Holder C L, Thompson H C, Bowman M C
J Chromatogr Sci. 1981 Dec;19(12):625-33. doi: 10.1093/chromsci/19.12.625.
Sulfamethazine, a widely used antibacterial drug additive in feeds for swine, chickens, and cattle, was scheduled for toxicological evaluation because of potential human health hazards associated with its residues in edible animal tissues. Analytical chemical procedures that would ensure proper concentration, homogeneity, and stability of the drug in dosed feed and its safe usage during the animal studies were prerequisites for such toxicological tests. Electron capture gas chromatographic (EC/GC) methods were therefore devised for the analysis of sulfamethazine residues in animal feed, human urine, and wastewater at levels as low as 100, 10, and 10 ppb, respectively. Sample extracts were cleaned up by using liquid/liquid partitioning, and the extracts were subjected to two derivatizations followed by cleanup on a silica gel column. The derivatizations of sulfamethazine consisted of methylation followed by trifluoroacetylation of the primary amine function. Ancillary data concerning stability of the compound in animal feed, water, and as a dry residue on glass, extraction efficiencies, partition values with various solvents, and the analysis of residues in feed by high pressure liquid chromatography (HPLC) at levels as low as 1.0 ppm are presented.
磺胺二甲嘧啶是一种广泛用于猪、鸡和牛饲料中的抗菌药物添加剂，由于其在食用动物组织中的残留可能对人类健康造成危害，因此计划对其进行毒理学评估。确保药物在给药饲料中的浓度、均匀性和稳定性以及在动物研究期间安全使用的分析化学程序是此类毒理学测试的先决条件。因此，设计了电子捕获气相色谱（EC/GC）方法，分别用于分析动物饲料、人尿和废水中低至100、10和10 ppb水平的磺胺二甲嘧啶残留。样品提取物通过液/液分配进行净化，提取物经过两次衍生化，然后在硅胶柱上进行净化。磺胺二甲嘧啶的衍生化包括甲基化，然后是伯胺官能团的三氟乙酰化。还提供了有关该化合物在动物饲料、水中以及玻璃上干燥残留物中的稳定性、提取效率、与各种溶剂的分配值以及通过高压液相色谱（HPLC）分析低至1.0 ppm水平的饲料中残留物的辅助数据。
