Sulfonamides In Feed Research Articles

Determination of Sulfonamides in Feeds by High-Performance Liquid Chromatography after Fluorescamine Precolumn Derivatization.

A new multi-residue method for the analysis of sulfonamides (sulfadiazine, sulfamerazine, sulfamethazine, sulfaguanidine and sulfamethoxazole) in non-target feeds using high-performance liquid chromatography-fluorescence detection (HPLC-FLD) and precolumnderivatization was developed and validated. Sulfonamides (SAs) were extracted from feed with an ethyl acetate/methanol/acetonitrile mixture. Clean-up was performed on a Strata-SCX cartridge. The HPLC separation was performed on a Zorbax Eclipse XDB C18 column with a gradient mobile phase system of acetic acid, methanol, and acetonitrile. The method was validated according to EU requirements (Commission Decision 2002/657/EC). Linearity, decision limit, detection capability, detection and quantification limits, recovery, precision, and selectivity were determined, and adequate results were obtained. Using the HPLC-FLD method, recoveries were satisfactory (79.3–114.0%), with repeatability and reproducibility in the range of 2.7–9.1% to 5.9–14.9%, respectively. Decision limit (CCα) and detection capability (CCβ) were 197.7–274.6 and 263.2–337.9 µg/kg, respectively, and limit of detection (LOD) and limit of quantification (LOQ) were 34.5–79.5 and 41.3–89.9 µg/kg, respectively, depending on the analyte. Results showed that this analytical procedure is simple, rapid, sensitive, and suitable for the routine control of feeds.

Development of an immunoaffinity chromatography and HPLC-UV method for determination of 16 sulfonamides in feed

A novel and simple method for detecting 16 sulfonamides (SAs) in animal feed using high performance liquid chromatography equipped with a photo-diode array detector (HPLC/PDA) and immunoaffinity chromatography was developed. The chromatographic peaks of the 16 SAs were successfully identified by comparing their retention times and UV spectra with reference standards. Method validation was performed with linearity, sensitivity, selectivity, accuracy and precision. The limits of detection (LODs) for the instrument used to study sulfonamides ranged from 14.1 to 45.0μg/kg, and the limits of quantification (LOQs) ranged from 46.9 to 150.0μg/kg. Average recoveries of the 16 SAs ranged from 78.2% to 105.2%. Method replication resulted in intraday and interday peak area variation of <5.5%. The developed method was specific and reliable and is suited for the routine analysis of SAs in animal feed.

Determination of Sulfonamides in Feeds by High Performance Liquid Chromatography with Molecularly Imprinted Solid Phase Extraction

Determination of Sulfonamides in Feeds by High Performance Liquid Chromatography with Molecularly Imprinted Solid Phase Extraction

Optimization and Validation of a Confirmatory Method for Determination of Ten Sulfonamides in Feeds by LC and UV-Diode Array Detection

A simple, rapid, and reliable multiresidue method, based on liquid chromatography (LC) and ultraviolet (UV)-diode array detection (DAD), is described for assaying ten sulfonamides (sulfadiazine, sulfathiazole, sulfamerazine, sulfamethazine, sulfamethoxypyridazine, sulfamonomethoxine, sulfachloropyridazine, sulfamethoxazole, sulfaquinoxaline, and sulfadimethoxine) in feeds. The chromatographic separation is accomplished using a C18 column, eluted with a mobile phase consisting of acetate buffer, acetonitrile, and methanol. The sample preparation requires a simple extraction with chloroform/acetone and a purification step by solid-phase extraction. The analytical parameters of precision, detection and quantification limits, recovery, and ruggedness have been evaluated by a validation procedure following the European guidelines of Regulation 882/2004/EC and Decision 657/2002/EC.

Preparation of quality control materials for the determination of sulfonamides in animal feed

A feasibility study of the preparation of quality control materials for the analysis of medicated feeds has been carried out. Two analytical methodologies for the analysis of sulfonamides in feeds were developed, validated and applied to homogeneity and stability studies. Pig feeds spiked with sulfadiazine and sulfadimidine were prepared. The drugs were spiked at 500 µg g−1, representing what can be expected in a commercial medicated feed, and at 2 and 5 µg g−1, which roughly correspond to drug-free feeds cross-contaminated during the fabrication process. The homogeneity of both the bulk and the bottled materials was verified. A stability study of the materials containing 2 and 5 µg g−1 of sulfonamides was carried out over an 18-month period at room temperature, at 4°C and −20°C. The determination of sulfadiazine and sulfadimidine in samples coming from these homogeneity and stability studies of the quality control materials was carried out by high-performance liquid chromatography (HPLC) with either ultraviolet light or fluorimetric detection, depending on the concentration of the analytes in the samples.

Extraction and GLC Determination of Mixed Sulfonamides in Feeds

Abstract Seven sulfonamides added to feed samples were extracted with DMF and hydrolyzed to the amines with sulfuric acid. After alkalization, the extracts were analyzed by GLC, using a Carbowax 20M column. Recoveries averaged between 94 and 104%. The described method is rapid and requires a minimum of manipulations.