RESUMO
The global surge in pharmaceutical consumption, driven by increasing population and the demand for animal proteins, leads to the discharge of diverse pollutants, including antibiotic residues, into water bodies. Sulfonamides, being water-soluble compounds, can readily enter surface run-off, posing potential risks to non-target species despite their low environmental concentrations. Latin America has implemented intensive production systems highly dependent on antimicrobials for productivity and animal health, yet there is a paucity of information regarding their concentration in the region. The objective of this study was to evaluate the presence of sulfonamides in water and sediment samples and assess their potential ecological risks through an environmental risk assessment. The Río de la Plata basin collects the waters of the Paraguay, Paraná, and Uruguay rivers, together with their tributaries and various wetlands, passing through the provinces in Argentina known for their significant animal husbandry production. Two sampling campaigns were carried out for sediment, while only one campaign was conducted for surface waters. The samples were analyzed by high performance liquid chromatography tandem mass-spectrometry (HPLC-MS/MS). None of the examined sulfonamide antibiotics were detected in the sediment samples from both sampling campaigns. In contrast, sulfadiazine (95 %), sulfamethoxazole (91 %), and sulfathiazole (73 %) were detected in the water samples. Sulfadiazine was found in the concentration range of 8 to 128 ng/L, while sulfamethoxazole and sulfathiazole were observed at concentrations ranging from 3.0 to 32.5 ng/L and 2.9 to 8.1 ng/L, respectively. Based on the environmental risk assessment conducted using the sulfonamide concentrations, most samples indicated a medium risk for aquatic biota, with only one sample surpassing the high-risk threshold. This study represents the first report presenting data on the presence of sulfonamide antibiotics in the aquatic environment of Argentina.
Assuntos
Monitoramento Ambiental , Sulfonamidas , Poluentes Químicos da Água , Argentina , Medição de Risco , Poluentes Químicos da Água/análise , Sulfonamidas/análise , Antibacterianos/análise , Rios/química , Sedimentos Geológicos/química , Espectrometria de Massas em TandemRESUMO
The extensive occurrence of antibiotics in farmland soil might threaten food safety. The bioaccumulation potential of antibiotics in edible vegetables and crops grown under realistic farming scenarios was reviewed and the human health risk was assessed. A total of 51 antibiotics were documented in 37 species of daily consumed crops. Among different classes of antibiotics, tetracyclines (TCs) exhibited higher residue levels in plants than quinolones (QNs), sulfonamides (SAs), and macrolides (MLs), with median values ranging from 5.10 to 15.4 µg/kg dry weight. The favored accumulation of TCs in plants was probably linked to their relatively higher residual concentrations in soils and greater bioconcentration factors. Compared with the plants grown in open field, accumulation of antibiotics was higher in plant grown under greenhouse condition, probably due to the higher residue levels of antibiotics in the greenhouse soil with intensive application of manure. Cocktails of antibiotics were investigated in potato, corn, carrot, tomato, lettuce, and wheat. Among them, corn exhibited relatively high median concentrations of antibiotics (0.400-203 µg/kg dry weight). Antibiotics tended to accumulate in plant root and their concentrations in fruit were generally low. Risk assessment revealed that human health risk was under the alert line through the daily consumption of antibiotic contaminated vegetables and food crops.
Assuntos
Quinolonas , Poluentes do Solo , Humanos , Antibacterianos/análise , Poluentes do Solo/análise , Esterco , Plantas Comestíveis , Fazendas , Solo/química , Verduras/química , Produtos Agrícolas , Tetraciclinas/análise , Macrolídeos , Medição de Risco , Sulfonamidas/análiseRESUMO
In this study, an analytical method based on isotope dilution-liquid chromatography tandem mass spectrometry (ID-LC-MS/MS) was developed as a candidate reference method for the determination of sulfonamides (SAs) in honey. To guarantee the accuracy and authenticity, the impact of hydrolysis on bound SA residues was first investigated by enabling (i) identification of sugar-bound SAs, (ii) clarifying the binding reaction rule between the SAs and sugar, (iii) detection of free SAs and sugar-bound SAs, and (iv) preparation of SA-contaminated honey. Thus, the efficiency of different hydrolysis conditions was assessed by comparing the bound SA content before and after hydrolysis. In addition, optimization of the sample pretreatment procedures and LC conditions to minimize matrix effects by separation from significant matrix interferences was also performed. Satisfactory results in terms of hydrolysis efficiency (approximately 88.3%-99.2%), extraction efficiency (84.2%-105.3%), recovery (95.9%-103.1%), and limit of quantification (0.6-1.5 µg·kg-1) were obtained.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Análise de Alimentos/métodos , Mel/análise , Sulfonamidas/análise , Espectrometria de Massas em Tandem/métodos , Hidrólise , Técnicas de Diluição do Indicador , Isótopos , Reprodutibilidade dos Testes , Sulfonamidas/químicaRESUMO
BACKGROUND: Sulfonamides have been widely used in the prevention and clinical treatment of bacterial diseases in livestock and poultry. The use of sulfonamides increases the risk of veterinary drug residues in animal derived foods. The traditional reversed phase liquid chromatography methods for sulfonamides residues detection in animal derived foods have the problem of high consumption of organic solvents. OBJECTIVE: The aim of this study was to establish a green high-performance liquid chromatography method for the detection of sulfonamides residues in different animal-origin foods. METHOD: The sample extraction solutions were purified by the Agela Cleanert PEP-2 cartridge and analyzed by the high-performance liquid chromatography method using ethanol as the green alternative solvent. RESULTS: The proposed method was validated in terms of linear range (20-1000 µg/kg), limit of detection (3.0-12.3 µg/kg), limit of quantitation (10-43 µg/kg), accuracy (80.7-101.3%), and repeatability and reproducibility (RSD <5.9% and RSD <8.5% respectively). CONCLUSIONS: The proposed method is an environmentally friendly, sensitive and reliable high-performance liquid chromatography method for simultaneous determination of sulfonamide residues in animal-origin foods. HIGHLIGHTS: In this work, we firstly developed a green high-performance liquid chromatography method for simultaneous determination of the residues of nine sulfonamides in milk and beef with ethanol as the green alternative solvent.
Assuntos
Resíduos de Drogas , Leite , Animais , Bovinos , Cromatografia Líquida de Alta Pressão , Leite/química , Reprodutibilidade dos Testes , Sulfonamidas/análiseRESUMO
The pesticide residues in agri-foods are threatening people's health. This study aims to establish a fast and low-cost surface-enhanced Raman scattering (SERS) method for the on-site detection of flumetsulam in wheat. The two-step modified concentrated gold nanoparticles (AuNPs) acted as the SERS substrate with the aid of NaCl and MgSO4. NaCl is served as the activator to modify AuNPs, while MgSO4 is served as the aggregating agent to form high-density hot spots. The activation and aggregation are two essential collaborative procedures to generate remarkable SERS enhancement and achieve the trace-level detection of flumetsulam. This method exhibits good enhancement effect with an enhancement factor of 106 and wide linear range (5-1000 µg/L). With simple pretreatment, the flumetsulam residue in real wheat samples can be successfully detected with the limit of detection (LOD) down to 0.01 µg/g, which is below the maximum residue limit of flumetsulam in wheat (0.05 µg/g) set in China. The recovery of flumetsulam residue in wheat ranges from 88.3% to 95.6%. These results demonstrate that the proposed SERS method is a powerful technique for the detection of flumetsulam in wheat, which implies the great application potential in the rapid detection of other pesticide residues in various agri-foods.
Assuntos
Contaminação de Alimentos/análise , Nanopartículas Metálicas/química , Pirimidinas/análise , Análise Espectral Raman/métodos , Sulfonamidas/análise , Triticum/química , Análise de Alimentos/instrumentação , Análise de Alimentos/métodos , Ouro/química , Limite de Detecção , Microscopia Eletrônica de Varredura , Tamanho da Partícula , Resíduos de Praguicidas/análise , Espectrofotometria Ultravioleta , Análise Espectral Raman/instrumentação , Sulfatos/químicaRESUMO
Manure, soil, and vegetable samples were collected from different-sized livestock farms in Xinxiang, China. The residues of sulfadiazine, sulfamonomethoxine, and sulfamethoxazole were analyzed by high-performance liquid chromatography. The results indicated that the concentration ranges of the three total sulfonamides in manure, soil, and vegetables were 10.13-566.23 µg kg-1, 7.60-176.26 µg kg-1, and 0-32.70 µg kg-1, respectively. The mean concentrations were 219.71 µg kg-1, 70.73 µg kg-1, and 7.08 µg kg-1 for manure, soil, and vegetables, respectively. The mean concentrations in soil were lower than the ecotoxic effect trigger value (100 µg kg-1), indicating a low risk for organisms in soil. The concentrations of the three sulfonamides varied significantly in different types of vegetables and all were lower than the acceptable daily intake value (50 µg (kg day)-1). However, the potential ecotoxicity and danger to human and animal health via accumulation of the antibiotic in the food chain cannot be ignored.
Assuntos
Antibacterianos/análise , Gado , Esterco/análise , Poluentes do Solo/análise , Solo/química , Sulfonamidas/análise , Verduras/química , Animais , China , Cromatografia Líquida de Alta Pressão , Medição de RiscoRESUMO
A method for simultaneous quantitation of rimsulfuron, quizalofop-P-ethyl and quizalofop-P in potato plant, soil and potato tuber samples was established. The mean recoveries of rimsulfuron, quizalofop-P-ethyl and quizalofop-P in different matrices spiked with them were 81.4%-101.1%, 76.1%-99.0% and 77.4%-106.4% with relative standard deviations (RSDs) of 2.7%-13.3%, 0.9%-5.5%, 1.7%-11.3%, respectively. The open-field trials in China were conducted in potato cultivation system of Changchun and Jinan. The results indicated that the half-lives of rimsulfuron and quizalofop-P-ethyl were 0.04-13.1 days. The residues of quizalofop-P during the harvest time in Jinan soil were < 0.01-0.044 mg kg-1, while there was no residue of target herbicides detected in all other samples. The risk assessment results demonstrated that the risk quotients (RQs) of rimsulfuron and quizalofop-P-ethyl were 7.857 × 10-5 and 8.730 × 10-3, respectively, which exhibited an acceptable dietary risk to Chinese consumers.
Assuntos
Resíduos de Praguicidas/análise , Propionatos/análise , Piridinas/análise , Quinoxalinas/análise , Poluentes do Solo/análise , Sulfonamidas/análise , China , Herbicidas/análise , Medição de Risco , Solo/química , Solanum tuberosumRESUMO
In this study, the degradation of Nimesulide (NIM), a non-steroidal anti-inflammatory drug, using photolysis, heterogeneous (TiO2 in dispersion) and homogeneous (photo-Fenton reactant) photocatalysis, under simulated solar light (SSL) radiation, was investigated. Various parameters affecting the degradation rate of the target compound during the applied processes were optimized. The efficiency of all treatments used (direct photolysis; TiΟ2/SSL; TiΟ2/Η2Ο2/SSL; TiΟ2/S2Ο82-/SSL; Fe3+/H2O2/SSL; Fe3+/S2O82-/SSL and [Fe(C2O4)3]3-/H2O2/SSL) was evaluated by means of initial reaction rate and mineralization. Moreover, the generated transformation products (TPs) by each basic process (photolysis; TiΟ2/SSL and Fe3+/H2O2/SSL) were identified, using liquid chromatography coupled to high resolution mass spectrometry, and their formation kinetic profiles were given. The main transformation routes of NIM were hydroxylation and fragmentation, for all three treatments applied. Finally, toxicity measurements were conducted using Microtox bioassay in order to evaluate the potential risk of NIM and its TPs to aqueous organisms. Although, the acute toxicity increased during the first stages of treatment the final outcome lead to very low toxicity levels even within 60â¯min of TiO2/SSL treatment. Concluding, the obtained results suggest that the photocatalytic degradation of NIM can lead to its complete elimination and simultaneously to the detoxification of the solution.
Assuntos
Anti-Inflamatórios não Esteroides/análise , Fotólise , Sulfonamidas/análise , Titânio/química , Eliminação de Resíduos Líquidos/métodos , Águas Residuárias/análise , Aliivibrio fischeri/efeitos dos fármacos , Anti-Inflamatórios não Esteroides/toxicidade , Catálise , Cinética , Sulfonamidas/toxicidade , Luz Solar , Testes de Toxicidade Aguda , Águas Residuárias/toxicidadeRESUMO
Occurrence and distribution of 24 antibiotics from 7 categories were screened in sea cucumbers (Echinodermata: Holothuroidea) collected from different coastal regions of China. The samples were simultaneously extracted and purified using accelerated solvent extraction with in-cell clean-up and analyzed by ultra-performance liquid chromatography-tandem mass spectrometry. A total of ten antibiotics were detected in the sea cucumbers with concentrations ranging from not detected to 32.8 µg/kg (dry weight). Sulfonamides are predominant antibiotics with a mean concentration of 11.5 µg/kg (dry weight), followed by macrolides (11.3 µg/kg, dry weight) and fluoroquinolones (11.2 µg/kg, dry weight). High concentrations of the antibiotics were found in the samples from the South China Sea, implying that the antibiotic pollution in sea cucumbers was geographical region-dependent, which was further confirmed by principal component analysis. It was also found that the antibiotic levels are slightly higher in instant sea cucumbers than in the dried ones. Hazard quotient calculation suggested no obvious human health risks associated with the consumption of sea cucumbers regarding antibiotics.
Assuntos
Antibacterianos/metabolismo , Monitoramento Ambiental , Pepinos-do-Mar/metabolismo , Poluentes Químicos da Água/metabolismo , Animais , Antibacterianos/análise , China , Cromatografia Líquida , Fluoroquinolonas/análise , Humanos , Macrolídeos/análise , Medição de Risco , Sulfonamidas/análiseRESUMO
OBJECTIVES: An alarming rate of emergence of antimicrobial resistance (AMR) globally has urged Bhutan to take firm steps towards antibiotic stewardship through rational use in humans, animals and agriculture. This study aimed to investigate the use of three important antibiotic classes in animal feeds in Bhutan. METHODS: Thirteen samples were selected randomly from a pool of feed samples submitted by bidders for Annual Animal Feed Tender (fiscal year 2015-2016) of the Department of Livestock. The 13 samples were tested for nitrofurans and their metabolites, tetracyclines and sulphonamides. The objectives of the study were to evaluate the feed samples for the presence of three antibiotic classes and, if present, to understand the level of presence (mg/kg) in terms of AMR emergence and spread in a Bhutanese context. RESULTS: Two feed samples, belonging to Indian Feed Agents, tested positive for oxytetracycline at levels of 0.072mg/kg and 0.037mg/kg, respectively. Compared with the Feed Additive Compendium recommended dose (10-50g/ton) of oxytetracycline for poultry, the levels found in these two feeds were low. Samples testing positive for antibiotics were rejected in the bidding procedure as being medicated at prophylactic levels and could be the cause of emergence and spread of AMR in the country. CONCLUSION: Although the samples containing antibiotics were rejected by the Department of Livestock for use in government farms, some farmers may still use medicated feeds. Therefore, more screening needs to be conducted to further confirm and to prevent antibiotic abuse in animal feed in Bhutan.
Assuntos
Ração Animal/análise , Antibacterianos/análise , Contaminação de Alimentos/análise , Nitrofuranos/análise , Sulfonamidas/análise , Tetraciclina/análise , Ração Animal/economia , Animais , Butão , Contaminação de Alimentos/economia , Índia , Nitrofuranos/economia , Aves Domésticas , Sulfonamidas/economia , Tetraciclina/economiaRESUMO
BACKGROUND: Dofetilide is an effective antiarrhythmic medication for rhythm control in atrial fibrillation, but carries a significant risk of pro-arrhythmia and requires meticulous dosing and monitoring. The cornerstone of this monitoring, measurement of the QT/QTc interval, is an imperfect surrogate for plasma concentration, efficacy, and risk of pro-arrhythmic potential. OBJECTIVE: The aim of our study was to test the application of a deep learning approach (using a convolutional neural network) to assess morphological changes on the surface ECG (beyond the QT interval) in relation to dofetilide plasma concentrations. METHODS: We obtained publically available serial ECGs and plasma drug concentrations from 42 healthy subjects who received dofetilide or placebo in a placebo-controlled cross-over randomized controlled clinical trial. Three replicate 10-s ECGs were extracted at predefined time-points with simultaneous measurement of dofetilide plasma concentration We developed a deep learning algorithm to predict dofetilide plasma concentration in 30 subjects and then tested the model in the remaining 12 subjects. We compared the deep leaning approach to a linear model based only on QTc. RESULTS: Fourty two healthy subjects (21 females, 21 males) were studied with a mean age of 26.9 ± 5.5 years. A linear model of the QTc correlated reasonably well with dofetilide drug levels (r = 0.64). The best correlation to dofetilide level was achieved with the deep learning model (r = 0.85). CONCLUSION: This proof of concept study suggests that artificial intelligence (deep learning/neural network) applied to the surface ECG is superior to analysis of the QT interval alone in predicting plasma dofetilide concentration.
Assuntos
Eletrocardiografia/métodos , Fenetilaminas/análise , Sulfonamidas/análise , Adulto , Antiarrítmicos/uso terapêutico , Biomarcadores Farmacológicos , Estudos Cross-Over , Aprendizado Profundo , Eletrocardiografia/efeitos dos fármacos , Eletrocardiografia/estatística & dados numéricos , Feminino , Humanos , Aprendizado de Máquina , Masculino , Redes Neurais de Computação , Fenetilaminas/efeitos adversos , Fenetilaminas/sangue , Estudo de Prova de Conceito , Sulfonamidas/efeitos adversos , Sulfonamidas/sangue , Adulto JovemRESUMO
Thirteen antibiotics including sulfonamides (SAs), tetracyclines (TETs) and fluoroquinolones (FQs) were measured in Hanjiang River (HR) during two periods. The total concentrations of 13 antibiotics in surface water and sediments ranged from 3.1 to 109â¯ng/l and from 10 to 45â¯ng/g dry weight, respectively. SAs were dominant in water while the concentrations of TETs were the highest in sediments in two seasons. For their spatial distribution, total concentrations of 13 antibiotics in both matrices were significantly higher in the lower section of HR (pâ¯<â¯0.02, Fâ¯>â¯5.15) due to wastewater release, agricultural activities and water transfer project. Obvious seasonal variations of sulfadiazine, sulfameter, trimethoprim and oxytetracycline in water were observed (pâ¯<â¯0.05, Fâ¯>â¯4.62). Phase partition of antibiotics between water and sediments suggested a greater affinity of TETs and FQs to sediments. In addition, significantly positive relationships were found between SAs (sulfameter, sulfamethoxazole and trimethoprim) and sediment TOC (pâ¯<â¯0.05). Risk assessment indicated that the hazard quotients of antibiotics were higher in the sediment than those in the water. Moreover, antibiotic mixtures posed higher ecological risks to aquatic organisms.
Assuntos
Antibacterianos/análise , Rios/química , Poluentes Químicos da Água/análise , Agricultura , Antibacterianos/toxicidade , Organismos Aquáticos , China , Monitoramento Ambiental , Fluoroquinolonas/análise , Sedimentos Geológicos/química , Medição de Risco , Estações do Ano , Sulfonamidas/análise , Tetraciclinas/análise , Águas Residuárias , Poluentes Químicos da Água/toxicidadeRESUMO
Complexity of anthropogenic influences on coastal ecosystems necessitates use of an integrated assessment strategy for effective interpretation and subsequent management. In this study a multiple lines of evidence (LOE) approach for sediment assessment, that combined use of chemistry, toxicity, and benthic community structure in the sediment quality triad was used to assess spatiotemporal changes and potential risks of persistent toxic substances (PTSs) in sediments of Masan Bay highlighting "long-term changes" between 1998 and 2014. Specific target objectives encompassed sedimentary PTSs (PAHs, alkylphenols (APs), and styrene oligomers), potential aryl hydrocarbon receptor (AhR; H4IIE-luc assay)- and estrogen receptor (ER; MVLN assay)-mediated activities, and finally several ecological quality (EcoQ) indices of benthic community structure. Concentrations of target PTSs in Masan Bay sediments were generally less by half in 2014 compared to those measured in 1998. Second, AhR-mediated potencies in sediments also decreased during this time interval, whereas ER-mediated potencies increased (+3790%), indicating that there has been substantial ongoing, input of ER agonists over the past 16 years. Potency balance analysis revealed that only 3% and 22% of the AhR- and ER-mediated potencies could be explained by identified known chemicals, such as PAHs and APs, respectively. This result indicated that non-targeted AhR and ER agonists had a considerable presence in the sediments over time. Third, EcoQ indices tended to reflect PTSs contamination in the region. Finally, ratio-to-mean values obtained from the aforementioned three LOEs indicated that quality of sediments from the outer region of the bay had recovery more during the period of 16-years than did the inner region. Overall, the results showed that even with the progress supported by recent efforts from the Korean governmental pollution control, PTSs remain a threat to local ecosystem, especially in the inner region of Masan Bay.
Assuntos
Monitoramento Ambiental/métodos , Sedimentos Geológicos/química , Poluentes Químicos da Água/análise , Poluição Química da Água/estatística & dados numéricos , Baías/química , Bioensaio/métodos , Nitroimidazóis/análise , Hidrocarbonetos Policíclicos Aromáticos/análise , Receptores de Hidrocarboneto Arílico/agonistas , República da Coreia , Estireno/análise , Sulfonamidas/análiseRESUMO
Benzothiazole (BTHs), benzotriazole (BTRs) and benzenesulfonamide (BSAs) derivates are high production volume chemicals and they are used in several industrial and household applications, therefore it is expected their occurrence in various environments, especially water and air. In this study we developed a method based on gas chromatography-mass spectrometry (GC-MS) combined with pressurised liquid extraction (PLE) to simultaneously determine four BTR, five BTH and six BSA derivates in the particulate matter (PM10) of outdoor air samples collected in quartz fibre filters (QFFs). To the best of our knowledge, this is the first time these compounds have been determined in open ambient environments. Under optimised conditions, method recoveries at the lower and upper concentration levels (0.8 and 4.2 ng m-3) ranged from 70 to 120%, except for 1-H-benzothiazole and 2-chlorobenzothiazole, which were about 50%. The repeatability of the method was usually below 20% (n = 3, %RSD) for both concentration levels. This method enables the contaminants to be detected at pg m-3 concentration levels. Several samples from two different sites influenced by local industries showed that BTRs, followed by BTHs, were the most detected compounds, whereas BSAs were hardly found. The most frequently determined compounds were 1-H-benzothiazole, 2-chlorobenzothiazole, 1-H-benzotriazole, 2-hydroxibenzothiazole, 5,6-dimethyl-1-H-benzotriazole and the isomers 4- and 5-methyl-1-H-benzotriazole. With the concentrations found, the human exposure assessment and health risk characterization via ambient inhalation were also evaluated taking into account different subpopulation groups classified by age for the two sampling points.
Assuntos
Poluentes Atmosféricos/análise , Benzotiazóis/análise , Exposição Ambiental/análise , Material Particulado/análise , Sulfonamidas/análise , Triazóis/análise , Exposição Ambiental/estatística & dados numéricos , Humanos , BenzenossulfonamidasRESUMO
Vonoprazan fumarate is a novel potassium-competitive acid blocker for the treatment of acid-related diseases. In the present study, a simple, fast, and economic reversed-phase liquid chromatography (LC) method was developed for the analysis of ten related substances (raw materials, by-products and degradants) in vonoprazan fumarate. The optimized separation was performed on a Phenomenex Kinetex EVO C18 (250mm×4.6mm, 5.0µm) column. The mobile phase consisted of (A) 0.03M sodium phosphate buffer (pH adjusted to 6.5) - methanol - acetonitrile (72:25:3, v/v/v) and (B) 0.03M sodium phosphate buffer (pH adjusted to 6.5) - acetonitrile (30:70, v/v). Detection of the analytes was conducted at 230nm using a UV detector. The stability-indicating ability of this method was demonstrated by carrying out forced degradation studies. Vonoprazan underwent significant degradation when subjected to alkaline and oxidative stress conditions, while the drug proved to be stable to acidic, thermal and photolytic degradation. The degradants did not interfere with the detection of vonoprazan fumarate and its impurities. The performance of this method was validated in accordance to the regulatory guidelines recommended by the International Conference on Harmonisation (ICH) and this validation included specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision and robustness. The method proposed in this paper could be applied for process development as well as quality assurance of vonoprazan in bulk drug, since no monograph is available in official compendia.
Assuntos
Contaminação de Medicamentos/prevenção & controle , Fumaratos/análise , Inibidores da Bomba de Prótons/análise , Pirróis/análise , Sulfonamidas/análise , Tecnologia Farmacêutica/métodos , Química Farmacêutica/economia , Química Farmacêutica/instrumentação , Química Farmacêutica/métodos , Cromatografia Líquida de Alta Pressão/economia , Cromatografia Líquida de Alta Pressão/instrumentação , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia de Fase Reversa/economia , Cromatografia de Fase Reversa/instrumentação , Cromatografia de Fase Reversa/métodos , Análise Custo-Benefício , Estabilidade de Medicamentos , Fumaratos/química , Fumaratos/normas , Limite de Detecção , Oxirredução , Inibidores da Bomba de Prótons/química , Inibidores da Bomba de Prótons/normas , Pirróis/química , Pirróis/normas , Controle de Qualidade , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Sulfonamidas/química , Sulfonamidas/normas , Tecnologia Farmacêutica/economia , Tecnologia Farmacêutica/instrumentação , Tecnologia Farmacêutica/normas , Fatores de TempoRESUMO
The occurrence and temporal-spatial distributions of 13 antibiotics (tetracyclines, sulfonamides, and fluoroquinolones) in the water of a high-intensity aquaculture lake, Honghu Lake, and its associated river network and ponds were investigated. Tetracycline, oxytetracycline, chlortetracycline, and sulfadiazine are the four dominant antibiotics in this region, with maximum and median concentrations of 1454.8 and 304.8ng/L, 2796.6 and 161.9ng/L, 1431.3 and 349.9ng/L, and 499.5 and 106.5ng/L, respectively. The median concentrations of the other nine antibiotics are lower than 57.1ng/L. The highest contaminated sites are located in the Four-lake main canal and its lake inlets. Antibiotic concentrations were higher in November than in May and the concentrations were strongly correlated with water temperature, dissolved oxygen, and nitrates according to redundancy analysis. The source analysis indicated that besides untreated domestic and husbandry sewage, the aquaculture in the lake and ponds is a main source of antibiotics in the study region. The environmental hazards posed by the selected antibiotics were assessed by using the methods of hazard quotient and mixture hazard quotient. The results suggested that tetracycline, oxytetracycline, sulfadiazine, and ciprofloxacin pose medium to high ecological hazard to algae in almost all of the water samples, and the high combination ecological hazards of antibiotics are mainly posed by the high individual hazard quotient of tetracycline in the study area.
Assuntos
Antibacterianos/análise , Monitoramento Ambiental , Poluentes Químicos da Água/análise , Aquicultura , China , Ecologia , Lagos/química , Nitratos/análise , Esgotos , Sulfonamidas/análise , Espectrometria de Massas em Tandem , Tetraciclinas/análiseRESUMO
Among the wide range of compounds reaching the soil are the veterinary antimicrobials. Since no regulations regarding acceptable levels of drug concentrations in the environment exist, monitoring tests, particularly concerning soils, are carried out very rarely. This study presents a preliminary assessment of the contamination of agricultural soils in Northern Poland with seven antimicrobial veterinary medicines which has never been carried out before. Veterinary drugs were detected in 54% of the examined soil samples; the most commonly detected drugs were sulfonamides and trimethoprim. The highest indicated concentrations refer to enrofloxacin (57.0 µg kg-1) and trimethoprim (47.8 µg kg-1). The presence of these target drugs in the soil environment confirms the need for further monitoring studies. The analytical methods developed in this study are an excellent tool to achieve this goal and allow an estimation of the risk connected with the presence of veterinary antimicrobials in soils.
Assuntos
Antibacterianos/análise , Monitoramento Ambiental , Poluentes do Solo/análise , Solo/química , Drogas Veterinárias/análise , Cromatografia Líquida , Enrofloxacina , Monitoramento Ambiental/métodos , Fluoroquinolonas/análise , Polônia , Sulfonamidas/análise , Espectrometria de Massas em Tandem/métodos , Trimetoprima/análiseRESUMO
Availability of analytical method which is compatible with both Ultra high performance liquid chromatography (UHPLC) and Liquid chromatography mass spectrometry to identify and quantify the impurities in pharmaceutical products is an advantage for drug product development; such analytical method was developed for Nimesulide using a fused core column. Ammonium acetate and methanol were used as mobile phase in the gradient elution at a detection wavelength 230 nm. Quality-by-design principles helped in identifying the critical method development parameters and design space. Limit of detection and the limit of quantification are 0.025 and 0.075%, respectively. Precision of the method is <0.4% RSD and correlation coefficient is >0.999 for Nimesulide and all related substances. Accuracy of Nimesulide ranged from 99.3 to 100.4% at assay concentration. Application of this method in stability analysis has been demonstrated by analyzing stressed samples. The method was validated for specificity, linearity, accuracy, precision and robustness in compliance with International Conference on Harmonization (ICH) Q2(R1). This is the first reported UHPLC method for the estimation of Nimesulide and its related substances. According to ICH M7 guidelines, all impurities were assessed for genotoxicity, LD50, skin sensitization, irritation potential and carcinogenicity using Derek and TOPKAT software. Combined knowledge of analytical and toxicology assessment will help in developing safe and quality product.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Simulação por Computador , Sulfonamidas , Animais , Contaminação de Medicamentos , Humanos , Limite de Detecção , Modelos Lineares , Espectrometria de Massas/métodos , Relação Quantitativa Estrutura-Atividade , Ratos , Reprodutibilidade dos Testes , Testes de Irritação da Pele , Software , Sulfonamidas/análise , Sulfonamidas/química , Sulfonamidas/toxicidadeRESUMO
We evaluated the occurrence and distribution of 12 antibiotics from the sulfonamide (SAs), fluoroquinolone (FQs) and tetracycline (TCs) groups in the Weihe River, North China. The total antibiotic concentrations in surface water, pore water, and sediment samples ranged from 11.1 to 173.1 ng/L, 5.8 to 103.9 ng/L, and 9.5 to 153.4 µg/kg, respectively. The values of the sediment-water partitioning coefficient in the Weihe River varied widely, from not detected to 943, 2213, and 2405 L/kg for SAs, FQs, and TCs, respectively. The values of the partitioning coefficients between sediment and surface water were generally lower than those between sediment and pore water, which indicated ongoing inputs to the water. The risk assessment showed that there were relatively high ecological risks to aquatic algae in this area from sulfamethoxazole, norfloxacin, tetracycline, ofloxacin, and ciprofloxacin.
Assuntos
Fluoroquinolonas/análise , Sedimentos Geológicos/química , Rios/química , Sulfonamidas/análise , Tetraciclinas/análise , Antibacterianos/análise , China , Monitoramento Ambiental , Medição de Risco , Água , Poluentes Químicos da Água/análiseRESUMO
Cyazofamid, as a fungicide of the novel cyanoimidazole chemical class, has been widely used to control tomato late blight. Understanding of cyazofamid residues in environment and crops is an essential prerequisite for its risk assessment. In this study, field investigations in four typical tomato-producing areas were conducted to explore the dissipation kinetics and residues of cyazofamid and its primary metabolite 4-chloro-5-p-tolylimidazole-2-carbonitrile (CCIM) in soil and tomato. A robust method using QuEChERS coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for simultaneous analysis of cyazofamid and CCIM, with limits of quantification of 0.33 and 3.8 µg/kg, respectively. Field trials showed that the half-lives of cyazofamid were 3.6-6.9 days in soil and 12.2-18.3 days in tomato. The total residues of cyazofamid and CCIM in tomato collected at three time intervals were all below 0.5 mg/kg. Moreover, the potential risks of total residues via tomato intake to ten population subgroups were evaluated. We found that the risk quotient values were all generally low (0.13-1.3%), indicating that the recommended dose of cyazofamid on tomato will not result in a consumer exposure exceeding the toxicological reference value. Here, the results of field investigation provided important information for further understanding the behavior and risk of cyazofamid in the natural environment.