Zou Qiong-Hui, Xie Meng-Xia, Wang Xiang-Feng, Liu Yuan, Wang Jin, Song Jia, Gao Hui, Han Jie
Analytical & Testing Center of Beijing Normal University, Beijing China.
J Sep Sci. 2007 Nov;30(16):2647-55. doi: 10.1002/jssc.200700241.
A novel approach for simultaneous determination of 12 sulphonamides (sulphadiazine, sulphamethazine, sulphathiazole, sulphadimethoxine, sulphamerazine, sulphapyridine, sulphamethoxazole, suphamethizole, sulphaquinoxaline, sulphameter, sulphamonomethoxine, and sulphachloropyridazine) in animal tissues (swine muscle and liver, chicken muscle, beef muscle) by HPLC with UV detection has been developed. A pre-column derivatization of the sulphonamide compounds with 9-fluorenylmethyl chloroformate (FMOC-Cl) has been proposed and the reaction conditions have been optimized. The FMOC-sulphonamide derivatives were purified by SPE with silica gel as solid support prior to HPLC separation. The limits of detection for the sulphonamide compounds were greatly improved after the derivatization and purification step for the derivatives. Sulphonamide residues in animal tissues were extracted by acetonitrile and purified by solid phase extraction with C(18) as the solid support. The method developed has high sensitivity and good repeatability, and the average recoveries for most of the sulphonamides at various spiking levels were above 70% with relative standard deviations below 13.7%. The limits of detection for most sulphonamides can reach 3-5 microg/kg.
已开发出一种通过高效液相色谱-紫外检测同时测定动物组织（猪肌肉和肝脏、鸡肌肉、牛肌肉）中12种磺胺类药物（磺胺嘧啶、磺胺二甲嘧啶、磺胺噻唑、磺胺二甲氧嘧啶、磺胺甲嘧啶、磺胺吡啶、磺胺甲恶唑、磺胺甲噻二唑、磺胺喹恶啉、磺胺间甲氧嘧啶、磺胺对甲氧嘧啶和磺胺氯哒嗪）的新方法。提出了用9-芴基甲基氯甲酸酯（FMOC-Cl）对磺胺类化合物进行柱前衍生化，并对反应条件进行了优化。在进行高效液相色谱分离之前，用硅胶作为固相载体通过固相萃取对FMOC-磺胺衍生物进行纯化。对衍生物进行衍生化和纯化步骤后，磺胺类化合物的检测限得到了极大提高。动物组织中的磺胺类药物残留用乙腈提取，并用C(18)作为固相载体通过固相萃取进行纯化。所开发的方法具有高灵敏度和良好的重复性，大多数磺胺类药物在不同加标水平下的平均回收率高于70%，相对标准偏差低于13.7%。大多数磺胺类药物的检测限可达3-5微克/千克。
