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气相色谱法测定猪和牛组织中的磺胺二甲嘧啶

Gas-liquid chromatographic determination of sulfamethazine in swine and cattle tissues.

作者信息

Manuel A J, Steller W A

出版信息

J Assoc Off Anal Chem. 1981 Jul;64(4):794-9.

PMID:7275892
Abstract

A gas-liquid chromatographic (GLC) method is described for determining sulfonamide residues in animal tissues, with specificity for 7 sulfonamides. Residues are extracted from tissues with acetone-chloroform, fatty substances are removed, and the sulfonamide residue is methylated with diazomethane in acetone-ether to render it amenable to determination by gas-liquid chromatography on an all-glass column suitable for direct on-column injection and a Ni electron-capture detector. Quantitation is achieved by external standardization. The method has a validated limit of sensitivity of 0.10 ppm with the corresponding control values for all tissues being less than 0.01 ppm. Satisfactory recoveries have been obtained for sulfamethazine in swine and cattle tissues. Specificity for sulfamethazine in the presence of sulfathiazole, sulfaquinoxaline, sulfadimethoxine, sulfabromomethazine, sulfaethoxypyridazine, and sulfachloropyrazine is attained by resolution of the respective methyl derivatives on the GLC column.

摘要

描述了一种气相色谱(GLC)方法,用于测定动物组织中的磺胺类药物残留,该方法对7种磺胺类药物具有特异性。用丙酮 - 氯仿从组织中提取残留物,去除脂肪物质,然后在丙酮 - 乙醚中用重氮甲烷将磺胺类药物残留甲基化,使其适合在适用于直接柱上进样的全玻璃柱和镍电子捕获检测器上进行气相色谱测定。通过外标法进行定量。该方法的有效灵敏度极限为0.10 ppm,所有组织的相应对照值均小于0.01 ppm。在猪和牛组织中,磺胺二甲嘧啶的回收率令人满意。通过在GLC柱上分离各自的甲基衍生物,可实现磺胺二甲嘧啶在磺胺噻唑、磺胺喹恶啉、磺胺二甲氧嘧啶、磺胺溴甲嘧啶、磺胺乙氧哒嗪和磺胺氯吡嗪存在下的特异性测定。

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