Dispersive solid-phase extraction for the determination of sulfonamides in chicken muscle by liquid chromatography.
A new, fast and low-cost sample preparation for the determination of sulfonamide (SA) residues in chicken muscle by LC technique has been developed. The procedure involves single extraction of sample with acetonitrile, followed by a rapid clean-up and was called "dispersive solid-phase extraction" (dispersive SPE). Using dispersive SPE 25 mg of octadecyl sorbent was added to 1 ml of acetonitrile extract, mixed and centrifuged. The acetonitrile layer was evaporated and residue was dissolved in acetate buffer (pH 3.5). Analysed compounds were detected by fluorescence detector after pre-column derivatization with fluorescamine. The separation of analytes was performed with gradient elution with mobile phase methanol: 2% acetic acid and RP-LC analytical column. The whole procedure was evaluated for six sulfonamides (sulfadiazine, sulfamerazine, sulfamethazine, sulfametoxypirydazine, sulfametoxazole and sulfadimetoxine) according to the European Commission Decision 2002/657/EC. Specificity, decision limit (CCalpha), detection capacity (CCbeta), trueness and precision were determined during validation process. The dispersive SPE with octadecyl sorbent was found suitable for sample preparation before sulfonamide determination in chicken muscle. As it was found the most of endogenous matrix components were removed and the analytes were isolated from spiked samples with recoveries above 90%. The used analytical conditions allow to successively separate all the tested sulfonamides with the limit of detection at the level of 1-5 microg/kg. The method is simple, rapid and more effective than conventional methods.
Posyniak
Andrzej
A
National Veterinary Research Institute, Department of Pharmacology and Toxicology, al Partyzantow 57, 24-100 Pulawy, Poland. aposyn@piwet.pulawy.pl
Zmudzki
Jan
J
Mitrowska
Kamila
K
D000818:Animals; D002645:Chickens; D002853:Chromatography, Liquid / Q000379:methods*; D009132:Muscles / Q000737:chemistry*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013050:Spectrometry, Fluorescence; D013449:Sulfonamides / Q000032:analysis*
D013449:Sulfonamides