Woolley J L, Murch O, Sigel C S
J Assoc Off Anal Chem. 1978 May;61(3):545-9.
Because of the lack of specificity of the Bratton-Marshall procedure for assaying sulfonamides, a sensitive, specific tissue residue assay for sulfadiazine (SDZ) was developed. The methodology has been extended to provide a highly sensitive screen for sulfonamide residues, which employs 2-dimensional thin layer chromatography in conjunction with fluorescamine derivatization. The procedure described, which has been developed for SDZ in calf tissues, involves direct ethyl acetate extraction of tissue homogenates. Following evaporation of the organic phase, a portion of the residue is spotted on a 20 X 20 cm silica gel 60 plate, which is then developed in 2 dimensions with solvent systems devised to separate SDZ from endogenous substances as well as from 12 other sulfonamides that might be present in calf tissues. The presence of SDZ at a concentration of 0.1 ppm or its absence is easily demonstrated in calf kidney, liver, muscle, plasma, and urine. The basic method can be modified for a particular sulfonamide in a target tissue and can be used as a quantitative assay for sulfonamide residues.
由于用于检测磺胺类药物的布拉顿 - 马歇尔方法缺乏特异性，因此开发了一种灵敏、特异的磺胺嘧啶（SDZ）组织残留检测方法。该方法已得到扩展，以提供一种高度灵敏的磺胺类药物残留筛查方法，该方法采用二维薄层色谱结合荧光胺衍生化技术。所描述的方法是针对小牛组织中的SDZ开发的，包括直接用乙酸乙酯提取组织匀浆。有机相蒸发后，将一部分残留物点在20×20 cm的硅胶60板上，然后用设计用于将SDZ与内源性物质以及小牛组织中可能存在的其他12种磺胺类药物分离的溶剂系统进行二维展开。在小牛的肾脏、肝脏、肌肉、血浆和尿液中，很容易检测到浓度为0.1 ppm的SDZ是否存在。该基本方法可针对目标组织中的特定磺胺类药物进行修改，并可用于磺胺类药物残留的定量检测。
