title: Determination of sulphonamides in animal tissues by high performance liquid chromatography with pre-column derivatization of 9-fluorenylmethyl chloroformate.
abstract: A novel approach for simultaneous determination of 12 sulphonamides (sulphadiazine, sulphamethazine, sulphathiazole, sulphadimethoxine, sulphamerazine, sulphapyridine, sulphamethoxazole, suphamethizole, sulphaquinoxaline, sulphameter, sulphamonomethoxine, and sulphachloropyridazine) in animal tissues (swine muscle and liver, chicken muscle, beef muscle) by HPLC with UV detection has been developed. A pre-column derivatization of the sulphonamide compounds with 9-fluorenylmethyl chloroformate (FMOC-Cl) has been proposed and the reaction conditions have been optimized. The FMOC-sulphonamide derivatives were purified by SPE with silica gel as solid support prior to HPLC separation. The limits of detection for the sulphonamide compounds were greatly improved after the derivatization and purification step for the derivatives. Sulphonamide residues in animal tissues were extracted by acetonitrile and purified by solid phase extraction with C(18) as the solid support. The method developed has high sensitivity and good repeatability, and the average recoveries for most of the sulphonamides at various spiking levels were above 70% with relative standard deviations below 13.7%. The limits of detection for most sulphonamides can reach 3-5 microg/kg.
authors.affiliation: Analytical & Testing Center of Beijing Normal University, Beijing China.
authors.forename: Qiong-Hui
authors.initials: QH
authors.lastname: Zou
authors.forename: Meng-Xia
authors.initials: MX
authors.lastname: Xie
authors.forename: Xiang-Feng
authors.initials: XF
authors.lastname: Wang
authors.forename: Yuan
authors.initials: Y
authors.lastname: Liu
authors.forename: Jin
authors.initials: J
authors.lastname: Wang
authors.forename: Jia
authors.initials: J
authors.lastname: Song
authors.forename: Hui
authors.initials: H
authors.lastname: Gao
authors.forename: Jie
authors.initials: J
authors.lastname: Han
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D005449:Fluorenes / Q000737:chemistry*; D006863:Hydrogen-Ion Concentration; D007700:Kinetics; D012680:Sensitivity and Specificity; D013056:Spectrophotometry, Ultraviolet; D013449:Sulfonamides / Q000032:analysis*; D013696:Temperature
chemical_list: D005449:Fluorenes; D013449:Sulfonamides; C054007:1-(9-fluorenyl)methyl chloroformate