Orejuela Eva, Silva Manuel
Department of Analytical Chemistry, Campus of Rabanales, University of Córdoba, E-14004 Córdoba, Spain.
J Chromatogr A. 2003 Jul 25;1007(1-2):197-201. doi: 10.1016/s0021-9673(03)00934-8.
A systematic investigation of optimal conditions for determining three of the most common phenoxyl-type N-methylcarbamate pesticides (carbaryl, carbofuran and propoxur) in fruit juices by HPLC with peroxyoxalate-chemiluminescence detection is described. The required pre-column hydrolysis of pesticides and derivatization of their hydrolytic metabolites with dansyl chloride was simultaneously carried out in a short time thanks to the micellar catalytic effect provided by cetyltrimethyl ammonium bromide micelles on the hydrolysis step. The liquid chromatographic separation of the dansylated phenols was performed on a reversed-phase C18 column with isocratic elution. The analytes were detected by using an integrated derivatization chemiluminescence detection unit based on the bis(2,4,6-trichlorophenyl)oxalate-hydrogen peroxide system. Fruit juice samples containing 4.0-1500 microg/l pesticides were analysed with a precision of ca. 6.5%. After contamination of the fruit juice samples, average recovery > 93% at fortification levels of 10-100 microg/l was obtained.
本文描述了通过高效液相色谱-过氧草酸酯化学发光检测法，对果汁中三种最常见的苯氧基型氨基甲酸甲酯类农药（西维因、克百威和残杀威）进行测定的最佳条件的系统研究。由于十六烷基三甲基溴化铵胶束在水解步骤中提供的胶束催化作用，所需的农药柱前水解及其水解代谢物与丹磺酰氯的衍生化反应在短时间内同时进行。丹磺酰化酚类的液相色谱分离在反相C18柱上进行等度洗脱。使用基于双（2,4,6-三氯苯基）草酸酯-过氧化氢体系的集成衍生化化学发光检测单元对分析物进行检测。对含有4.0-1500微克/升农药的果汁样品进行分析，精密度约为6.5%。果汁样品受污染后，在10-100微克/升的加标水平下，平均回收率>93%。
