通过柱后pH值调节及荧光检测的液相色谱法测定鳟鱼肌肉组织和尿液中的吡咯米酸残留量。

Determination of piromidic acid residues in trout muscle tissue and in urine by liquid chromatography with post-column modification of pH and fluorimetric detection.

作者信息

Durán Merás I, Galeano Díaz T, Salinas López F, Rodríguez Cacéres M I

机构信息

Department of Analytical Chemistry, University of Extremadura, Badajoz, Spain.

出版信息

J Chromatogr B Biomed Sci Appl. 1998 Oct 23;718(1):135-41. doi: 10.1016/s0378-4347(98)00332-6.

DOI:10.1016/s0378-4347(98)00332-6

PMID:9832370

Abstract

A rapid high-performance liquid chromatographic method has been developed to determine piromidic acid in trout muscle tissue and in urine, in the presence of nalidixic, 7-hydroxymethylnalidixic, oxolinic and pipemidic acids and cinoxacin. A Nova-Pak C18 column was used with acetonitrile-4x10(-4) M oxalic acid (40:60, v/v) as the mobile phase. A post-column change of pH was made with NaOH. Fluorimetric detection at 456 nm (lambda ex 275 nm) was used. The instrumental detection limit was 5.91 ng/ml, based on height of peak. Pretreatment of the urine samples was not necessary and fish samples were extracted with sodium hydroxide solutions and cleaned by means of an extraction with chloroform. Detection limit was 147 ng/ml for urine and 5.91 ng/g for trout muscle. Good separation without interference from any other components was obtained. Recovery was better than 87% in urine and better than 72% in trout muscle tissue.

摘要

已开发出一种快速高效液相色谱法，用于在存在萘啶酸、7-羟甲基萘啶酸、恶喹酸、吡哌酸和西诺沙星的情况下，测定鳟鱼肌肉组织和尿液中的吡咯米酸。使用Nova-Pak C18柱，以乙腈-4×10(-4)M草酸（40:60，v/v）作为流动相。用氢氧化钠进行柱后pH值变化。采用在456nm（激发波长275nm）处的荧光检测。基于峰高，仪器检测限为5.91ng/ml。尿液样品无需预处理，鱼样品用氢氧化钠溶液提取，并用氯仿萃取进行净化。尿液的检测限为147ng/ml，鳟鱼肌肉的检测限为5.91ng/g。获得了良好的分离效果，无任何其他成分的干扰。尿液中的回收率优于87%，鳟鱼肌肉组织中的回收率优于72%。