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1.
J Environ Manage ; 323: 116148, 2022 Dec 01.
Artículo en Inglés | MEDLINE | ID: mdl-36088761

RESUMEN

Biochar (BP) obtained from palm fiber wastes was combined with H2O2, peroxymonosulfate (PMS), or persulfate (PDS) to treat valsartan, acetaminophen, and cephalexin in water. BP activated PMS and PDS but no H2O2. Computational calculations indicated that interactions of PMS and PDS with BP are more favored than those with HP. The highest synergistic effect was obtained for the removal of valsartan by BP + PMS. This carbocatalytic process was optimized, evaluating the effects of pH, BP dose, and peroxymonosulfate concentration, and minimizing the oxidant quantity to decrease costs and environmental impacts of the process. SO4•-, HO•, 1O2, and O2•- were the agents involved in the degradation of the pharmaceuticals. The reusability of BP was tested, showing that the carbocatalytic process removed ∼80% of target pollutants after 120 min of treatment even at the fourth reuse cycle. Also, the process decreased the phytotoxicity of the treated sample. Simulated hospital wastewater was treated and its components induced competing effects, but the system achieved the target pharmaceuticals removal in this matrix. Additionally, the analysis of environmental impact using a life cycle assessment unraveled that the carbocatalytic process had a carbon footprint of 2.87 Kg CO2-Eq, with the biochar preparation (which involves the use of ZnCl2 and electric energy consumption) as the main hotspot in the process.


Asunto(s)
Oxidantes , Contaminantes Químicos del Agua , Acetaminofén , Dióxido de Carbono/análisis , Cefalexina/análisis , Carbón Orgánico , Peróxidos , Preparaciones Farmacéuticas , Valsartán/análisis , Aguas Residuales/análisis , Agua/análisis , Contaminantes Químicos del Agua/análisis
2.
Ultrason Sonochem ; 79: 105777, 2021 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-34649167

RESUMEN

Cephalexin (CPX) and doxycycline (DOX) are two of the most used antibiotics to treat bacterial infections in human medicine, veterinary practices, animal husbandry, agriculture, aquaculture, among others. Nevertheless, due to their excessive consumption and incomplete absorption during their metabolization, they have been detected in different environmental matrices and the effluents of wastewater treatment plants, which reflects that conventional water treatment methods are not enough to eliminate this type of compounds. This paper presents the main results about the removal of the antibiotics CPX and DOX under low frequency (40 kHz) ultrasonic radiation (US). The effects of operational parameters such as the solution initial pH and the applied US power were assessed considering the response surface methodology and a face centered, central composite experimental design. The results indicated that evaluated operational factors significantly affect the pollutants elimination and that US technology is able to remove them completely. In addition, in terms of mineralization, experimental results showed a reduction of the organic carbon present in the solutions and a significant increase of ions (nitrates and sulfates) concentration, suggesting that part of the organic matter was transformed into CO2, H2O and inorganic species. Finally, results regarding the samples toxicity indicated that ultrasonic treatment could promote a significant reduction in this parameter, and the potential negative effect associated to CPX and DOX presence in water bodies.


Asunto(s)
Ultrasonido , Antibacterianos , Cefalexina/análisis , Doxiciclina , Humanos , Contaminantes Químicos del Agua/análisis , Purificación del Agua
3.
Molecules ; 26(11)2021 Jun 02.
Artículo en Inglés | MEDLINE | ID: mdl-34199337

RESUMEN

This study aimed to understand the adsorption process of cephalexin (CPX) from aqueous solution by a biochar produced from the fiber residue of palm oil. Scanning electron microscopy, Fourier transform infrared spectroscopy, Boehm titration, and the point of zero charge were used to characterize the morphology and surface functional groups of the adsorbent. Batch tests were carried out to evaluate the effects of the solution pH, temperature, and antibiotic structure. The adsorption behavior followed the Langmuir model and pseudo-second-order model with a maximum CPX adsorption capacity of 57.47 mg g-1. Tests on the thermodynamic behavior suggested that chemisorption occurs with an activation energy of 91.6 kJ mol-1 through a spontaneous endothermic process. Electrostatic interactions and hydrogen bonding represent the most likely adsorption mechanisms, although π-π interactions also appear to contribute. Finally, the CPX removal efficiency of the adsorbent was evaluated for synthetic matrices of municipal wastewater and urine. Promising results were obtained, indicating that this adsorbent can potentially be applied to purifying wastewater that contains trace antibiotics.


Asunto(s)
Cefalexina/análisis , Aceite de Palma/química , Contaminantes Químicos del Agua/análisis , Adsorción , Carbón Orgánico/química , Concentración de Iones de Hidrógeno , Microscopía Electrónica de Rastreo , Espectroscopía Infrarroja por Transformada de Fourier , Temperatura , Purificación del Agua
4.
Ecotoxicol Environ Saf ; 201: 110739, 2020 Sep 15.
Artículo en Inglés | MEDLINE | ID: mdl-32505047

RESUMEN

In the study, antibiotic resistance genes (ARGs) were examined in wastewater and sludge samples to explore the effect of cephalexin (CFX) on the spreading and removal of ARGs in the Expanded Granular Sludge Bed (EGSB) reactor treating antibiotics wastewater. The result showed that the addition of CFX in the wastewater affected the removal amount of ß-lactam ARGs and other types ARGs. Besides, the addition of CFX in the wastewater had no obviously effect on total concentration of targeted ARGs in the sludge, but it was related to the accumulation of some typical ARGs. Based on gene cassette array libraries analysis, the diversity of gene cassettes carried by intI1 gene was increased by the addition of CFX in the wastewater. Furthermore, the co-occurrence patterns between ARGs and bacterial genus were also investigated. The results showed the CFX in the wastewater not only affected the number of potential host bacteria of ARGs, but also changed the types of potential host bacteria of ARGs. The correlation analysis of ARG in influent, effluent and sludge showed that, for blaCTX-M, sul2, qnrS and AmpC genes, their removal amount in EGSB reactor treating antibiotic wastewater system might be enhanced by reducing their concentration in the sludge.


Asunto(s)
Antibacterianos/farmacología , Cefalexina/farmacología , Farmacorresistencia Microbiana/efectos de los fármacos , Eliminación de Residuos Líquidos/métodos , Aguas Residuales/microbiología , Antibacterianos/análisis , Bacterias/efectos de los fármacos , Bacterias/genética , Bacterias/crecimiento & desarrollo , Bacterias/aislamiento & purificación , Cefalexina/análisis , Farmacorresistencia Microbiana/genética , Genes Bacterianos/efectos de los fármacos , Aguas del Alcantarillado/química , Aguas del Alcantarillado/microbiología , Aguas Residuales/química
5.
Mikrochim Acta ; 187(1): 40, 2019 12 11.
Artículo en Inglés | MEDLINE | ID: mdl-31828439

RESUMEN

The authors have synthesized a phosphorescent probe of type SiO2-QD-MIP, where QD stands for Mn:ZnS quantum dots and MIP is a polymer coating that was molecularly imprinted with cephalexin. The nanoprobe with high specificity was prepared via sol-gel polymerization using thioglycolic acid (TGA)-modified QDs as luminescent materials, cephalexin as the template, 3-aminopropyltriethoxysilane as the functional monomer, and tetraethoxysilane as the crosslinking agent. The SiO2-QD-MIPs were characterized by X-ray powder diffraction, transmission electron microscopy, scanning electron microscopy, and Fourier transform infrared spectrometry. The orange emission of the probe, with excitation/emission maxima at 295/590 nm, decreases linearly in the 2.5-50 µg·L-1 cephalexin concentration range with a limit of detection (LOD) of 0.81 µg·L-1. The nanoprobe was successfully applied to the determination of cephalexin in (spiked) raw milk and milk powder. The recoveries ranged from 91.7 to 103.7%.


Asunto(s)
Cefalexina/análisis , Sustancias Luminiscentes/química , Impresión Molecular , Polímeros/química , Puntos Cuánticos/química , Tioglicolatos/química , Sustancias Luminiscentes/síntesis química , Manganeso/química , Estructura Molecular , Tamaño de la Partícula , Porosidad , Sulfuros/química , Propiedades de Superficie , Compuestos de Zinc/química
6.
Artículo en Inglés | MEDLINE | ID: mdl-31233944

RESUMEN

An ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed to analyze cephalexin in swine tissues, urine, and feces. Samples were extracted with 1% sulfuric acid, followed by purification using MCX cartridges. Mean recoveries were 95.4%-100.7% with inter-day relative standard deviations of <8.6%. The quantitation limit was 5 µg/kg for fat and urine, and 10 µg/kg for muscle, liver, kidney, and feces. Cephalexin residue depletion was determined using 32 healthy pigs, randomly divided into eight (seven treated and one control) groups. Treated groups were intramuscularly administered 10 mg/kg b.w. five times at 24-h intervals and euthanized 6 h and 1, 2, 3, 5, 7, and 10 days after the last injection. Cephalexin was eliminated rapidly in swine muscle, liver, fat, and feces. The highest concentrations among edible organs were detected in the kidney. Moreover, the longest elimination period of cephalexin in swine was determined in urine. These results indicated that kidney and urine were likely target matrices for cephalexin residue detection in swine.


Asunto(s)
Antibacterianos/análisis , Cefalexina/análisis , Cromatografía Líquida de Alta Presión/métodos , Residuos de Medicamentos/análisis , Espectrometría de Masas en Tándem/métodos , Animales , Antibacterianos/orina , Cefalexina/orina , Grasas/química , Heces/química , Riñón/química , Hígado/química , Músculos/química , Porcinos
7.
J Pharm Biomed Anal ; 166: 421-434, 2019 Mar 20.
Artículo en Inglés | MEDLINE | ID: mdl-30716654

RESUMEN

A highly sensitive, selective and precise HPTLC method coupled with fluorescence detection was developed and validated for the determination of α-aminocephalosporin antibiotics; namely cefalexin, cefadroxil and cefradine in their standard solutions. The applicability of the developed methodology was demonstrated via analysis of cefalexin in goat milk samples. Full optimization of the fluorescence derivatization reaction was carried out with regard to the standard solutions of the studied compounds or after extraction of milk samples. The separation of the studied compounds was performed on HPTLC precoated silica gel plates 60 F254 using acetonitrile: water in a ratio 85:15 (v/v) as a mobile phase. The retention behavior of the formed derivatives was discussed in detail. It was found that hydrophilic interaction mode is the main interaction mechanism governing the retention of the formed derivatives. In addition, an experimental design approach was conducted for optimization of the chromatographic conditions. Modified QuEChERS was applied as an efficient extraction technique of cefalexin from both spiked and real goat milk samples. Optimization of QuEChERS extraction technique to achieve the highest extraction recovery was performed and the results indicate that this method provides a good extraction recovery (83-116%) for cefalexin from goat milk samples. Limit of detection (LOD) of the developed method was found to be 0.023, 0.005, and 0.023 ng band-1 for cefalexin, cefadroxil and cefradine, respectively in their standard solutions and 0.165 ng band-1 for cefalexin in goat milk samples. According to the achieved LOD values, the method sensitivity was quasi-equivalent to other methods based on expensive techniques such as HPLC-UV and HPLC-MS and it is sufficient to determine cefalexin below its MRL in milk samples. Moreover, the method was successfully applied to a pharmacokinetic study of cefalexin in goat milk after single intramuscular injection of 10 mg of cefalexin kg-1 per body weight.


Asunto(s)
Antibacterianos/análisis , Cefalexina/análisis , Cabras , Leche/química , Drogas Veterinarias/análisis , Animales , Antibacterianos/administración & dosificación , Antibacterianos/farmacocinética , Cefalexina/administración & dosificación , Cefalexina/farmacocinética , Cromatografía Liquida , Interacciones Hidrofóbicas e Hidrofílicas , Inyecciones Intramusculares , Límite de Detección , Extracción en Fase Sólida , Drogas Veterinarias/administración & dosificación , Drogas Veterinarias/farmacocinética
8.
Sci Total Environ ; 648: 377-387, 2019 Jan 15.
Artículo en Inglés | MEDLINE | ID: mdl-30121037

RESUMEN

The elimination of cephalexin (CPX) using electro-generated Cl2-active on Ti/RuO2-IrO2 anode was assessed in different effluents: deionized water (DW), municipal wastewater (MWW) and urine. Single Ti/RuO2 and Ti/IrO2 catalysts were prepared to compare their morphologies and electrochemical behavior against the binary DSA. XRD and profile refinement suggest that Ti/RuO2-IrO2 forms a solid solution, where RuO2 and IrO2 growths are oriented by the TiO2 substrate through substitution of Ir by Ru atoms within its rutile-type structure. SEM reveals mud-cracked structures with flat areas for all catalysts, while EDS analysis indicates atomic ratios in the range of the oxide stoichiometries in the nominal concentrations used during synthesis. A considerably higher CPX degradation is achieved in the presence of NaCl than in Na2SO4 or Na3PO4 media due to the active chlorine generation. A faster CPX degradation is reached when the current density is increased or the pH value is lowered. This last behavior may be ascribed to an acid-catalyzed reaction between HClO and CPX. Degradation rates of 22.5, 3.96, and 0.576 µmol L-1 min-1 were observed for DW, MWW and urine, respectively. The lower efficiency measured in these last two effluents was related to the presence of organic matter and urea in the matrix. A degradation pathway is proposed based on HPLC-DAD and HPLC-MS analysis, indicating the fast formation (5 min) of CPX-(S)-sulfoxide and CPX-(R)-sulfoxide, generated due the Cl2-active attack at the CPX thioether. Furthermore, antimicrobial activity elimination of the treated solution is reached once CPX, and the initial by-products are considerably eliminated. Finally, even if only 16% of initial TOC is removed, BOD5 tests prove the ability of electro-generated Cl2-active to transform the antibiotic into biodegradable compounds. A similar strategy can be used for the abatement of other recalcitrant compounds contained in real water matrices such as urine and municipal wastewaters.


Asunto(s)
Cefalexina/análisis , Cloro/química , Iridio/química , Rutenio/química , Eliminación de Residuos Líquidos/métodos , Contaminantes Químicos del Agua/análisis , Antibacterianos/análisis , Electrodos , Aguas Residuales/análisis
9.
J Glob Antimicrob Resist ; 15: 210-211, 2018 12.
Artículo en Inglés | MEDLINE | ID: mdl-30316965

RESUMEN

OBJECTIVES: This study reports the draft genome sequence of Xenophilus sp. E41, a strain resistant to multiple antimicrobials isolated from an activated sludge reactor treating wastewater with a high cephalexin concentration. METHODS: Genomic DNA of Xenophilus sp. E41 was extracted and sequenced using an Illumina NovaSeq 6000 system. The generated sequence reads were assembled using MEGAHIT in combination with SOAPdenovo. Mauve and CompareM were used to align the Xenophilus sp. E41 genome to other draft genomes of the genus Xenophilus in order to determine their evolutionary relationships. The draft genome was annotated using the Rapid Annotation using Subsystem Technology (RAST) server and the nr database, whilst antimicrobial resistance genes (ARGs) were identified using the SARG 2.0 database, RAST server and nr database. RESULTS: Xenophilus sp. E41, with a genome length of 5919552bp, harbours seven types of ARGs involving resistance to ß-lactams, tetracycline, aminoglycosides, sulfonamides, chloramphenicol, teicoplanin and bleomycin. No virulence factors or plasmids were identified. CONCLUSION: The genome sequence reported here will provide useful information for a better understanding of antimicrobial resistance profiles in this strain and the genus Xenophilus.


Asunto(s)
Burkholderiales/genética , Cefalexina/análisis , Genoma Bacteriano , Aguas del Alcantarillado/microbiología , Proteínas Bacterianas/genética , Secuencia de Bases , Reactores Biológicos/microbiología , Burkholderiales/clasificación , Burkholderiales/aislamiento & purificación , Burkholderiales/metabolismo , Cefalexina/metabolismo , Aguas del Alcantarillado/análisis , Aguas Residuales/análisis , Aguas Residuales/microbiología
10.
Ther Drug Monit ; 40(6): 682-692, 2018 12.
Artículo en Inglés | MEDLINE | ID: mdl-30015652

RESUMEN

BACKGROUND: Pharmacokinetic studies and therapeutic drug monitoring of antibiotics require a simple, rapid, and reliable analytical method for monitoring the concentrations in plasma, including unbound concentrations for highly protein-bound drugs. The aim of the current work was to develop and validate a liquid chromatography-tandem mass spectrometry method for the simultaneous determination of total and unbound concentrations of 3 widely used ß-lactam antibiotics (cefalexin, cefazolin, and flucloxacillin) and the often coadministered drug probenecid in human plasma, suitable for pharmacokinetic studies and for routine use in ordinary, busy hospital laboratories. METHODS: Unbound drug was separated from bound drug by ultrafiltration. A simple 1-step protein precipitation was used for sample preparation. Cefalexin, cefazolin, flucloxacillin, probenecid, and their corresponding isotopically labeled internal standards were then resolved on a C18 (2) column. All the compounds were detected using electrospray ionization in the positive mode. RESULTS: Standard curves were linear for all compounds over the concentration range of 0.2-100 mg/L (r > 0.99) for total drug in plasma and 0.01-10 mg/L (r > 0.99) for unbound drug in plasma ultrafiltrate. For both total and unbound drugs, bias was <±10%, and intra- and interday coefficients of variation (imprecision) were <10%. The limit of quantification was 0.2 mg/L for total plasma concentrations and 0.01 mg/L for plasma ultrafiltrate concentrations of all drugs. CONCLUSIONS: The method has proven to be simple, rapid, robust, and reliable and is currently being used in clinical pharmacokinetic studies and in the routine clinical service to enhance the effective use of the ß-lactam antibiotics.


Asunto(s)
Cefazolina/análisis , Cefalexina/análisis , Monitoreo de Drogas/métodos , Floxacilina/análisis , Plasma/química , Probenecid/análisis , Adyuvantes Farmacéuticos/análisis , Adolescente , Adulto , Anciano , Anciano de 80 o más Años , Niño , Cromatografía Líquida de Alta Presión , Humanos , Límite de Detección , Persona de Mediana Edad , Espectrometría de Masas en Tándem/métodos , Adulto Joven , beta-Lactamas/análisis
11.
J Dairy Res ; 85(3): 321-326, 2018 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-29969084

RESUMEN

The purpose of this study was to determine tetracycline and other antimicrobial residues in milk from dairy cows treated for clinical mastitis. Data on cow health and drugs used were obtained from the farm veterinarians. A milk sample from each affected udder quarter of each cow was taken for bacterial identification before treatment. All 35 cows in the study were treated with an intramammary product containing tetracycline, neomycin, bacitracin, and prednisolone (tetracycline injector) and also simultaneously with other drugs via the intramammary or parenteral route. The withhold period of the 'tetracycline product' was eight milkings but, in all cases, longer withhold periods were prescribed due to off-label application of additional combinations of drugs. Milk samples from treated udder quarters, taken two milkings before and two after the prescribed withhold period, were analysed for antimicrobial residues. Additionally, milk samples were taken from untreated healthy udder quarters to check if any crossover of drugs had occurred. Three screening tests were used for antimicrobial detection. In 15 (42·9%) cows the milk samples from the treated infected quarters contained tetracycline residues above the maximum residue limit (MRL) after the prescribed withhold period and, in two cases (5·7%) the same was true for neomycin and cefquinome residues. Cephalexin above the MRL was detected in only one case (2·9%). Beta-lactams did not exceed the MRL after the prescribed withhold period. Antimicrobial residues were not detected in milk samples from untreated quarters. Cow condition including parity, decreased milk production and severity of mastitis significantly influenced the excretion of antimicrobials in milk (P ≤ 0·05). No significant differences were found between the tetracycline positive and tetracycline negative cows regarding the bacteria involved, combination antimicrobial therapy, or treatment interval and duration.


Asunto(s)
Antibacterianos/análisis , Quimioterapia Combinada/veterinaria , Mastitis Bovina/tratamiento farmacológico , Leche/química , Tetraciclina/análisis , Animales , Bovinos , Cefalexina/análisis , Residuos de Medicamentos/análisis , Femenino , Mastitis Bovina/microbiología , Drogas Veterinarias/análisis
12.
Rapid Commun Mass Spectrom ; 32(7): 576-582, 2018 Apr 15.
Artículo en Inglés | MEDLINE | ID: mdl-29397004

RESUMEN

RATIONALE: Cephalosporins (e.g. cephalexin, cefradine) are a major group of widely used ß-lactam antibiotics. Hydrolysis of the ß-lactam ring is an important reaction (often undesired) which leads to deactivation of ß-lactams. To the best of our knowledge there is no electrospray ionization mass spectrometry (ESI-MS) data reported concerning the products of hydrolysis of cephalosporins. METHODS: The hydrolysis of cephalexin and cefradine was performed in aqueous NaOH solutions. After the process the solutions were analyzed by high-performance liquid chromatography (HPLC)/ESI-MS. The elemental compositions of the ions discussed were confirmed by the accurate mass measurements on a quadrupole time-of-flight (QTOF) mass spectrometer. RESULTS: Unexpectedly, complexes between the hydrolysis products of cephalexin and cefradine (CFLh and CFRh ) and iron cation were detected upon HPLC/ESI-MS analysis, namely the ions [(CFLh -H)2 +Fe]+ and [(CFRh -H)2 +Fe]+ , although iron was not added to the analyzed solutions or to the mobile phase. These ions were found to be very stable in the gas phase. CONCLUSIONS: The detection of the complexes between the hydrolysis products of cephalosporins and iron may have a positive impact on the sensitivity and specificity of HPLC/ESI-MS analyses of the hydrolysis products of some cephalosporins.


Asunto(s)
Cefalexina/análisis , Cefradina/análisis , Cromatografía Líquida de Alta Presión/métodos , Compuestos de Hierro/análisis , Espectrometría de Masa por Ionización de Electrospray/métodos , Cefalexina/química , Cefradina/química , Hidrólisis , Compuestos de Hierro/química , Hidróxido de Sodio
13.
Braz. J. Pharm. Sci. (Online) ; 54(3): e17277, 2018. tab, graf
Artículo en Inglés | LILACS | ID: biblio-974420

RESUMEN

The purpose of the study is to develop cephalexin controlled-release matrix tablets by using lower proportions of release retardant polymer and to establish their in vitro & in vivo correlation. Tablets were compressed by incorporating polymers in a matrix form along with drug which prolong the drug release. Twelve formulations were prepared by mixing ethyl cellulose (EC) and hydroxypropyl methylcellulose (HPMC) (three different viscosity grades) in various proportions. F-1 to F-4 formulations were prepared by incorporating drug, HPMC K4M and ethyl cellulose in 100 : 5 : 5, 100 : 10 : 5, 100 : 15 : 5 and 100 : 20 : 5; similarly, F-5 to F-8 were prepared with HPMC K15M; and F-9 to F-12 were prepared with HPMC K100M using a wet granulation process maintained same proportions, along with drug and EC. Tablets were evaluated for their pre-compression and post-compression characteristics and they were found to be in limits. From the dissolution testing, F-4 showed 100.34% medicament release in 12 h. In vivo studies were conducted on rabbit and pharmacokinetic parameters of the optimized formulation were evaluated using HPLC method. It was found that matrix tablets showed increased t1/2 and decreased Kel. The design signified that the drug release rate from tablets was influenced by the small proportion (around 7% of a tablet weight) of polymer mixture and it controlled 100% medicament release upto 12 h effectively with the low grade viscosity of HPMC combination, with good in vitro & in vivo correlation.


Asunto(s)
Comprimidos/análisis , Técnicas In Vitro/instrumentación , Cefalexina/análisis , Polímeros , Cromatografía Líquida de Alta Presión/métodos , Preparaciones de Acción Retardada , Composición de Medicamentos
14.
Chemosphere ; 184: 215-223, 2017 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-28599150

RESUMEN

In order to investigate long-term effect of cefalexin (CFX) on the performance of expanded granular sludge bed (EGSB) system and microbial community structure, two 1.47 L EGSB reactors E1 and E2 were designed and run for 224 days treating with synthetic antibiotic wastewater. For the purpose of comparison, E1 was fed with synthetic antibiotic industry wastewater with CFX added as the test reactor, while, E2 was fed without any CFX added as the control reactor (E2). The addition of CFX resulted in the continual increasing of soluble COD (sCOD) and accumulation of VFAs in the effluent of E1 system. Besides, it was found that the accumulation of CFX by-products D-1, D-2 and D-3 was negative correlation with sCOD removal efficiency. Furthermore, the microbial community structures were also investigated. For the bacterial community, Gelria and Syntrophorhabdus which can ferment propionate and other organic pollutants as their substrate were obviously enriched in E1 system. For the archaea, there was more functional diversity in E1 system than in E2 system. Furthermore, fungi also played an important role on the removal of complex organics in E1 system.


Asunto(s)
Antibacterianos/análisis , Biodegradación Ambiental/efectos de los fármacos , Cefalexina/análisis , Eliminación de Residuos Líquidos/métodos , Antibacterianos/toxicidad , Archaea , Reactores Biológicos/microbiología , Cefalexina/toxicidad , Aguas del Alcantarillado/química , Aguas Residuales , Microbiología del Agua
15.
Anal Bioanal Chem ; 409(17): 4157-4166, 2017 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-28516278

RESUMEN

Although stir bar sportive extraction was thought to be a highly efficiency and simple pretreatment approach, its wide application was limited by low selectivity, short service life, and relatively high cost. In order to improve the performance of the stir bar, molecular imprinted polymers and magnetic carbon nanotubes were combined in the present study. In addition, two monomers were utilized to intensify the selectivity of molecularly imprinted polymers. Fourier transform infrared spectroscopy, scanning electron microscopy, and selectivity experiments showed that the molecularly imprinted polymeric stir bar was successfully prepared. Then micro-extraction based on the obtained stir bar was coupled with HPLC for determination of trace cefaclor and cefalexin in environmental water. This approach had the advantages of stir bar sportive extraction, high selectivity of molecular imprinted polymers, and high sorption efficiency of carbon nanotubes. To utilize this pretreatment approach, pH, extraction time, stirring speed, elution solvent, and elution time were optimized. The LOD and LOQ of cefaclor were found to be 3.5 ng · mL-1 and 12.0 ng · mL-1, respectively; the LOD and LOQ of cefalexin were found to be 3.0 ng · mL-1 and 10.0 ng · mL-1, respectively. The recoveries of cefaclor and cefalexin were 86.5 ~ 98.6%. The within-run precision and between-run precision were acceptable (relative standard deviation <7%). Even when utilized in more than 14 cycles, the performance of the stir bar did not decrease dramatically. This demonstrated that the molecularly imprinted polymeric stir bar based micro-extraction was a convenient, efficient, low-cost, and a specific method for enrichment of cefaclor and cefalexin in environmental samples.


Asunto(s)
Antibacterianos/análisis , Cefaclor/análisis , Cefalexina/análisis , Monitoreo del Ambiente/métodos , Impresión Molecular/métodos , Microextracción en Fase Sólida/métodos , Contaminantes Químicos del Agua/análisis , Adsorción , Antibacterianos/aislamiento & purificación , Cefaclor/aislamiento & purificación , Cefalexina/aislamiento & purificación , Cromatografía Líquida de Alta Presión/métodos , Lagos/análisis , Nanotubos de Carbono/química , Polímeros/química , Agua/análisis , Contaminantes Químicos del Agua/aislamiento & purificación
16.
Chemosphere ; 168: 638-647, 2017 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-27847122

RESUMEN

The contamination of surface and ground water by antibiotics is of significant importance due to their potential chronic toxic effects to the aquatic and human lives. Thus, in this work, the electrochemical oxidation of cephalexin (CEX) was carried out in a one compartment filter-press flow cell using a boron-doped diamond (BDD) electrode as anode. During the electrolysis, the investigated variables were: supporting electrolyte (Na2SO4, NaCl, NaNO3, and Na2CO3) at constant ionic strength (0.1 M), pH (3, 7, 10, and without control), and current density (5, 10 and 20 mA cm-2). The oxidation and mineralization of CEX were assessed by high performance liquid chromatography, coupled to mass spectrometry and total organic carbon. The oxidation process of CEX was dependent on the type of electrolyte and on pH of the solution due to the distinct oxidant species electrogenerated; however, the conversion of CEX and its hydroxylated intermediates to CO2 depends only on their diffusion to the surface of the BDD. In the final stages of electrolysis, an accumulation of recalcitrant oxamic and oxalic carboxylic acids, was detected. Finally, the growth inhibition assay with Escherichia coli cells showed that the toxicity of CEX solution decreased along the electrochemical treatment due to the rupture of the ß-lactam ring of the antibiotic.


Asunto(s)
Cefalexina , Diamante/química , Técnicas Electroquímicas/métodos , Contaminantes Químicos del Agua , Purificación del Agua/métodos , Boro/química , Dióxido de Carbono/análisis , Ácidos Carboxílicos/análisis , Cefalexina/análisis , Cefalexina/toxicidad , Cromatografía Líquida de Alta Presión , Técnicas Electroquímicas/instrumentación , Electrodos , Electrólisis , Escherichia coli/efectos de los fármacos , Oxidación-Reducción , Espectrometría de Masas en Tándem , Contaminantes Químicos del Agua/análisis , Contaminantes Químicos del Agua/toxicidad , Purificación del Agua/instrumentación
17.
Anal Bioanal Chem ; 407(28): 8525-32, 2015 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-26416019

RESUMEN

In this paper we describe the development of a sensitive, fast, and easily performed fluorescence polarization immunoassay for determination of cephalexin in milk. The experimental work was performed to increase sensitivity and specificity. Therefore, the structures of the tracers were varied by synthesis of both cephalexin (CEX) and cephalotin (CET) conjugates with a variety of fluorescent labels. Two rabbit antisera containing antibodies against cephalexin and cephalotin were tested in homologous and heterologous combinations with the tracers. For every working antibody-tracer combination, the analytical conditions and cross-reactivity for structural analogues-cephalosporins and other antibiotics that could also be present in milk-were determined. It was found that the highest sensitivity was achieved by use of the homologous pair CET-EDF-anti-CET antibody (limit of detection (LOD) 0.4 µg kg(-1) for standard solutions prepared in buffer), but this combination was not appropriate because of high cross-reactivity with CET. For subsequent experiments, therefore, CEX- EDF-anti-CEX antibody were chosen (LOD 0.8 µg kg(-1) for standard solutions prepared in buffer). Part of this manuscript is devoted to the variation of precipitation agents for pretreatment of milk before analysis; milk is an extremely complicated matrix. The optimum protein precipitation agent was methanol. This technique for cephalexin determination was characterized by a limit of detection of 1 µg kg(-1). The method was validated by using naturally contaminated and spiked milk samples. The results obtained corresponded very well with those obtained by HPLC, which was used as confirmation method.


Asunto(s)
Antibacterianos/análisis , Cefalexina/análisis , Cefalotina/análisis , Residuos de Medicamentos/análisis , Inmunoensayo de Polarización Fluorescente/métodos , Leche/química , Animales , Anticuerpos/química , Reacciones Cruzadas , Fluoresceínas/química , Inmunoensayo de Polarización Fluorescente/normas , Colorantes Fluorescentes/química , Análisis de los Alimentos/métodos , Humanos , Inmunoconjugados/química , Límite de Detección , Conejos
18.
PLoS One ; 10(4): e0124267, 2015.
Artículo en Inglés | MEDLINE | ID: mdl-25897517

RESUMEN

Antimicrobial usage is common in Asian aquaculture. This study aimed to determine the quality of antimicrobial products used by Vietnamese striped catfish (Pangasianodon hypophthalmus) farmers. Twenty one antimicrobial products (11 products contained a single antimicrobial and 10 products contained a mixture of two different antimicrobials) commonly used by catfish farmers were obtained from so-called chemical shops located in the Mekong Delta, Vietnam. Ultra High Performance Liquid Chromatography Mass Spectrometry was used to analyze concentration of sulfonamides, trimethoprim, amoxicillin, cefalexin and ciprofloxacin whereas concentrations of florfenicol and doxycycline were analyzed by High Performance Liquid Chromatography with UV detection. Results revealed that only 4/11 products with a single antimicrobial and 2/10 products with a mixture of antimicrobials contained active substances within ±10% of the concentration declared on the product label. Two products with antimicrobial mixtures did not contain any of the declared antimicrobials. Comparing two batches, analysis of 11 products revealed that only one product contained a concentration of active compound that varied with less than 10% in both batches. Several product labels provided inadequate information on how to calculate therapeutic dosage and further stated withdrawal time despite lack of pharmacokinetic data on the antimicrobials in catfish. There is an urgent need to strengthen approval procedures and in particular regularly to monitor the quality of antimicrobials used in Vietnamese aquaculture.


Asunto(s)
Antiinfecciosos/análisis , Bagres , Drogas Veterinarias/análisis , Amoxicilina/análisis , Amoxicilina/normas , Animales , Antiinfecciosos/normas , Acuicultura , Cefalexina/análisis , Cefalexina/normas , Ciprofloxacina/análisis , Ciprofloxacina/normas , Doxiciclina/análisis , Doxiciclina/normas , Control de Calidad , Estándares de Referencia , Sulfonamidas/análisis , Sulfonamidas/normas , Tianfenicol/análogos & derivados , Tianfenicol/análisis , Tianfenicol/normas , Trimetoprim/análisis , Trimetoprim/normas , Drogas Veterinarias/normas , Vietnam
19.
Spectrochim Acta A Mol Biomol Spectrosc ; 109: 308-12, 2013 May 15.
Artículo en Inglés | MEDLINE | ID: mdl-23545436

RESUMEN

In this paper, a novel chemometric method was developed for rapid, accurate, and quantitative analysis of cefalexin in samples. The experiments were carried out by using the short near-infrared spectroscopy coupled with artificial neural networks. In order to enhancing the predictive ability of artificial neural networks model, a modified genetic algorithm was used to select fixed number of wavelength.


Asunto(s)
Antibacterianos/análisis , Cefalexina/análisis , Espectroscopía Infrarroja Corta/métodos , Algoritmos , Redes Neurales de la Computación , Espectroscopía Infrarroja Corta/economía
20.
Chemosphere ; 89(3): 280-6, 2012 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-22591850

RESUMEN

In recent years, increasing attention has been paid to the trace-level contamination of pharmaceuticals in the water environment all over the world. Considering a large number of pharmaceuticals used, it is crucial to establish a priority list of pharmaceuticals that should be monitored and/or treated first. In the present study, we developed a ranking system based on the pharmaceutical consumption, removal performance in the wastewater treatment plants (WWTPs) and potential ecological effects, and applied to the situation of China. 39 pharmaceuticals, which had available consumption data and also been reported previously in the WWTPs of China, were selected as candidate pharmaceuticals. Among them, seventeen pharmaceuticals were considered as priority pharmaceuticals, out of which, erythromycin, diclofenac acid and ibuprofen, had the high priority. Compared with other literatures, we found that some pharmaceuticals given concerns to globally should also be included in the priority list in China; while some pharmaceuticals, not mentioned in other literatures, such as cefalexin, ketoconazole, should be also given prior consideration in China. Among all the therapeutic classes, antibiotics, which were grossly abused in China, contributed the most to the priority pharmaceuticals. However, priority antibiotics accounted for only 32% of candidate antibiotics, while 71% and 100% of the candidate anti-inflammatory and antilipidemic respectively were identified as the priority pharmaceuticals, indicating that antibiotics might be overanxiously considered in the previous studies on their behaviors in the WWTPs of China.


Asunto(s)
Preparaciones Farmacéuticas/análisis , Contaminantes Químicos del Agua/análisis , Antibacterianos/análisis , Cefalexina/análisis , China , Diclofenaco/análisis , Utilización de Medicamentos , Efectos Colaterales y Reacciones Adversas Relacionados con Medicamentos , Ecosistema , Monitoreo del Ambiente , Eritromicina/análisis , Humanos , Ibuprofeno/análisis , Cetoconazol/análisis , Ríos , Eliminación de Residuos Líquidos , Purificación del Agua
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