Pena Angelina L, Lino Celeste M, Silveira M Irene N
University of Coimbra, Centre of Pharmaceutical Studies, Faculty of Pharmacy, Group of Bromatology, 3000 Coimbra, Portugal.
J AOAC Int. 2003 Sep-Oct;86(5):925-9.
A simple and accurate cleanup procedure using polymeric sorbent was developed for the determination of oxytetracycline (OTC) and tetracycline (TC) residues in salmon muscle. It was applied to the analysis of 20 salmon samples during a month period. The OTC and TC residues were extracted with ethylenediaminetetracetic acid (EDTA)-McIlvaine buffer acidified at pH 4.0 and cleaned up by solid-phase extraction with a polymeric sorbent. The advantages of the polymeric sorbent over the silica-based sorbent in the cleanup of salmon muscle samples are described. A liquid chromatographic method with post-column derivatization and fluorescence detection is proposed because of its sensitivity and specificity. The average recoveries of OTC and TC from muscle salmon tissue fortified at 50, 100, and 200 microg/kg levels, ranged from 83.9 to 93.4% with a coefficient of variation between 4.09 and 5.80%. The limit of quantitation for OTC and TC in salmon muscle was 50 microg/kg.
开发了一种使用聚合物吸附剂的简单且准确的净化程序,用于测定鲑鱼肌肉中的土霉素(OTC)和四环素(TC)残留。在一个月的时间内,该程序应用于20个鲑鱼样本的分析。OTC和TC残留用pH值为4.0的乙二胺四乙酸(EDTA)-麦克尔维恩缓冲液进行提取,并用聚合物吸附剂通过固相萃取进行净化。描述了聚合物吸附剂相对于硅胶基吸附剂在净化鲑鱼肌肉样本方面的优势。由于其灵敏度和特异性,提出了一种柱后衍生化和荧光检测的液相色谱法。在50、100和200微克/千克水平下加标的鲑鱼肌肉组织中,OTC和TC的平均回收率在83.9%至93.4%之间,变异系数在4.09%至5.80%之间。鲑鱼肌肉中OTC和TC的定量限为50微克/千克。