Goodspeed D P, Simpson R M, Ashworth R B, Shafer J W, Cook H R
J Assoc Off Anal Chem. 1978 Sep;61(5):1050-3.
Free and conjugated sulfonamides are extracted from edible animal tissue with acetone. Carbohydrate is precipitated and removed, and the acetone is evaporated. The residue is transferred to a separatory funnel with ethyl ether and 1N HCl. The acid layer is drawn off and a portion of the 1N HCl is screened, using the Bratton-Marshall reaction. If this portion is positive, the remaining portion is buffered to pH 6.5 and extracted with methylene chloride. The residue is methylated with diazomethane and then acylated with pentafluoropropionic anhydride. The resulting derivatives are detected by gas-liquid chromatography, using electron capture (63Ni) detection and a column packed with 3% OV-17 on Gas-Chrom Q. This method has been validated by recovering sulfathiazole, sulfachloropyrazine, sulfamethazine, sulfadimethoxine, and sulfabromomethazine from liver, kidney, and muscle at levels of 0.1, 0.5, and 1.0 ppm. The 5 sulfonamides were recovered in excess of 60%, with an average mean recovery of 81.5% at the 0.1 ppm level, 79.1% at the 0.5 ppm level, and 76.0% at the 1.0 ppm level.
游离和结合的磺胺类药物用丙酮从食用动物组织中提取。碳水化合物沉淀并去除，丙酮蒸发。残留物转移至分液漏斗，加入乙醚和1N盐酸。放出酸层，用布氏-马歇尔反应检测一部分1N盐酸。如果该部分呈阳性，则将其余部分缓冲至pH 6.5，并用二氯甲烷萃取。残留物用重氮甲烷甲基化，然后用五氟丙酸酐酰化。所得衍生物通过气液色谱法检测，采用电子捕获（63Ni）检测，色谱柱填充有3% OV-17的Gas-Chrom Q。该方法已通过从肝脏、肾脏和肌肉中回收噻唑磺胺、氯吡嗪磺胺、磺胺二甲嘧啶、磺胺二甲氧嘧啶和磺胺溴甲嘧啶进行验证，回收水平分别为0.1、0.5和1.0 ppm。5种磺胺类药物的回收率超过60%，在0.1 ppm水平下平均回收率为81.5%，在0.5 ppm水平下为79.1%，在1.0 ppm水平下为76.0%。
