title: Comparison of the determination of four sulphonamides and their N4-acetyl metabolites in swine muscle tissue using liquid chromatography with ultraviolet and mass spectral detection.
abstract: A discharge-assisted LC-MS method has been developed and validated for the analysis of four sulphonamides (sulphathiazole, sulphadiazine, sulphamerazine and sulphadimidine) and their N4-acetyl metabolites in the muscle of swine treated with Polysulpha-Complex, which contains all four drugs. The clean-up procedure developed involved chloroform-acetone extraction followed by Sep-Pak silica solid-phase extraction. In parallel a LC-UV method was validated using the same clean-up procedure. Blank tissue was fortified at levels between 20 and 100 micrograms/kg. [13C]sulphadimidine was used as internal standard. The samples were analysed with thermospray LC-MS. The [M + H]+ ion was the major ion in all cases and was employed for single-ion monitoring. The limits of detection (LOD) were below 25 micrograms/kg and the limits of quantification (LOQ) for most sulphonamides were ca. 100 micrograms/kg. Incurred muscle tissues were measured by both LC methods and the concentrations of the sulphonamides were found to be similar. However, the LC-MS procedure is more suitable for confirmatory analysis due to its specificity.
authors.affiliation: Bundesgesundheitsamt Berlin, Institute of Veterinary Medicine, Germany.
authors.forename: G
authors.initials: G
authors.lastname: Balizs
authors.forename: L
authors.initials: L
authors.lastname: Benesch-Girke
authors.forename: S
authors.initials: S
authors.lastname: Börner
authors.forename: S A
authors.initials: SA
authors.lastname: Hewitt
mesh_terms: D000107:Acetylation; D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis / Q000378:metabolism; D008401:Gas Chromatography-Mass Spectrometry; D013058:Mass Spectrometry; D008460:Meat / Q000032:analysis; D009132:Muscles / Q000737:chemistry* / Q000378:metabolism; D013411:Sulfadiazine / Q000032:analysis / Q000378:metabolism; D013416:Sulfamerazine / Q000032:analysis / Q000378:metabolism; D013418:Sulfamethazine / Q000032:analysis / Q000378:metabolism; D000077589:Sulfathiazole; D013432:Sulfathiazoles / Q000032:analysis / Q000378:metabolism; D013449:Sulfonamides / Q000032:analysis* / Q000378:metabolism*; D013552:Swine / Q000378:metabolism*; D014466:Ultraviolet Rays
chemical_list: D013432:Sulfathiazoles; D013449:Sulfonamides; D013411:Sulfadiazine; D013418:Sulfamethazine; D013416:Sulfamerazine; D000077589:Sulfathiazole