023. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)

A nationwide study of the occurrence, distribution, potential drivers, and ecological risks of 24 quinolone antibiotics (QNs) in 74 Chinese sludge samples from 48 wastewater treatment plants (WWTPs) was conducted. In domestic sludge, the ∑QNs concentrations were  3rd-generation QNs > 4th-generation QNs > 1st-generation QNs. Meanwhile, abundant veterinary and human/veterinary quinolones (

Antibiotics are widely used in medical care, livestock production, and aquaculture. However, antibiotic pollution has attracted increasing global concerns due to their ecological risks after entering into environmental ecosystem via animal excretion, effulent from industrial and domestic sewage treatment facilities. In this study, 30 antibiotics were investigated in soils and irrigation rivers using ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometer. This study evaluated the occurrence, source apportionment, and ecological risks of these target compounds in soils and irrigation rivers (i.e., sediments and water) of farmland system by using principal component analysis-multivariate linear regression (PCA-MLR) and risk quotients (RQ). The concentration range of antibiotics in soils, sediments, and water was 0.38-689.58 ng/g, 81.99-658.00 ng/g, and 134.45-1547.06 ng/L, respectively. In soils, the most abundant antibiotics were quinolones and antifungals with an average concentration of 30.00 ng/g and 7.69 ng/g, respectively, contributing to 40% of total antibiotics. Macrolides were the most frequently detected antibiotics in soils with an average concentration of 4.94 ng/g. In irrigation rivers, quinolones and tetracyclines, the most abundant antibiotics, accounted for 78% and 65% of antibiotics in water and sediments, respectively. Higher antibiotic contamination of irrigation water was primarily distributed in highly populated urban areas, while increasing antibiotic contamination of sediments and soils was particularly observed in rural areas. PCA-MLR analysis indicated that antibiotic contamination in soils was mainly ascribed to the irrigation of sewage-receiving water body and manure application of livestock and poultry farming, which cumulatively contributed to 76% of antibiotics. According to RQ assessment, quinolones in irrigation rivers posed high risk to algae and daphnia, contributing 85% and 72% to the mixture risk, respectively. In soils, macrolides, quinolones and sulfonamides were responsible for more than 90% to the mixture risk of antibiotics. Ultimately, these findings can improve our fundamental knowledge on contamination characteristics and source pathways towards risk management of antibiotics in farmland system., 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 Ltd. All rights reserved.)

This is the first comprehensive report on antibiotics in the Huai River, a major Chinese river. To illuminate the concentrations, prioritization, spatial distributions, sources, and ecological risks of antibiotics, surface water samples were collected and three types of most widely used antibiotics (16 sulfonamides, 8 tetracyclines, and 14 quinolones) were analyzed. The results indicated that concentrations of ∑quinolones (86 ± 31 ng/L) > ∑tetracyclines (20 ± 13 ng/L) > ∑sulfonamides (11 ± 3.7 ng/L). Oxolinic acid (OXA), cinoxacin(CINX), norfloxacin (NFX), and methacycline (MTC) were the priority antibiotics with mean concentrations > or close to 10 ng/L, however, they were rarely included as target compounds in most previous Chinese investigations. Different spatial distributions of antibiotics were discovered across three reaches separated by two sluices, demonstrating that the sluices may impact antibiotic dissemination. According to the results of the source analysis, the aquaculture industry was the major source of observed antibiotics (49%), followed by livestock & poultry farming (26%) and mixed sources (25%). Because commercial fishing in the Huai River has been prohibited, the aquaculture industry will expand in the next years, and antibiotic contamination caused by the aquaculture industry deserves more attention. The risk quotients were calculated by comparing observed antibiotics to predicted no-effect concentrations, and the results showed that observed antibiotics posed negligible or low integrated risks for Green algae, and medium or low integrated risks for Daphnia magna., (© 2023. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)

As a non-traditional sample matrix, feather samples can be used to effectively monitor antibiotic addition and organismal residue levels in poultry feeding. Therefore, an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed to simultaneously determine the residue levels of 26 quinolones in poultry feathers. The feather samples were extracted by sonication with a 1% formic acid and acetonitrile mixture in a water bath at 50 °C for 30 min, purified by the adsorption of multiple matrix impurities, dried with nitrogen, redissolved, and analyzed by UPLC-MS/MS. The linearity, limit of detection (LOD), limit of quantification (LOQ), recovery and precision were calculated. The 26 antibiotics demonstrated good linearity in the linear range. The recoveries and coefficients of variation were 78.9-110% and <13.7% at standard spiked levels of 10, 100 and 200 μg/kg, respectively. The LOD and LOQ were 0.12-1.31 and 0.96-2.60 μg/kg, respectively. The method also successfully identified quinolone residues in 50 poultry feather samples. The results showed that quinolones can accumulate and stabilize for a certain period of time after transferring from the body to the feathers of poultry.

Due to their importance in human medicine, quinolones (QNs), as a typical class of antibiotics, are considered to be the "highest priority critically important antimicrobials" by the World Health Organization (WHO). In order to clarify the spatial-temporal variation and risk of QNs in soil, 18 representative topsoil samples were respectively collected in September 2020 (autumn) and June 2021 (summer). The contents of QNs antibiotics in soil samples were determined using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), and the ecological risk and resistance risk were calculated using the risk quotient method (RQ). The results showed that:① the average content of QNs decreased from autumn to summer (the average contents of QNs were 94.88 μg·kg -1 in autumn and 44.46 μg·kg -1 in summer); the highest values appeared in the middle area. ② The average proportion of silt was without change, whereas the average proportion of clay and sand was increased and decreased, respectively; the average contents of total phosphorus (TP), ammonia nitrogen (NH 4 + -N), and nitrate nitrogen (NO 3 - -N) also decreased. ③ The content of QNs was significantly correlated with soil particle size, nitrite nitrogen (NO 2 - -N), and nitrate nitrogen (NO 3 - -N) ( P <0.05). ④ The combined ecological risk of QNs showed high risk level (RQ sum >1), whereas the combined resistance risk of QNs showed medium risk level (0.1sum ≤ 1). In terms of seasonal variation, RQ sum showed a downward trend. Overall, the ecological risk and resistance risk of QNs in soil for Shijiazhuang City require further attention, and the risk control of antibiotics in soil should be strengthened in the future.

Quinolone (QN) antibiotics are a kind of broad-spectrum antibiotics commonly used in the treatment of human and animal diseases. They have the characteristics of strong antibacterial activity, stable metabolism, low production cost, and no cross-resistance with other antibacterial drugs. They are widely used in the world. QN antibiotics cannot be completely digested and absorbed in organisms and are often excreted in urine and feces in the form of original drugs or metabolites, which are widely occurring in surface water, groundwater, aquaculture wastewater, sewage treatment plants, sediments, and soil environment, thus causing environmental pollution. In this paper, the pollution status, biological toxicity, and removal methods of QN antibiotics at home and abroad were reviewed. Literature data showed that QNs and its metabolites had serious ecotoxicity. Meanwhile, the spread of drug resistance induced by continuous emission of QNs should not be ignored. In addition, adsorption, chemical oxidation, photocatalysis, and microbial removal of QNs are often affected by a variety of experimental conditions, and the removal is not complete, so it is necessary to combine a variety of processes to efficiently remove QNs in the future., (© 2023. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)

The accumulation of antibiotics in farmland and its ecological risk have become a research hotspot at home and abroad. The objective of this study was to investigate the occurrence and accumulation of antibiotics and their potential environmental and ecological risks in vegetable fields in Kaizhou district of Chongqing country. The occurrence characteristics of antibiotics including tetracyclines, sulfonamides, quinolones, macrolides, and chloramphenicols were detected using experimental analysis. The results showed that there was an accumulation of antibiotics in the vegetable soil, and 18 antibiotics in five categories were detected (0-42.88 μg·kg -1 ), mainly for tetracyclines and quinolones. The detection rate of quinolone antibiotics was the highest (15.38%-100%), especially for norfloxacin and ofloxacin (100%), whereas the tetracyclines presented the highest concentration (0-42.88 μg·kg -1 ). The amount of total antibiotics in the vegetable soil was 1.64-233.11 μg·kg -1 , whereas different vegetable soils showed the following trend:water spinach soil (89.73 μg·kg -1 )>cabbage soil (32.53 μg·kg -1 )>pepper soil (32.16 μg·kg -1 )>tomato soil (32.13 μg·kg -1 )>cucumber soil (26.46 μg·kg -1 )>grassland (7.32 μg·kg -1 ). The correlation results showed that there was a significantly positive correlation between total antibiotic residues and organic fertilizer application ( P <0.05) but a significantly negative correlation with soil pH ( P <0.05). Quinolones and sulfonamides were negatively correlated with soil water content ( P <0.05), whereas quinolones positively correlated with soil available phosphorus and organic matter content ( P <0.05). The potential eco-environmental risk assessment results showed that tetracyclines and quinolones in vegetable soil in Kaizhou district had certain ecological risks, of which 62%-92% and 62%-100% of soil samples with quinolones had potential toxicity to soil animals and microorganisms.

Quinolone antibiotics (QNs) pollution in lake environments is increasingly raising public concern due to their potential combined toxicity and associated risks. However, the spatiotemporal distribution and trophodynamics of QNs in transit-station lakes for water diversion are not well documented or understood. In this study, a comprehensive investigation of QNs in water, sediment, and aquatic fauna, including norfloxacin (NOR), ciprofloxacin (CIP), enrofloxacin (ENR), and ofloxacin (OFL), was conducted in Luoma Lake, a major transit station for the eastern route of the South-to-North Water Diversion Project in China. The target QNs were widely distributed in the water (∑QNs: 70.12 ± 62.79 ng/L) and sediment samples (∑QNs: 13.35 ± 10.78 ng/g dw) in both the non-diversion period (NDP) and the diversion period (DP), where NOR and ENR were predominant. All the QNs were detected in all biotic samples in DP (∑QNs: 80.04 ± 20.59 ng/g dw). The concentration of ∑QNs in the water in NDP was significantly higher than those in DP, whereas the concentration in the sediments in NDP was comparable to those in DP. ∑QNs in the water-sediment system exhibited decreasing trends from northwest (NW) to southeast (SE) in both periods; however, the K oc (organic carbon normalized partition coefficients) of individual QNs in DP sharply rose compared with those in NDP, which indicated that water diversion would alter the environmental fate of QNs in Luoma Lake. In DP, all QNs, excluding NOR, were all biodiluted across the food web; whereas their bioaccumulation potentials in the SE subregion were higher than those in the NW subregion, which was in contrast to the spatial distribution of their exposure concentrations. The estimated daily QN intakes via drinking water and aquatic products suggested that residents in the SE side were exposed to greater health risks, despite less aquatic pollution in the region., 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 © 2022. Published by Elsevier Ltd.)

Antibiotics are widely used in daily life, which has created a global scenario where many pathogenic organisms have become effectively resistant to antibiotics. The abuse or overuse of antibiotics causes significant environmental pollution and even endangers human health. It is well-known that antibiotics' efficacy (toxicity) is determined by molecular structure. Therefore, structure-level qualitative analysis with high sensitivity and accuracy is vitally important. Characterized by fingerprinting recognition, Raman spectroscopy, especially surface-enhanced Raman spectroscopy (SERS), has become an essential qualitative analysis tool in various fields, such as environmental monitoring and food safety. With the exception of chirality, this study completed the qualitative trace analysis of 16 quinolone antibiotics (QNs) with fine molecular structure differences using SERS. The sensitivity was tuned in by one order of magnitude through the different electronegativity and steric hindrances of the slightly changed functional groups in the specific antibiotics. The fine structure dependent sensitivity enables SERS to be a powerful on-site monitoring tool to control the abuse of antibiotics with high toxicity; thus, decreasing the subsequent risk to the environmental ecology and human society., (Copyright © 2022. Published by Elsevier B.V.)

The widespread use of quinolones in humans and animals has become a major threat to public health. In this study, a simple, rapid, sensitive, and high throughput method based on automatic solid-phase extraction and isotope dilution ultra-performance liquid chromatography tandem mass spectrometry was described for the determination of trace quinolones in environmental water. The proposed automated solid-phase extraction method was initially optimized, and the optimum experimental conditions found were 1 L water sample with 0.5 g/L Na 2 EDTA (pH 3) extracted and enriched by CNW Poly-Sery HLB cartridge at a flow rate of 50 mL/min and eluted by 8 mL of methanol. The linearity of the method ranged from 0.05 to 100 μg/L for 15 quinolones, with correlation coefficients ranging from 0.9993 to 0.9999. The limits of detection were in the low ng/L level, ranging from 0.005 to 0.051 ng/L. Finally, the optimized method was applied for determining trace levels of 15 quinolones in Wahaha pure water, tap water, river water, and seawater samples with good recoveries of 93 %-119 % and satisfactory relative standard deviations of 0.1 %-13.9 %. Fourteen quinolones were detected, and ofloxacin was the predominant congener in river water and seawater., 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 © 2022 Elsevier B.V. All rights reserved.)

River carrying antibiotics from upstream posed serious threats to receiving lake, and plants might had effects on antibiotics. Therefore, samples of waters, sediments and tissues of cultivated and wild Phragmites australis were collected to analyse antibiotics fate and ecological risks (RQs) in Zaozhadian Lake. Our results revealed that the total antibiotics showed an increasing tendency in surface/pore water and P. australis tissues and a decreasing tendency in overlying water and sediments from the lake entrance to the centre. The bioaccumulation factors (BAFs) of two sulfonamides (SAs) and three quinolones (QNs) increased in sediments and decreased in those of erythromycin in pore water from Site 1 to Site 11. Three QNs and two tetracyclines (TCs) were dominant antibiotics in pore water/sediment and surface/overlying water respectively. Higher levels of two SAs in surface/pore water and two macrolides (MAs) in overlying/pore water and sediments were observed in the wild P. australis region, while higher values of two TCs in overlying/pore water and three QNs in sediment were observed in the cultivated P. australis region. Higher BAFs of SAs and QNs in sediments were observed in the cultivated and wild P. australis region respectively. The RQs of oxytetracycline and two MAs posed moderate risks in surface/overlying water from more than 50% of sampling sites. Norfloxacin exhibited moderate RQ and low ∑RQ levels in sediments, and showed high risk in pore water. Our findings imply that much more attention should be given to the antibiotics from river inputs and management normatives to control antibiotic pollution., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

The presence of unauthorized substances, such as residues of veterinary medicines or chemical contaminants, in food can represent a possible health concern. For this reason, a complete legislative framework has been established in the European Union (EU), which defines the maximum limits allowed in food and carries out surveillance programs to control the presence of these substances. Official food control laboratories, in order to ensure a high level of consumer protection, must respond to the challenge of improving and harmonizing the performance of the analytical methods used for the analysis of residues of authorized, unauthorized, or prohibited pharmacologically active substances. Laboratories must also consider the state of the art of the analytical methodologies and the performance requirements of current legislation. The aim of this work was to develop a multiresidue method for the determination of antibiotics in milk, compliant with the criteria and procedures established by Commission Implementing Regulation (EU) 2021/808. The method uses an LC-Orbitrap-HRMS for the determination of 57 molecules of antibiotic and active antibacterial substances belonging to different chemical classes (beta-lactams, tetracyclines, sulfonamides, quinolones, pleuromutilins, macrolides, and lincosamides) in bovine, ovine, and goat milk samples. It provides a simple and quick sample pretreatment and a subsequent identification phase of analytes, at concentrations equal to or lower than the maximum residual limit (MRL), in compliance with Commission Regulation (EU) 2010/37. The validation parameters: selectivity, stability, applicability, and detection capability (ccβ), are in agreement with the requirements of Commission Implementing Regulation (EU) 2021/808 and demonstrated the effectiveness of the method in detecting veterinary drug residues at the target screening concentration (at the MRL level or below), with a false positive rate of less than 5%. This method represents an effective solution for detecting antibiotics in milk, which can be successfully applied in routine analyses for official food control plans.

Sediment is the main storage medium of antibiotics in a water environment, and a growing body of research has focused on the distribution behavior of antibiotics in water-sediment. However, most of the previous studies were based on laboratory simulation, and less attention was paid to the distribution behavior of antibiotics in a natural water environment and its correlation with environmental factors. Thus, the surface water and sediment in Shijiazhuang were taken as the research object for this study. The temporal and spatial distribution characteristics of quinolone (QNs) antibiotics in Shijiazhuang water were analyzed by using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS), calculating the distribution coefficients of quinolone (QNs) antibiotics in water and sediment, and confirming the main environmental factors influencing the distribution coefficient in natural water. The results showed that:① the content of ΣQNs in water and sediment ranged from 8.0 to 4.4×10 3 ng·L -1 and 16 to 2.2×10 3 ng·g -1 in Shijiazhuang water, whereas the primary QNs in water and sediment were enrofloxacin (ENR) and ofloxacin (OFL), respectively. ② The total concentrations of ΣQNs in Shijiazhuang water showed a tendency of being higher in December (1.0×10 4 ng·L -1 ) than in April (5.5×10 3 ng·L -1 ), and QNs in sediment were also higher in December (7.8×10 3 ng·g -1 ) than in April (6.2×10 3 ng·g -1 ). ③ The distribution coefficient of QNs in Shijiazhuang water varied from 34 to 2.9×10 5 L·kg -1 and showed a trend of being greater in December than in April. ④ The results of correlation analysis showed that total nitrogen (TN), nitrate nitrogen (NO 3 - -N), nitrite nitrogen (NO 2 - -N), and ammonia nitrogen (NH 4 + -N) were significantly correlated with most distribution coefficients of QNs[OFL, norfloxacin (NOR), ENR, difloxacin (DIF), and oxolinic acid (OXO)], whereas temperature ( T ), total organic carbon (TOC), and total dissolved solids (TDS) were significantly correlated with individual distribution coefficients of QNs[marbofloxacin (MAR) and DIF]. Therefore, the eutrophication level of water affects the distribution behavior of antibiotics in water-sediment.

Most studies on antibiotics in groundwater have focused on pollution characteristics, whereas less attention has been paid to the ecological risks of antibiotics and the correlation to environmental parameters. In this study, the groundwater in Shijiazhuang City was selected as the research area. Through high performance liquid chromatography-tandem mass spectrometry (HPLC-MS), the concentration of quinolones (QNs) in the groundwater was analyzed. Correlation analysis was conducted between QNs concentrations and physical-chemical parameters. The results showed that:① the detection frequency of flumequine (FLU) was the highest (100%), followed by enoxacin (ENO) (80.0%) and ciprofloxacin (CIP) (75.0%). ② The concentration of QNs ranged from 3.02 to 98.5 ng·L -1 ; in terms of spatial distribution, the highest concentration of QNs appeared at S4 (98.5 ng·L -1 ), whereas the lowest concentration was exhibited at S19 (3.02 ng·L -1 ). ③ Temperature ( T ), chemical oxygen demand (COD), total dissolved solids (TDS), total number of colonies (BCTC), and pH were significantly correlated with QNs ( P <0.01 or P <0.05) based on correlation analysis. ④ For the spatial distribution of ecological risk, the results showed that the ecological risk at S4 was high, whereas the risks for other sites were low. For the type of QNs, ciprofloxacin (CIP) was at a medium-high risk level, whereas the other QNs were at a low-risk level. Thus, in order to guarantee the ecological safety of groundwater in Shijiazhuang City, more attention should be paid to the risk management and control of antibiotics in groundwater in the future.

The multiclass determination of antibiotic residues in the soil is challenging because of its complex physicochemical properties. In this study, a simple analytical method was developed to simultaneously extract and determine 58 antibiotics from the soil. A novel acidity-regulated extraction-partition-concentration protocol was established for the simultaneous extraction of five classes (23 sulfonamides, 18 quinolones, five tetracyclines, eight macrolides, and four chloramphenicols) of antibiotics from the soil. Compared to traditional methods, the sample preparation efficiency was significantly improved by four times (45 min vs. 230 min) by optimizing the extraction method and omitting the time-consuming solid-phase extraction (SPE) procedure. The ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was optimized to determine the 58 antibiotics in a single run by applying positive/negative switching acquisition mode in less than 10 min with the baseline separation of sulfameter and sulfamethoxypyridazine. Suitable recoveries, ranging between 60 and 120%, were obtained for most antibiotics, with RSD <20%. The limits of quantification (LOQ) of the method were 2 μg/kg and 5 μg/kg. Thus, this study provides a simple, reliable, and economical method for accurately and rapidly determining a multiclass of antibiotics in the soil., (© 2022. Springer-Verlag GmbH Germany, part of Springer Nature.)

A quantitative multi-class multi-residue analytical method was developed for the determination of veterinary drugs in milk by high-performance liquid chromatography - tandem mass spectrometry (HPLC-MS/MS). A total of 132 veterinary drugs investigated belonged to almost 15 classes including sulfonamides, β-lactams, tetracyclines, quinolones, macrolides, nitrofurans, nitroimidazoles, phenicols, lincosamides, pleuromutilins, macrocyclic lactones, quinoxaline antibiotics, benzimidazoles, anthelmintics, coccidiostats and some others. A magnetic solid-phase extraction procedure was developed using magnetic hypercrosslinked polystyrene (HCP/Fe 3 O 4 ) for the sample preparation prior to HPLC-MS/MS without deproteinization step. The results indicated recoveries of 85-107% for 14 sulfonamides, 85-120% for 13 β-lactams, 89-115% for 4 tetracyclines, 82-119% for 14 quinolones, 82-115% for 8 macrolides, 97-109% for 4 nitrofurans, 84-115% for 10 nitroimidazoles, 89-114% for 3 phenicols, 86-111% for 3 lincosamides, 97-102% for 2 pleuromutilins, 72-88% for 4 macrocyclic lactones, 87-104% for 4 quinoxaline antibiotics, 76-119% for 21 benzimidazoles, 79-115% for 12 anthelmintics, 81-118% for 12 coccidiostats and 75-119 % for 5 unclassified drugs, with relative standard deviations (RSDs) of less than 20%, and the LOQs ranged from 0.05 to 1 μg kg -1 . This methodology was then applied to field-collected real milk samples and trace levels of some veterinary drugs were detected., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

The fruit of Tetradium ruticarpum (TR) is commonly used in Chinese herbal medicine and it has known antiproliferative and antitumor activities, which can serve as a good source of functional ingredients. Although some antiproliferative compounds are reported to be present in TR fruit, most studies only focused on a limited range of metabolites. Therefore, in this study, the antiproliferative activity of different extracts of TR fruit was examined, and the potentially antiproliferative compounds were highlighted by applying an untargeted liquid chromatography-tandem mass spectrometry (LC-MS/MS)-based multi-informative molecular networking strategy. The results showed that among different extracts of TR fruit, the EtOAc fraction F2-3 possessed the most potent antiproliferative activity against HL-60, T24, and LX-2 human cell lines. Through computational tool-aided structure prediction and integrating various data (sample taxonomy, antiproliferative activity, and compound identity) into a molecular network, a total of 11 indole alkaloids and 47 types of quinolone alkaloids were successfully annotated and visualized into three targeted bioactive molecular families. Within these families, up to 25 types of quinolone alkaloids were found that were previously unreported in TR fruit. Four indole alkaloids and five types of quinolone alkaloids were targeted as potentially antiproliferative compounds in the EtOAc fraction F2-3, and three (evodiamine, dehydroevodiamine, and schinifoline) of these targeted alkaloids can serve as marker compounds of F2-3. Evodiamine was verified to be one of the major antiproliferative compounds, and its structural analogues discovered in the molecular network were found to be promising antitumor agents. These results exemplify the application of an LC-MS/MS-based multi-informative molecular networking strategy in the discovery and annotation of bioactive compounds from complex mixtures of potential functional food ingredients.

Objective: To investigate the dietary exposure of Ningbo residents to quinolones and tetracyclines antibiotics in animal derived foods, so as to estimate the health risk caused by the exposure., Methods: Animal derived foods in Ningbo markets from 2018 to 2020 were collected and analyzed by ultra-fast liquid chromatography-tandem mass spectrometry. Based on the result of the measurements, median(M), P97.5, average and the maximum values of the data were obtained. Coupling the food intake data of residents in Zhejiang Province, an international point estimate model was applied to evaluate the health risk caused by the dietary exposure., Results: Enrofloxacin, ciprofloxacin, ofloxacin, doxycycline, oxytetracycline were detected in freshwater fishes, cultured pseudosciaena crocea, freshwater shrimps, chicken, eggs and pork. The detection rates of enrofloxacin, ciprofloxacin, ofloxacin, doxycycline, oxytetracycline were 21.2%(77/363), 11.6%(42/363), 2.8%(10/363), 1.4%(5/363), 0.6%(2/363), respectively. The dietary exposure of adults and children from animal derived foods were in the range of 0.8-909.0 and 0.6-518.9 ng/(kg·d), respectively. The hazard quotient(HQ) values were in the range of 0.000030-0.17., Conclusion: Quinolone and tetracycline antibiotics such as enrofloxacin and oxytetracycline have no dietary health risk to the population.

A simple and efficient pH-mediated dispersive solid phase extraction (dSPE) based on terbium doped titanium dioxide nanoparticles (TiO 2 -Tb NPs) combined with high performance liquid chromatography (HPLC) has been firstly developed for the determination of quinolones (QNs) in various biological samples. The adsorption kinetics and isotherms were investigated to indicate that the kinetic and equilibrium adsorption were well-described by pseudo-second order kinetic and Henry, Langmuir isotherm model, respectively. The parameters influencing the extraction performance were systematically investigated. The QNs are transferred into TiO 2 -Tb NPs in the first step at pH = 6.0 and eluted into acidic aqueous phase at pH = 2.5 in the second step. Under the optimum extraction and determination conditions, a linearity range with the coefficient of determination ( R 2 ) from 0.9977 to 0.9991 were obtained in a range of 10-10,000 ng mL -1 . The limits of detection (LODs) based on a signal-to-noise ratio of 3 were 3.3 ng mL -1 . The recoveries of the three QNs in human urine, rabbit plasma and serum samples ranged from 69.3% to 117.6%, with standard deviations ranging from 2.4% to 9.9%. Therefore, this pH-mediated dSPE-HPLC method exhibited the advantages of remarkable sensitivity, ease of operation, rapidity, low cost and environmental friendliness.

Brexpiprazole (BRX) is approved for the treatment of schizophrenia and major depressive disorders and it is mainly metabolized by CYP3A4 and CYP2D6. Grapefruit juice (GFJ), pomegranate juice (PJ) and tomato juice (TJ) have the potential to inhibit CYP3A4 enzymes in the body. However, fruit juice-drug interactions between BRX and GFJ, PJ and TJ have not been studied extensively. The present study describes the influence of GFJ, PJ and TJ on the pharmacokinetic parameters of BRX in rats. The study samples were analyzed using a mass-accurate and single-step bioanalytical method by ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry over a wide calibration range of 20-1,500 ng/ml. The results of the pharmacokinetic study denoted that the combined administration of GFJ and PJ could increase systemic exposure of BRX. The area under the curve of BRX increased 3.43- and 1.88-fold with co-administration of GFJ and PJ, respectively, while TJ with BRX had no effect on the area under the curve. Time to peak concentration and half-life were not significantly changed by any juice co-administration. The results show that GFJ and PJ affect the pharmacokinetic profile of BRX and hence advice needs to be given to patients., (© 2021 John Wiley & Sons, Ltd.)

In this study, well-defined core-shell ethylenediamine-functional magnetic ferroferric oxide polymers were prepared and were fully characterized by transmission electron microscopy, scanning electron microscopy, FTIR spectroscopy, and vibrating sample magnetometry. Then, it was used as a magnetic solid-phase extraction adsorbent for simultaneous determination of 11 trace quinolone residues in freshwater fish samples coupled to liquid chromatography-tandem mass spectrometry. The obtained results revealed that the adsorbent showed good extraction efficiency and the adsorption mechanisms referred to hydrogen bond and π-π stacking interaction. Moreover, the magnetic solid-phase extraction conditions were also carefully optimized. The limits of quantitation of 11 quinolones were in the range of 0.15-0.36 μg/kg, while spiking recoveries were in the range of 80.2-99.5% for the 11 quinolones in freshwater fish samples at four spiked levels including limits of quantitation, 1.0, 40.0, and 80.0 μg/kg with the relative standard deviations ranging from 0.8 to 9.1%. The proposed method was applied to analyze 45 freshwater fish samples, and enrofloxacin was detected in 91.1% samples with concentrations ranging from 0.659 to 333 μg/kg. It could be concluded that the proposed method is fast, simple, sensitive, and accurate for the routine monitor of freshwater fish., (© 2021 Ningbo municipal center for disease control and prevention. Journal of Separation Science published by Wiley-VCH GmbH.)

The widespread use of quinolones has become an increasing global public health threat. In this study, IRMOF-3 coated SiO 2 /Fe 3 O 4 were prepared via a facile room-temperature method. The prepared IRMOF-3 coated SiO 2 /Fe 3 O 4 was used as a sorbent for magnetic solid phase extraction, and then combined with high-performance liquid chromatography-tandem mass spectrometry for the determination of 10 quinolines. The extraction conditions of magnetic solid phase extraction were studied in detail, and the optimal conditions were established. Under the optimal experimental conditions, the limits of quantification of 10 quinolones were in the range of 0.005-0.01 μg L -1 , the relative standard deviations were 6.58-10.6% (n=7), the enrichment factors were 21.0-23.8 for water samples. The limits of quantification of 10 quinolones were in the range of 0.10-0.20 μg kg -1 , the relative standard deviations were 5.95-14.5% (n=7), the enrichment factors were 1.08-1.24 for fish samples. The proposed method was applied for the determination of 10 quinolones in river water, aquacultural water and a fish sample, and enrofloxacin and ciprofloxacin were found in the fish sample., 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 © 2021. Published by Elsevier B.V.)

During infections, fast identification of the microorganisms is critical to improve patient treatment and to better manage antibiotics use. Electrochemistry exhibits several advantages for rapid diagnostic: it enables easy, cheap and in situ analysis of redox molecules in most liquids. In this work, several culture supernatants of different Pseudomonas aeruginosa strains (including PAO1 and its isogenic mutants PAO1ΔpqsA, PA14, PAK and CHA) were analyzed by square wave voltammetry on glassy carbon electrode during the bacterial growth. The obtained voltamograms shown complex traces exhibiting numerous redox peaks with potential repartitions and current amplitudes depending on the studied bacterium and/or growth time. Among them, some peaks were clearly associated to the well-known redox toxin Pyocyanin (PYO) and the autoinducer Pseudomonas Quinolone Signal (PQS). Other peaks were observed that are not yet attributed to known secreted species. Each complex electrochemical response (number of peaks, peak potential and amplitude) can be interpreted as a fingerprint or "ID-card" of the studied strain that may be implemented for fast bacteria strain identification., 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., (Published by Elsevier B.V.)

In this paper, we present a microstructured optofluidic in-fiber Raman sensor for the detection of quinolone antibiotic residue in a water environment based on Ag surface-enhanced Raman scattering (SERS) substrate grown on the surface of the suspended core of micro-hollow optical fiber (MHF). Here, MHF has a special structure with a suspended core and a microchannel inside, which can become a natural in-fiber optofluidic device. Meanwhile, the self-assembled Ag SERS substrate can be grown on the suspended core's surface through chemical bonds, forming a microstructured optofluidic device with a Raman enhancement effect. Therefore, it can effectively detect the Raman signal of unlabeled trace quinolone antibiotic residue (ciprofloxacin and norfloxacin) inside the optical fiber. The results show that the ciprofloxacin and norfloxacin detection limits (LOD) are 10 -10 M and 10 -11 M , respectively. Compared with the maximum residue limit (3.01×10 -7 m o l / L ) stipulated by the European Union, the results are much lower, and an ideal quantitative relationship can be obtained within the detection range. Significantly, this study provides an in-fiber microstructured optofluidic Raman sensor for the label-free detection of quinolone antibiotic residue, which will have good development prospects in the field of antibiotic water pollution environmental detection.

A simple extraction procedure coupled with liquid chromatography-Q Orbitrap high resolution mass spectrometry (LC-Q Orbitrap HRMS) for the determination of 19 quinolones in animal-derived foods (pork, fish, egg and milk) has been developed. Sample preparation is based on homogeneous liquid-liquid extraction at pH > 9 using water-miscible acetonitrile with cold-induced phase separation. The procedure allowed one-step enrichment and cleanup of all the 19 quinolones with different logP properties to lower aqueous phase, which eliminated the process of preconcentration and re-dissolution for sample solution. Furthermore, an adsorption phenomenon was observed between conventional borosilicate glass injection vials and most of quinolones. In detection analysis, a scheduled variable full scan strategy was performed to improve detection performance in Q Orbitrap HRMS. Under optimal conditions, a superior limit of quantitation (0.028-0.192 μg/kg) in animal-derived foods was achieved using this proposed method. Lastly, this method was validated and applied successfully in real samples., 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 © 2021. Published by Elsevier B.V.)

Antibiotic pollution in water has become an increasingly serious problem, posing a potentially huge threat to human health. Ofloxacin (OFL), norfloxacin (NOR), and enoxacin (ENX) are typical broad-spectrum quinolone antibiotics, which are frequently detected in various water environments. An electrochemical sensor is a rapid and effective tool to detect antibiotics in the aquatic environment. The molecular structure of target pollutants is an important factor affecting the detection performance of electrochemical sensors. Based on the electrochemical detection results of antibiotics (OFL, NOR, and ENX), we first used the molecular structure analysis method based on quantum chemistry to accurately identify the electronegativity and the electrocatalytic degree of the oxidizable (and non-oxidizable) functional groups of pollutants. We also clarified the influence mechanism of the molecular structure on the peak current and peak potential. These results can provide theoretical support for rapidly selecting electrodes with a suitable electrochemical window to efficiently detect trace organic pollutants (such as antibiotics) in water based on the molecular structure of the target pollutant.

Antibiotic usage for beekeeping, including quinolones, can lead to residues in honey and these residues usually result from the drugs used in the treatment of American or European foulbrood diseases. Residues in honey may cause allergic reactions as well as increased antibiotic resistance. Within this study, rapid and breakthrough analysis methods were developed using UHPLC-ESI-MS/MS and sample preparation processes were minimised. Practical, low cost, time-effective analysis was provided utilising 'dilute & shoot' methodology and a QuEChERS-based procedure has been developed alternatively for improved sensitivity. Recovery values were 85%-112% for the 'dilute & shoot' method, and 82%-117% for the modified QuEChERS method. For accuracy studies, RSD% values were between 0.7% and 13.4% for both methods in intra-day and inter-day precision studies. CCα (1.1 μg/kg and 0.6 μg/kg) and CCβ (1.2 μg/kg and 0.6 μg/kg) mean values were calculated for the 'dilute & shoot' and QuEChERS method, respectively. These novel methods achieved simultaneous quantification of 21 quinolones in 7 min with high specificity and were used to analyse 50 honey samples. Quinolone residues were found in samples, and enrofloxacin, danofloxacin, pipemidic acid, lomefloxacin, cinoxacin, and ciprofloxacin were quantified.

Anthropogenic activities especially water pollution can affect the diversity and composition of microbial communities and promote the spread of antibiotic resistance genes (ARGs). In this study, water samples and guppies (Poecilia reticulata) were sampled from six sampling sites along the Uberabinha River in southeastern Brazil, both microbial communities and ARGs of surface waters and intestinal microbiota of guppies (Poecilia reticulata) were detected. According to the results of 16S rRNA amplicon sequencing, Proteobacteria, Bacteroidetes, Firmicutes and Actinobacteria were dominant phyla in both water and intestinal microbiota, but the abundance of putative pathogens was higher at heavily polluted sites. Up to 83% of bacteria in intestinal microbiota originated from water microbiota; this proportion was relatively higher in less polluted compared to polluted environments. ARGs providing resistance of tetracyclines and quinolones were dominant in both water and gut microbiota. The relative abundances of class I integrons and ARGs were as high as 1.74 × 10 -1 /16S rRNA copies and 3.61 × 10 -1 /16S rRNA copies, respectively, at heavily polluted sites. Correlation analysis suggests that integrons and bacteria play key roles in explaining the widespread occurrence of ARGs in the surface, but not in intestinal microbiota. We could rule out the class I integrons a potential intermediary bridge for ARGs between both types of microbiomes. Our results highlight the tight link in microbial communities and ARGs between ambient microbiota of stream ecosystems and intestinal microbiota of fish. Our study could have far-reaching consequences for fisheries and consumer safety and calls for investigations of gut microbiota of target species of both commercial fisheries and recreational (hobby) angling., (Copyright © 2021 The Authors. Published by Elsevier Inc. All rights reserved.)

Quality-by-design-based UPLC method was developed for chromatographic separation to quantify the antischizophrenic drug brexpiprazole in the presence of impurities. Research findings from pH-scouting studies were used as control variables which influence the chromatographic separation. The peak tailing and resolution are the response variables and established the design-space by DoE-study for selection of suitable chromatographic conditions. Separation was achieved with lower particle size stationary phase and buffer pH 2.0 in the mobile phase. The present method developed through C18 50 × 2.1 mm, Ethylene-Bridged-Hybrid technology column with 1.7 μm particles, mobile phase consists of pH 2.0 buffer and acetonitrile (67:33 v/v), flow rate of 0.5 mL min-1 and detection wavelength at 215 nm. The retention time of brexpiprazole is 0.6 min and all impurities were eluted within 2 min. The method linearity ranges were 20.4-61.3 μg mL-1 for assay and 0.88-6.59 μg mL-1 for dissolution with correlation-coefficients of 0.9999 and 0.9998 for assay and dissolution, respectively. The recovery values were found in between 99.3 and 100.9%. The method shows stability-indicating on the basis of noninterference of placebo, and impurities from forced-degradation studies. Method validation was carried out according to ICH guideline Q2 (R1)., (© The Author(s) 2020. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.)

Objectives: Quantitative structure activity relationship (QSAR) was used to study the partition coefficient of some quinolones and their derivatives., Methods: These molecules are broad-spectrum antibiotic pharmaceutics. First, data were divided into two categories of train and test (validation) sets using a random selection method. Second, three approaches, including stepwise selection (STS) (forward), genetic algorithm (GA), and simulated annealing (SA) were used to select the descriptors, to examine the effect feature selection methods. To find the relation between descriptors and partition coefficient, multiple linear regression (MLR), principal component regression (PCR) and partial least squares (PLS) were used., Results: QSAR study showed that both regression and descriptor selection methods have a vital role in the results. Different statistical metrics showed that the MLR-SA approach with (r2=0.96, q2=0.91, pred&#95;r2=0.95) gives the best outcome., Conclusion: The proposed expression by the MLR-SA approach can be used in the better design of novel quinolones and their derivatives., (Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.net.)

A simple, rapid and sensitive screening method by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the identification of 7 macrolides (clarithromycin, erythromycin, oleandomycin, spiramycin, tilmicosin, troleandomycin and tylosin) and 8 quinolones (ciprofloxacin, difloxacin, enrofloxacin, flumequine, moxifloxacin, nalidixic acid, norfloxacin and ofloxacin) in meat and egg-based baby foods. Sample preparation was performed using an alkaline modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) extraction method without additional clean-up steps. A simplex-lattice mixture experimental design was used in the optimization of the QuEChERS extraction solvent. The developed method was successfully validated according to the Commission Decision 2002/657/EC and the European Community Reference Laboratories Residues Guidelines regarding the validation of screening methods 20/01/2010, adopting a fixed permited tolerance for relative ion ratio. Samples of baby food (n = 44) commercialized in Rio de Janeiro, Brazil, were analyzed using the validated method and none of them presented residues of the searched macrolides and quinolones, with a screening target value of 5 µg kg -1 .

Quorum sensing (QS) is the ability of some bacteria to detect and to respond to population density through signalling molecules. QS molecules are involved in motility and cell aggregation mechanisms in diseases such as sepsis. Few biomarkers are currently available to diagnose sepsis, especially in high-risk conditions. The aim of this study was the development of new analytical methods based on liquid chromatography-mass spectrometry for the detection and quantification of QS signalling molecules, including N-acyl homoserine lactones (AHL) and hydroxyquinolones (HQ), in biofluids. Biological samples used in the study were Pseudomonas aeruginosa bacterial cultures and plasma from patients with sepsis. We developed two MS analytical methods, based on neutral loss (NL) and product ion (PI) experiments, to identify and characterize unknown AHL and HQ molecules. We then established a multiple-reaction-monitoring (MRM) method to quantify specific QS compounds. We validated the HPLC-MS-based approaches (MRM-NL-PI), and data were in accord with the validation guidelines. With the NL and PI MS-based methods, we identified and characterized 3 and 13 unknown AHL and HQ compounds, respectively, in biological samples. One of the newly found AHL molecules was C12-AHL, first quantified in Pseudomonas aeruginosa bacterial cultures. The MRM quantitation of analytes in plasma from patients with sepsis confirmed the analytical ability of MRM for the quantification of virulence factors during sepsis. Graphical abstract.

In recent years, quinolone antibiotics (QNs), which easily bioaccumulate in aquatic organisms, have been widely detected in lake ecosystems, and the bioaccumulation and trophic transfer behavior are obviously spatiotemporally different. In this study, the bioaccumulation and trophic transfer behavior of fourteen QNs in nine dominant fish species were studied, the correlation with environmental factors was analyzed, and the health risk of QNs was evaluated in Baiyangdian Lake. The results showed that the mass concentrations of ∑QNs in water varied from 0.7400 to 1590 ng·L -1 . Furthermore, the detected frequencies of flumequine (FLU), oxolinic acid (OXO), and ofloxacin (OFL) were higher, and the average mass concentration of FLU was the highest. The content of ∑QNs in fish ranged from 17.1 to 146 ng·g -1 , and the average contents of ciprofloxacin (CIP) and OFL were higher. The bioaccumulation factors (BAF) were in the range of 96.2 (BAF MAR )-489 (BAF CIP ) L·kg -1 , indicating the bioaccumulation of QNs was low in dominant fish species. The trophic magnification factors (TMF) of five QNs (enrofloxacin (ENR), FLU, marbofloxacin (MAR), norfloxacin (NOR), and OFL) varied from 0.714 (TMF MAR ) to 1.33 (TMF ENR ), indicating ENR exhibited trophic magnification, while FLU, MAR, and ∑QNs exhibited trophic dilution. The results of correlation analysis between environmental parameters and BAF/TMF showed that pH, T , SD, DO, COD, TP, TN, NH 4 + -N, NO 3 - -N, and PO 4 3- -P were significantly related to the bioaccumulation of QNs in fish. The results of human health risk showed that the hazard quotient (HQ) of CIP (0.0040-0.026) was significantly higher than that of other QNs (≤ 0.0050), and the hazard indices (HI) ranged from 0.0010 to 0.035, indicating a high level of health risk. Therefore, to reduce the health risk, the standard and residue limits of QNs should be set in Baiyangdian Lake.

Segmental hair analysis provides information regarding previous long-term drug exposure, which is useful in the evaluation of cause of death for individuals with mental disorders. The aim was to analyze postmortem concentrations of the antipsychotic drug aripiprazole and its active metabolite dehydroaripiprazole in hair segments from individuals with known aripiprazole intake. Hair samples were collected during autopsy. Each sample was segmented into one to six 1cm segments, depending on the length of the hair shaft. Pulverized hair was extracted and analyzed using a previously published ultra-high-performance liquid chromatography-tandem mass spectrometric method. The 10th-90th percentile of aripiprazole concentrations in all hair segments (n=78) from 17 individuals were 0.024ng/mg-11ng/mg with a median of 2.3ng/mg, and the 10th-90th percentile concentrations of dehydroaripiprazole were 0.020ng/mg-11ng/mg, with a median of 2.6ng/mg, in all hair segments (n=71). The metabolite-to-parent drug ratios ranged from 0.21 to 1.5, with a median of 0.72. The administered doses were calculated for each individual based on aripiprazole prescription data and pharmacy pickups, giving dose estimates of 1mg-32mg daily. A positive significant correlation was observed between concentrations in hair and blood, whereas no trends were observed between the concentrations in hair and the estimated doses. Besides aripiprazole, other antipsychotic drugs were found in several hair segments, indicating a high degree of polypharmacy among all subjects. The present study establishes concentrations of aripiprazole and dehydroaripiprazole in hair segments from 17 deceased individuals with long-term aripiprazole use. In addition, hair analysis demonstrates the possibility of evaluating polypharmacy., (Copyright © 2020 Elsevier B.V. All rights reserved.)

A new HPLC method was developed for the enantio-separation and chiral recognition mechanism of quinolones (lomefloxacine, ofloxacine, primaquine and quinacrine) on Vancomycin CSP. The column used was Chirabiotic V column (150 × 4.6 mm, 5.0 μm) with two mobile phases i.e. (I) MeOH:ACN:H 2 O:TEA (50:30:20:0.1%) and (II) MeOH:ACN: H 2 O:TEA (70:10:20:0.1%) at 1.0 mL/minute flow rate with various UV detection. The values of retention, separation and resolution factors in a solvent system I were ranged from 2.20 to 5.05, 1.70 to 1.96 and 1.75 to 2.20 while these values were 1.93 to 6.85, 1.62 & 2.01 and 2.30 & 2.40 in solvent system II. The limits of detection and quantification were ranged from 8.0 to 10.5 µg and 24.4 to 33.5 µg. The resolution was controlled mainly by π-π interactions along with other forces like hydrogen bonding, van der Waal's forces, steric effects, etc. The determination of the chiral recognition mechanism may be beneficial to separate other racemates successfully. The method is fast precise and efficient and may be utilized to analyze enantiomers of the reported quinolones., 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 © 2020 Elsevier B.V. All rights reserved.)

The residual antibiotics in the environment have lately caused widespread concerns. However, little information is available on the antibiotic bioaccumulation and its health risk in drinking water resources of South China. Therefore, the occurrence, distribution, and health risk of four quinolone antibiotics including ofloxacin (OFX), norfloxacin (NOR), ciprofloxacin (CIP), and enrofloxacin (ENR) in the Qingshitan reservoir using high-performance liquid chromatography were investigated. Results revealed that the concentrations in water, sediment, and edible fish ranged from 3.49-660.13 ng/L, 1.03-722.18 μg/kg, and 6.73-968.66 μg/kg, respectively. The ecological risk assessment via the risk quotient (RQ) method showed that the values in sediment were all greater than 1, posing a high risk to the environment. The health risk index of water samples was at the maximum acceptable level, with OFX at the top while the rest were at the medium risk level. The main edible fish kinds of the reservoir had high dietary safety and the highest contaminations were found in carnivorous feeding habits and demersal habitat fishes with OFX as the highest magnitude. Source identification and correlation analysis using SPSS showed significant relationships between NOR with pH and turbidity (in water), as well as total phosphor (TP) and total organic carbon (TOC) in sediment. NOR was the highest in sediment which mostly sourced from livestock wastewater, croplands irrigation drain water, and stormwater. Correlations between CIP and ENR with TP were significant, while OFX was positively associated with total nitrogen (TN) which mainly originated from urban sewage as well as directly dosed drugs in fish farms. In conclusion, our results are of great significance for ensuring the safety of drinking water and aquatic products in this region.

Thirty-nine kinds of antibiotics (11 quinolones, 10 tetracyclines, and 18 sulphonamides) residues were screened in 146 samples including chicken, chicken giblets, and eggs in Fujian by ultra-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) and analysed the contamination status of antibiotic residues.seventeen kinds of antibiotics were detected, with an overall detection rate of 47.3% and the exceeding rate was 11.6%. Antibiotics were found in 46.7% chicken, 72.2% chicken giblets, and 30% eggs. In 11.1% of chicken giblets and 26% of eggs, the detected concentration exceeded the maximum residue level (MRLs). The total detection rate of tetracycline antibiotics was higher than that of quinolones (33.6% vs. 24.7%) and the sulphonamides (33.6% vs. 4.8%). The exceeding rates of tetracyclines, quinolones, and sulphonamides were 2.7%, 10.3%, and 1.4%, respectively. We suggested that the abuse of antibiotics in poultry foods still exists, and more attention should be paid to the antibiotic residues in poultry eggs.

Bivalves, such as freshwater clams ( Corbicula fluminea ) and hard clams ( Meretrix lusoria ), are the most extensive and widely grown shellfish in land-based ponds in Taiwan. However, few studies have examined the contamination of bivalves by quinolone and organophosphorus insecticides. Thus, we adapted an established procedure to analyze 8 quinolones and 12 organophosphorus insecticides using liquid and gas chromatography-tandem mass spectrometry. Surveys in Taiwan have not noted high residual levels of these chemicals in bivalve tissues. A total of 58 samples of freshwater or hard clams were obtained from Taiwanese aquafarms. We identified 0.03 mg/kg of enrofloxacin in one freshwater clam, 0.024 mg/kg of flumequine in one freshwater clam, 0.02 mg/kg of flumequine in one hard clam, 0.05 mg/kg of chlorpyrifos in one freshwater clam, 0.03 mg/kg of chlorpyrifos in one hard clam, and 0.02 mg/kg of trichlorfon in one hard clam. The results indicated that 5.17% of the samples had quinolone insecticide residues and 5.17% had organophosphorus residues. However, the estimated daily intake (EDI)/acceptable daily intake quotient (ADI) indicated no significant risk and no immediate health risk from the consumption of bivalves. These results provide a reference for the food-safety screening of veterinary drugs and pesticides in aquatic animals. Aquatic products should be frequently screened for residues of prohibited chemicals to safeguard human health.

Fluorescent sensors are a vital research tool, enabling the study of intricate cellular processes in a sensitive manner. The design and synthesis of responsive and targeted probes is necessary to allow such processes to be interrogated in the cellular environment. This remains a challenge, and requires methods for functionalisation of fluorophores with multiple appendages for sensing and targeting groups. Methods to synthesise more structurally complex derivatives of fluorophores will expand their potential scope. Most known 4-amino-1,8-naphthalimides are only functionalised at imide and 4-positions, and structural modifications at additional positions will increase the breadth of their utility as responsive sensors. In this work, methods for the incorporation of a hypoxia sensing group to 4-amino-1,8-naphthalimide were evaluated. An intermediate was developed that allowed us to incorporate a sensing group, targeting group, and ICT donor to the naphthalimide core in a modular fashion. Synthetic strategies for attaching the hypoxia sensing group and how they affected the fluorescence of the naphthalimide were evaluated by photophysical characterisation and time-dependent density functional theory. An extracellular hypoxia probe was then rationally designed that could selectively image the hypoxic and necrotic region of tumour spheroids. Our results demonstrate the versatility of the naphthalimide scaffold and expand its utility. This approach to probe design will enable the flexible, efficient generation of selective, targeted fluorescent sensors for various biological purposes., (© 2020 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.)