Department of Analytical Chemistry, Faculty of Sciences, University of Córdoba, Edificio Anexo Marie Curie, Campus de Rabanales, 14071 Córdoba, Spain.
J Chromatogr A. 2010 Oct 1;1217(40):6250-7. doi: 10.1016/j.chroma.2010.08.017. Epub 2010 Aug 13.
A multiresidue method was described for determining eight sulfonamides, SAs (sulfadiazine, sulfamerazine, sulfamethoxypyridazine, sulfachloropyridazine, sulfadoxine, sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline) in animal muscle tissues (pork, chicken, turkey, lamb and beef) at concentrations below the maximum residue limit (100 μg kg(-1)) set by the European Commission. The method was based on the microextraction of SAs in 300-mg muscle samples with 1 mL of a supramolecular solvent made up of reverse micelles of decanoic acid (DeA) and posterior determination of SAs in the extract by LC/fluorescence detection, after in situ derivatization with fluorescamine. Recoveries were quantitative (98-109%) and matrix-independent, no concentration of the extracts was required, the microextraction took about 30 min and several samples could be simultaneously treated. Formation of multiple hydrogen bonds between the carboxylic groups of the solvent and the target SAs (hydrogen donor and acceptor sum between 9 and 11) were considered as the major forces driving microextraction. The method was validated according to the European Union regulation 2002/657/EC. Analytical performance in terms of linearity, selectivity, trueness, precision, stability of SAs, decision limit and detection capability were determined. Quantitation limits for the different SAs ranged between 12 μg kg(-1) and 44 μg kg(-1), they being nearly independent of matrix composition. Repeatability and reproducibility, expressed as relative standard deviation, were in the ranges 1.8-3.6% and 3.3-6.1%. The results of the validation process proved that the method is suitable for determining sulfonamide residues in surveillance programs.
建立了一种多残留检测方法,用于测定动物肌肉组织(猪肉、鸡肉、火鸡肉、羊肉和牛肉)中 8 种磺胺类药物(磺胺嘧啶、磺胺甲恶唑、磺胺二甲嘧啶、磺胺氯哒嗪、磺胺间甲氧嘧啶、磺胺甲噁唑、磺胺二甲氧嘧啶和磺胺喹噁啉)残留量。该方法基于 300mg 肌肉样品中 1ml 超分子溶剂(癸酸反胶束)的微萃取,随后用荧光胺原位衍生化,在 LC/荧光检测下测定提取物中的磺胺类药物残留量。回收率为定量(98-109%),且与基质无关,无需对提取物进行浓缩,微萃取时间约 30min,可同时处理多个样品。认为溶剂的羧酸基团与目标磺胺类药物之间形成的氢键(供体和受体的氢键总数为 9-11)是推动微萃取的主要力。该方法按照欧盟 2002/657/EC 法规进行了验证。确定了方法的线性、选择性、准确度、精密度、磺胺类药物稳定性、决定限和检测能力等分析性能。不同磺胺类药物的定量限范围为 12μgkg(-1)到 44μgkg(-1),几乎与基质组成无关。重复性和再现性(表示为相对标准偏差)分别在 1.8-3.6%和 3.3-6.1%范围内。验证过程的结果表明,该方法适用于监测计划中磺胺类药物残留的测定。