Determination Of Sulfonamide Residues Research Articles

Studies Regarding the Detection of Sulfonamide Residues and Evaluation of the Level of Contamination in Poultry Meat

The excessive or uncontrolled use of antibiotics in poultry farming can lead to contaminated food products. Subsequently, the human consumption of products contaminated with these substances increases the global phenomenon of antibiotic resistance. The aim of this study was to develop and validate a high-performance liquid chromatography (HPLC) method suitable for the determination of sulfonamide residues in poultry meat and to check the presence of residues in random samples. The level of antimicrobial resistance was identified in order to evaluate the current stage and to estimate the tendency of this phenomenon. The HPLC method validation was performed in accordance with Commission Regulation (EC) No 657/2002 of 14 August 2002 Samples of fresh meat collected from a poultry slaughterhouse were analysed using the validated method in order to reveal the level of contamination. The data from EFSA was collected and analysed following the antimicrobial resistance for isolates of Salmonella spp., E. coli and Campylobacter spp. The method had good selectivity, linearity (R2 ≥ 0.99), precision (<6%), recoverybetween 97.7-109.6% and low limits of detection (LOD) and quantification (LOQ) Sulfaquinoxaline residues were present in 2 samples and the level of contamination did not exceed the Maximum Residue Level (31.98 ± 5.18 µg/kg and 23.70 ± 3.84 µg/kg). The analysis of data from EFSA highlighted the general presence of antimicrobial resistance especially for the following antibiotics: ciprofloxacin, tetracycline, nalidixic acid, ampicillin, sulfamethoxazole and trimethoprim. The present study brings a contribution to the process of stopping antibiotic resistance through new methods of monitorization of sulfonamide residues. The statistical data shows that there is a direct correlation between the market availability of antibiotics used in poultry farming and the occurrence of antibiotic resistance.

Determination of sulfonamide residues in cultured sea cucumber by pre-column derivatization capillary electrophoresis with fluorescence detection

A simple and mild method for the separation of sulfonamide residues based on a condensation reaction with O-phthalaldehyde solution (OPA) as labeling reagent with capillary electrophoresis has been developed. A 58.5 cm × 50 μm i.d. (50 cm effective length) untreated fused-silica capillary was used. To optimize the separation conditions, the background electrolyte concentration, pH, column temperature, voltage and other factors were evaluated. The optimal separation conditions were as follows: 20 mmol L−1 borate buffer; pH 9.1; column temperature 20 °C; separation voltage 18 kV, pressure 50 mbar and injection time 8 s. Under the optimal conditions, 10 kinds of sulfonamide derivatives could be well-separated within 8 min, and the linear ranges were 0.35–100 μg kg−1. The detection limit (at a signal-to-noise ratio of 3) was in the range of 0.12–0.25 μg kg−1, and the quantification limit (at a signal-to-noise ratio of 10) was in the range of 0.35–0.70 μg kg−1. The sulfonamide residues from cultured sea cucumber samples were determined under the optimal conditions with satisfactory results.

Synthesis of the Magnetically Nanoporous Organic Polymer Fe3O4@SiO2-NH2-COP and Its Application in the Determination of Sulfonamide Residues in Surface Water Surrounding a Cattle Farm.

Efficient extractions of trace antibiotic residues in the environment are a key factor for accurate quantification of the residues. A new nanoporous material, namely, magnetically covalent organic polymer (MCOP, Fe3O4@SiO2-NH2-COP) was synthesized in this work and was used for magnetic solid-phase extraction (MSPE). The combination of MSPE with high-performance liquid chromatography separation together with ultraviolet detection (HPLC-UV) was established as an effective method for the determination of four sulfonamide (SA) residues in surface water surrounding a cattle farm. The synthesized magnetic material was characterized by SEM, TEM, FT-IR, magnetic properties measurement system (MPMS), and nitrogen gas porosimetry. The material possessed many attractive features, such as a unique microporous structure, a larger specific surface area (137.93 m2·g−1) than bare Fe3O4 (24.84 m2·g−1), high saturation magnetization (50.5 emu·g−1), open adsorption sites, and high stability. The influencing parameters, including pH, the used amount of MCOPs, the type of eluent, adsorption solution, and desorption time, were optimized. Under the optimized conditions, the method conferred good linearity ranges (R2 ≥ 0.9990), low detection limits (S/N = 3, LOD, 0.10–0.25 μg·L−1), and satisfactory recoveries (79.7% to 92.2%). The enrichment factor (EF) for the four SAs was 34.13–38.86. The relative standard deviations of intraday (n = 5) and of interday (n = 3) were less than 4.8% and 8.9%, respectively. The equilibria between extraction and desorption for SAs could be reached within 150 s. The proposed method was sensitive and convenient for detecting SA residues in complex environmental matrices, and the successful application of the new MCOPs as an adsorbent was demonstrated.

Determination of sulfonamide residues in animal foodstuffs by magnetic dispersive solid-phase extraction using magnetic carbon nanocomposites coupled with ion pair-dispersive liquid\u2013liquid micro-extraction combined with HPLC-DAD

In this study, magnetic-dispersive solid-phase extraction coupled with ion pair-dispersive liquid–liquid micro-extraction (MSPE-i-DLLME) was used to the pre-concentration and extraction of five sulfonamides residues (sulfadiazine, sulfathiazole, sulfacetamide, sulfamethazine and sulfamethoxazole) in animal foodstuffs. The sulfonamides are extracted using magnetic carbon nanocomposite and then eluted with acetonitrile. In the DLLME step, the target analytes are collected in 1-octanol containing 10% Aliquat-336 (as extraction solvent). Finally, the compounds are quantified by HPLC with DAD detection. The extraction parameters optimized using the one at the time and central composite design methods. Under the optimized conditions: sample solution volume was 100 mL; initial pH: 12, amounts of MCNs: 30 mg; desorption solvent (ACN) volume, 1 mL; desorption condition, 10 min sonication at two step; extraction solvent (1-octanol + 10% aliquat) volume, 115 µL; pH of DLLME step, 3; salt effect, 24.6%, (w/v) NaCl; centrifuge, 5 min, 4000 rpm. In these extraction conditions, the proposed procedure represented good pre-concentration factors between 130 and 490; detection limits in the range from 0.01 to 5 μg kg−1 (at S/N = 3), and linear response in the 0.1–400 μg kg−1 concentration range. The method is successfully applied to the determination of sulfonamides residues in animal foodstuffs.

Determination of Sulfonamide Residues in Livestock and Poultry Manure Using Carbon Nanotube Extraction Combined with UPLC-MS/MS

Combined with ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), a method for simultaneous determination of 15 sulfonamides in livestock and poultry manure was established and further optimizes and improves the pre-treatment conditions. In this study, Fe3O4-multi-walled carbon nanotubes (MWCNTs) were used as the purification material, and achieved solid-liquid separation by an external magnet, which was faster than the traditional centrifugation process. The results showed that the recoveries of sulfonamides were from 89 to 119% and had relative standard deviations (RSDs) of less than 10%. The limit of detection (LOD) of the method was reached 0.5 to 1.0 μg/kg, and the limit of quantification (LOQ) was between 1.0 and 3.0 μg/kg. On the premise that a satisfactory recoveries can be obtained, Fe3O4-MWCNTs can be effectively used at least 3 times. We can conclude that this method has certain applicability and reliability in the analysis and detection of sulfonamides in livestock and poultry manure.

Determination of Sulfonamide Residues in Honey and Milk by HPLC Coupled with Novel Graphene Oxide/Polypyrrole Foam Material-Pipette Tip Solid Phase Extraction

A rapid, sensitive, and economical pipette tip solid phase extraction (PT-SPE) based on graphene oxide/polypyrrole (GO/PPy) coupled with high performance liquid chromatography (HPLC) was developed for the extraction and determination of sulfonamides (SAs) in honey and milk samples. The PT-SPE procedure involved only 3.0 mg of adsorbent, 3 min adsorptive extraction time, and less than 1.0 mL of solvent consumption (sample, washing, or eluent). Under the optimal conditions, good linearities (0.01–10.00 μg mL−1) were obtained with correlation coefficients (r) > 0.9996. The limits of detection (S/N = 3) were in the range of 1.04–1.50 ng mL−1. Meanwhile, the proposed method was successfully applied for the analysis of SAs in honey and milk with average recoveries within 62.3–109.0% and relative standard deviations less than 11.2%. The results demonstrated that the developed PT-SPE-HPLC method was suitable for the analysis of SAs in complex matrix due to its high sensitivity and accuracy.

CdTe量子点分子印迹传感器对水中磺胺类药物残留的检测

CdTe量子点分子印迹传感器对水中磺胺类药物残留的检测

Molybdenum Disulfide as a Dispersive Solid-Phase Extraction Adsorbent for Determination of Sulfonamide Residues in Water Samples Using Capillary Electrophoresis

Molybdenum Disulfide as a Dispersive Solid-Phase Extraction Adsorbent for Determination of Sulfonamide Residues in Water Samples Using Capillary Electrophoresis

Determination of sulfonamide residues in water samples by in-line solid-phase extraction-capillary electrophoresis

An in-line solid-phase extraction-capillary electrophoresis method with UV–vis detection was developed for the monitoring of residues of five sulfonamides (sulfadoxin, sulfadimethoxine, sulfamerazine, sulfachloropyridazine and sulfamethoxazole) in tap, bottled mineral and river waters. For this purpose an analyte concentrator was constructed, based on the introduction of a small portion of a solid-phase extraction sorbent into the electrophoretic capillary to carry out an in-line concentration step, improving sensitivity. A detailed study was carried out to optimize parameters affecting the in-line solid-phase extraction process, such as the design of the concentrator device, type of sorbent and conditions of elution and injection. The proposed method is simple for the environmental monitoring of these antibiotic residues in waters, allowing the direct injection of the samples without any off-line pretreatment and achieving limits of detection between 0.3 and 0.6 μg/L. Recoveries ranging 52.2–109.2% and relative standard deviations below 13.4% were obtained.

Determination of Sulfonamide Residues in Food by Micellar Liquid Chromatography

ABSTRACTThis paper presents new methods of determination of sulfonamide residues in food products of animal origin, based on liquid chromatography with a micellar mobile phase. The methods employ a technique of direct injection of the sample and preliminary isolation of the analyte by extraction in the liquid-solid and liquid-liquid system. The methods have been characterized by providing the parameters of the calibration curves, the range of linearity, limit of detection, and precision and accuracy of particular determinations. The recovery of the sulfonamides introduced into the food products studied has also been determined.

Determination of Sulfonamide Residues in the Tissues of Food Animals Using Automated Precolumn Derivatization and Liquid Chromatography with Fluorescence Detection

A liquid chromatographic method for the determination of sulfachloropyridazine, sulfadiazine, sulfadimethoxine, sulfadoxine, sulfaethoxypyridazine, sulfamethazine, sulfaquinoxaline, and sulfathiazole residues in the muscle, liver, and kidney of food animals using sulfapyridine as internal standard is reported. Tissues are extracted using a modified version of AOAC Official Method 983.31 (Sulfonamide Residues in Animal Tissues). The sample extract is reconstituted in pH 3.0 buffer-acetonitrile (60 + 40) and filtered into an autosampler vial. Using a programmable autosampler of a liquid chromatograph, a portion of the sample is derivatized precolumn with fluorescamine. The sulfonamide derivatives are separated by liquid chromatography using a C18 column with a mobile phase of 0.02M phosphoric acid-acetonitrile (60.5 + 39.5) and detected by fluorescence (excitation, 405 nm; emission, 495 nm). The method was applied to swine and cattle muscle, liver, and kidney; sheep and horse muscle and kidney; and chicken muscle and liver. The mean values for samples fortified with sulfonamides at levels between 0.05 and 0.2 microg/g agreed within 96-99% of spiked levels, with coefficients of variation ranging from 4-10%. The limit of detection (LOD) for all sulfonamides was 0.01 microg/g, with the exception of sulfaquinoxaline, for which the LOD was 0.015 microg/g.

Determination of Sulfonamide Residues in Milk by On‐Line Microdialysis and HPLC

A technique for the simultaneous determination of sulfonamides in milk was studied by using a home‐made microdialysis system on‐line to high‐performance liquid chromatography. Six sulfonamides (sulfadiazine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfadimethoxine, and sulfamethoxazole) in milk were isolated by a hollow dialysis fiber prior to chromatographic determination. The results shows 2–5 fold enrichments and the detection limits in sub‐µg L−1 levels. As the milk sample was spiked with the six sulfonamides, in the concentration ranges between 0.005 and 10 mg L−1, recoveries ranging from 97.8% to 100.4% were obtained, and the regression coefficients >0.995. The proposed method provides a simple, fast, and eco‐friendly procedure for isolating and determining sulfonamides in milk samples.

Determination of Sulfonamide Residues in Eggs by Liquid Chromatography

A method was developed for determining residual sulfonamide antibacterials such as sulfamethazine (SMZ), sulfamonomethoxine (SMM), sulfadimethoxine (SDM), and sulfaquinoxaline (SQ) in eggs using liquid chromatography with a photodiode array detector. The spiked and blank samples were cleaned up by using an Ultrafree-MC/PL centrifugal ultrafiltration unit. A Mightysil RP-4 GP column and a mobile phase of 28% (v/v) ethanol-H2O with a photodiode array detector were used for the determination. Average recoveries from eggs spiked with each drug at 0.1, 0.2, 0.4, and 1.0 ppm were > or = 80.9%, with relative standard deviations between 1.3 and 4.7%. The limits of quantitation were 0.060 ppm for SMZ, 0.045 for SMM, 0.044 for SDM, and 0.093 for SQ. The analysis of one sample required < 30 min and < 5 mL ethanol as solvent.