The Experts below are selected from a list of 360 Experts worldwide ranked by ideXlab platform
Damia Barcelo - One of the best experts on this subject based on the ideXlab platform.
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removal of sulfonamide antibiotics upon conventional activated sludge and advanced membrane bioreactor treatment
Analytical and Bioanalytical Chemistry, 2012Co-Authors: Maria Jesus Garcia Galan, Silvia M Diazcruz, Damia BarceloAbstract:This work reports the removal efficiencies of nine sulfonamides (SAs) and one of their acetylated metabolites during conventional activated sludge (CAS) and membrane bioreactor (MBR) treatments. Two different types of membranes were studied, hollow-fiber membranes and flat-sheet membranes, in two separate pilot plants operating in parallel to a full-scale CAS treatment. A total of 48 water samples and 16 sewage sludge samples were analyzed by liquid chromatography–tandem mass spectrometry. We obtained 100 % elimination in the MBR effluents for three SAs (sulfadiazine, sulfadimethoxine, and Sulfamethoxypyridazine) and the metabolite. For the rest of the SAs, the removal efficiencies during CAS and MBR treatments were similar and usually below 55 %. Sulfamethizole was the most recalcitrant SA, exhibiting negative removal efficiencies in all the treatments investigated. The concentrations of SAs in the different sewage sludge types were also calculated and ranged from 0.01 to 11 ng g-1. Furthermore, adsorption and biodegradation of SAs in activated sludge were investigated in two sets of batch reactors, which were spiked at high and low concentration (1,000 and 50 ng mL-1, respectively). All SAs followed a similar trend and, with the exception of sulfathiazole, were not fully eliminated after 25 days of treatment.
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development and validation of a pressurised liquid extraction liquid chromatography electrospray tandem mass spectrometry method for β lactams and sulfonamides in animal feed
Journal of Chromatography A, 2010Co-Authors: Lina Kantiani, Damia Barcelo, Marinella Farre, Josep Manuel Grases I FreixiedasAbstract:Abstract This study presents the development and validation of a sensitive and fast (30 min extraction time and 10 min chromatographic run) method for the detection of penicillins, cephalosporins and sulfonamides in animal feed using pressurised liquid extraction and solid phase extraction as extraction and pre-concentration procedures, followed by liquid chromatography–quadrupole-linear ion-trap mass spectrometry. The developed method was validated showing limits of detection ranging from 0.12 (ampicillin) to 3.94 ng/g (amoxicillin), instrumental and analytical linearity coefficients above 0.99 in both standard and matrix-based solutions as well as relative recoveries ranging from 71% (cefoperazone) to 115% (cefazolin). Repeatability of the method was in the range of 1–9% (RSD %), whereas reproducibility ranged from 3% to 13% (RSD %). The developed and validated method was finally applied to the analysis of real feed samples. The results showed 10 out of 18 analytes to be present in at least one sample and all 14 samples to contain at least one analyte. Penicillin V, oxacillin, ceftiofur, cefoperazone, cefalexin, cefazolin, Sulfamethoxypyridazine and sulfapyridine were not detected in any of the samples analysed. Considering the ban of antibacterials as growth promoters added in animal feed, this method is capable of detecting the low concentrations that could result from failure to comply with the regulations or on-site contamination.
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determination of antimicrobials in sludge from infiltration basins at two artificial recharge plants by pressurized liquid extraction liquid chromatography tandem mass spectrometry
Journal of Chromatography A, 2006Co-Authors: Silvia M Diazcruz, Maria Lopez J De Alda, Damia BarceloAbstract:This work describes the optimization of a multi-residue analytical approach for the simultaneous determination of 11 antimicrobials (9 sulphonamides and 2 penicillins) in sludge from infiltration basins. The method is based on pressurized liquid extraction (PLE) followed by solid-phase extraction (SPE) for pre-concentration and purification, and analysis by liquid chromatography-tandem mass spectrometry using electrospray in the positive ionization mode (LC-(ESI+)-MS/MS). Limits of detections (LODs) between 1 pg/g and 0.2 ng/g and limits of quantifications (LOQs) between 5 pg/g and 0.6 ng/g were achieved. Good recovery values (57.6-104%) were obtained for sulfamethazine, sulfapyridine, sulfadiazine and Sulfamethoxypyridazine, while medium recovery values (14-47%) were afforded for sulfadimethoxine, sulfathiazole and sulfamethoxazole. However, only a poor recovery (<1%) could be possible for both penicillins and two sulphonamides, namely nafcillin, dicloxacillin, sulfisoxazole and sulfamethizole. These low recoveries were attributed to the presence of ionic suppression effects (even after thorough extraction and purification) rather than to an inefficient extraction. The method developed was applied to the analysis of sludge samples from the infiltration basins of two artificial recharge plants located in Sweden and Denmark. All target compounds were found to be present in at least one sample. Sulfadimethoxine, nafcillin and dicloxacillin were detected in all the samples analysed.
Alberto Cepeda - One of the best experts on this subject based on the ideXlab platform.
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Determination of the Presence of Three Antimicrobials in Surface Water Collected from Urban and Rural Areas
The Journal of Antibiotics, 2013Co-Authors: Alejandra Iglesias, Carlos Manuel Franco Abuín, Carolina Nebot, Jose M Miranda, Beatriz I. Vázquez, Alberto CepedaAbstract:Due to the continuous release of antimicrobials into the environment, the aim of this study was to compare the frequency of detection of sulfamethazine, Sulfamethoxypyridazine and trimethoprim in surface water collected from urban and rural areas in Northwestern Spain. A monitoring study was conducted with 314 river water samples analyzed by high-performance liquid chromatography coupled to tandem mass spectrometry. The results indicated that 37% of the samples contained residues of at least one of the investigated antimicrobials, and every sampling site yielded positive samples. At sites located near the discharge points of wastewater treatment plants and near the collection point of a drinking-water treatment plant, more than 6% of the samples were positive for the presence of antimicrobial residues.
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detection and quantitative analysis of 21 veterinary drugs in river water using high pressure liquid chromatography coupled to tandem mass spectrometry
Environmental Science and Pollution Research, 2012Co-Authors: Alejandra Iglesias, Carolina Nebot, Jose M Miranda, B I Vazquez, Alberto CepedaAbstract:The use of veterinary drugs in food production focuses on the control and improvement of animal health. The disadvantage of this practice is that pharmaceuticals and their metabolites are released into the environment, finding their way to natural water systems and becoming a potential risk to non-target organism. This paper reports the development and validation of a quantitative method, based on high-performance liquid chromatography coupled to tandem mass spectrometry, for the simultaneous analysis of 21 veterinary drugs, antimicrobials, corticosteroids, coccidiostats and antifungal agents, in surface water. The precision of the method was established by calculating the mean recoveries, which were in the range of 94–101%. The developed method was employed to conduct the first monitoring study on the presence of veterinary drugs in the Galicia region, Northwest of Spain and was applied to 235 surface water samples. Eleven veterinary drugs were detected at concentrations from below the limit of quantification to 2,978.6 ng L−1. Limits of detection and quantification were in the range of 6.2 (betamethasone, cortisone, decoquinate, dexamethasone, maduramycin, monensin, narasin, salinomycin, sulfachloropyridazine, Sulfamethoxypyridazine and trimethoprim) to 12.5 ng L−1 (for the rest of the selected drugs) and 12.5 (betamethasone, cortisone, decoquinate, dexamethasone, maduramycin, monensin, narasin, salinomycin, sulfachloropyridazine, Sulfamethoxypyridazine and trimethoprim) to 25.0 ng L−1 (for the remaining pharmaceuticals), respectively. Sulfonamides were the group most frequently found, which are widely used in veterinary medicine.
Miguel Angel Rodriguezdelgado - One of the best experts on this subject based on the ideXlab platform.
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comparison between magnetic and non magnetic multi walled carbon nanotubes dispersive solid phase extraction combined with ultra high performance liquid chromatography for the determination of sulfonamide antibiotics in water samples
Talanta, 2013Co-Authors: Antonio V Herreraherrera, Javier Hernandezborges, Maria M Afonso, Antonio J Palenzuela, Miguel Angel RodriguezdelgadoAbstract:Abstract In this manuscript, a new method based on the use of off-line dispersive solid-phase extraction (dSPE) combined with ultra-high performance liquid chromatography with diode-array detection was developed to determine 11 sulfonamide antibiotics (sulfanilamide, sulfacetamide, sulfadiazine, sulfathiazole, sulfamerazine, sulfadimidin, Sulfamethoxypyridazine, sulfadoxine, sulfamethoxazole, sulfisoxazole and sulfadimethoxine) in mineral waters with different mineral content. For this purpose, pristine multi-walled carbon nanotubes (MWCNTs) and magnetic-MWCNTs (m-MWCNTs) were used as sorbents. Magnetic nanoparticles were synthesized by means of a solvothermal process, assembled onto CNTs through an “aggregation wrap” mechanism and characterized by scanning electron microscopy. Parameters affecting the extraction such as volume and pH of the sample, amount of sorbent and type and volume of eluent were optimized. Once optimum extraction conditions (250 mL of water at pH 6.0 and elution with 25 mL of MeOH) were obtained, the extraction efficiency of the different carbon nanomaterials was compared. Results demonstrated the higher extraction capacity of pristine MWCNTs with recoveries between 61 and 110% (except for sulfacetamide which ranged between 40 and 53%) and between 22 and 77% for m-MWCNTs. Limits of detection lower than 32 ng/L were achieved for all of the analyzed samples.
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dispersive liquid liquid microextraction combined with ultra high performance liquid chromatography for the simultaneous determination of 25 sulfonamide and quinolone antibiotics in water samples
Journal of Pharmaceutical and Biomedical Analysis, 2013Co-Authors: Antonio V Herreraherrera, Javier Hernandezborges, Teresa M Borgesmiquel, Miguel Angel RodriguezdelgadoAbstract:In this work, a dispersive liquid-liquid microextraction (DLLME) procedure combined with ultra-high performance liquid chromatography with diode-array detection was developed to determine 25 antibiotics in mineral and run-off waters. Optimum DLLME conditions (5 mL of water at pH=7.6, 20% (w/v) NaCl, 685 μL of CHCl₃ as extractant solvent, and 1250 μL of ACN as disperser solvent) allowed the repeatable, accurate and selective determination of 11 sulfonamides (sulfanilamide, sulfacetamide, sulfadiazine, sulfathiazole, sulfadimidin, Sulfamethoxypyridazine, sulfadoxine, sulfamethoxazole, sulfisoxazole, sulfadimethoxine and sulfaquinoxaline) and 14 quinolones (pipemidic acid, marbofloxacin, fleroxacin, levofloxacin, pefloxacin, ciprofloxacin, lomefloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, moxifloxacin, oxolinic acid and flumequine). The method was validated by means of the obtention of calibration curves of the whole method as well as a recovery study at two levels of concentration. The LODs of the method were in the range 0.35-10.5 μg/L with recoveries between 78% and 117%.
Shuo Wang - One of the best experts on this subject based on the ideXlab platform.
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development of a chemiluminescent enzyme linked immunosorbent assay for five sulfonamide residues in chicken muscle and pig muscle
Journal of the Science of Food and Agriculture, 2009Co-Authors: Junwei Liu, Yan Zhang, Guozhen Fang, Wenjie Zheng, Shuo WangAbstract:BACKGROUND: An enzyme-linked immunosorbent assay (ELISA) based on polyclonal antibodies with enhanced chemiluminescent (ECL) detection of sulfonamides in food samples has been optimised and characterised. The specificity of the assay was assessed by determining cross-reactivities with a set of 16 sulfonamides. The aim of this study was to develop a method for determining sulfonamides with high sensitivity. RESULTS: The sensitivity of the developed ECL-ELISA was higher than that of colorimetric ELISA. The sensitivities of five of the sulfonamides (sulfisozole, sulfathiazole, sulfameter, Sulfamethoxypyridazine and sulfapyridine) ranged from 0.73 to 2.92 µg L−1, with limits of detection of 0.10–0.43 µg L−1. The coefficients of variation of intra-assay and inter-assay studies carried out over 5 days were mostly less than 10%. Recovery studies of chicken muscle and pig muscle were performed with simple and rapid extraction. Good recoveries (62.1–110.3%) were achieved and the results correlated well with those obtained using high-performance liquid chromatography analysis. CONCLUSION: This study has provided an effective analytical technique for the rapid and reliable determination of residues of sulfisozole, sulfathiazole, sulfameter, Sulfamethoxypyridazine and sulfapyridine in food samples with high sensitivity. To the authors' knowledge, this is the first report on chemiluminescent ELISA for sulfonamide analysis. Copyright © 2008 Society of Chemical Industry
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multiwalled carbon nanotubes as sorbent for on line coupling of solid phase extraction to high performance liquid chromatography for simultaneous determination of 10 sulfonamides in eggs and pork
Journal of Chromatography A, 2006Co-Authors: Guozhen Fang, Shuo WangAbstract:Abstract The sulfonamides (SAs) have been widely used as effective chemotherapeutics and growth promoters in animals’ feeding, but their residues could be a potential danger to human health due to their carcinogenic potency and possible antibiotic resistance. Development of a simple and sensitive method for the determination of SAs residues in food of animal origin, therefore, is of great significance. An on-line solid-phase extraction (SPE) method using multiwalled carbon nanotubes as sorbent coupled with high-performance liquid chromatography (HPLC) for simultaneous determination of 10 sulfonamides (SAs) in eggs and pork was developed. The adsorptive potential of carbon nanotubes for solid-phase extraction of sulfonamides was investigated for the first time in the present paper. To on-line interface solid-phase extraction with HPLC, a conventional sample loop on the six-port injector valve of the HPLC was replaced by a preconcentration column packed with carbon nanotubes. The analytes in water solution were preconcentrated onto the preconcentration column and subsequently eluted with mobile phase of methanol–water (22:78). The developed on-line solid-phase extraction method for HPLC permitted the current HPLC separation and the next preconcentration proceeded in parallel, and thus allows one determination finished within 35 min. The RSD of 10 SAs for nine replicate measurements of a standard mixture of 1 μg l−1 were in the range of 2.5–7.8%. The method was applied to the determination of trace sulfadiazin (SDZ), sulfamerazine (SMR), sulfadimidine (SDMD), sulfathiazole (STZ), sulfamoxol (SMO), sulfamethizole (SMT), Sulfamethoxypyridazine (SMP), sulfachlorpyridazine (SCP), sulfadoxin (SDX) and sulfisoxazole (SIA) in eggs and pork. The results indicated that the proposed method was simple, cost-effective and sensitive.
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hapten synthesis and development of polyclonal antibody based multi sulfonamide immunoassays
Journal of Agricultural and Food Chemistry, 2006Co-Authors: Hongyan Zhang, Zhenjuan Duan, Lei Wang, Yan Zhang, Shuo WangAbstract:This paper reports the synthesis of five sulfonamide derivatives, the production of broad-specificity polyclonal antibodies for immunoassay of sulfonamides, and the analysis of milk samples by developed assay. The three-step synthesis procedure reported in most of the literature was adopted and modified in this study. In the procedure, the purification of the intermediate was avoided and the time of synthesis was shortened from >20 to 6-9 h with improved yields. This method is generally applicable to the synthesis of haptens containing the common structure of sulfonamides. Three haptens were coupled to keyhole limpet hemocyanin, and polyclonal antibodies were obtained from rabbits immunized with these conjugates. Using the antibodies obtained, from one of these was developed an enzyme-linked immunosorbent assay (ELISA) based on the competition between free sulfonamides and the hapten-horseradish peroxidase (HRP) conjugates. The hapten-HRP conjugate giving the best competitive results and 11 structurally different sulfonamides showed 50% inhibition at concentrations of <100 ng mL(-1). After removal of the protein with acetone, milk samples were analyzed by ELISA directly; a matrix effect could be avoided when a 1:20 dilution with phosphate-buffered saline was used, and 104-131% recoveries of spiked samples were obtained. The developed immunoassay is suitable to determine sulfisozole, sulfathiazole, sulfameter, Sulfamethoxypyridazine, sulfapyridine, and sulfamethizole below the maximum residue limit in milk (100 ng mL(-1) of total sulfonamides) rapidly and reliably.
Silvia M Diazcruz - One of the best experts on this subject based on the ideXlab platform.
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removal of sulfonamide antibiotics upon conventional activated sludge and advanced membrane bioreactor treatment
Analytical and Bioanalytical Chemistry, 2012Co-Authors: Maria Jesus Garcia Galan, Silvia M Diazcruz, Damia BarceloAbstract:This work reports the removal efficiencies of nine sulfonamides (SAs) and one of their acetylated metabolites during conventional activated sludge (CAS) and membrane bioreactor (MBR) treatments. Two different types of membranes were studied, hollow-fiber membranes and flat-sheet membranes, in two separate pilot plants operating in parallel to a full-scale CAS treatment. A total of 48 water samples and 16 sewage sludge samples were analyzed by liquid chromatography–tandem mass spectrometry. We obtained 100 % elimination in the MBR effluents for three SAs (sulfadiazine, sulfadimethoxine, and Sulfamethoxypyridazine) and the metabolite. For the rest of the SAs, the removal efficiencies during CAS and MBR treatments were similar and usually below 55 %. Sulfamethizole was the most recalcitrant SA, exhibiting negative removal efficiencies in all the treatments investigated. The concentrations of SAs in the different sewage sludge types were also calculated and ranged from 0.01 to 11 ng g-1. Furthermore, adsorption and biodegradation of SAs in activated sludge were investigated in two sets of batch reactors, which were spiked at high and low concentration (1,000 and 50 ng mL-1, respectively). All SAs followed a similar trend and, with the exception of sulfathiazole, were not fully eliminated after 25 days of treatment.
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determination of antimicrobials in sludge from infiltration basins at two artificial recharge plants by pressurized liquid extraction liquid chromatography tandem mass spectrometry
Journal of Chromatography A, 2006Co-Authors: Silvia M Diazcruz, Maria Lopez J De Alda, Damia BarceloAbstract:This work describes the optimization of a multi-residue analytical approach for the simultaneous determination of 11 antimicrobials (9 sulphonamides and 2 penicillins) in sludge from infiltration basins. The method is based on pressurized liquid extraction (PLE) followed by solid-phase extraction (SPE) for pre-concentration and purification, and analysis by liquid chromatography-tandem mass spectrometry using electrospray in the positive ionization mode (LC-(ESI+)-MS/MS). Limits of detections (LODs) between 1 pg/g and 0.2 ng/g and limits of quantifications (LOQs) between 5 pg/g and 0.6 ng/g were achieved. Good recovery values (57.6-104%) were obtained for sulfamethazine, sulfapyridine, sulfadiazine and Sulfamethoxypyridazine, while medium recovery values (14-47%) were afforded for sulfadimethoxine, sulfathiazole and sulfamethoxazole. However, only a poor recovery (<1%) could be possible for both penicillins and two sulphonamides, namely nafcillin, dicloxacillin, sulfisoxazole and sulfamethizole. These low recoveries were attributed to the presence of ionic suppression effects (even after thorough extraction and purification) rather than to an inefficient extraction. The method developed was applied to the analysis of sludge samples from the infiltration basins of two artificial recharge plants located in Sweden and Denmark. All target compounds were found to be present in at least one sample. Sulfadimethoxine, nafcillin and dicloxacillin were detected in all the samples analysed.
