Simultaneous Determination of N-Methylcarbamate Pesticides in Agricultural Products by Liquid Chromatography
Simultaneous Determination of N-Methylcarbamate Pesticides in Agricultural Products by Liquid Chromatography
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液相色谱法同时测定农产品中N-甲基氨基甲酸酯类农药
DOI：
10.3358/shokueishi.35.470
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发表时间：
1994
期刊：
影响因子：
--
通讯作者：
Y. Tamura
中科院分区：
文献类型：
--
作者：
T. Nagayama;Maki Kobayashi;H. Shioda;M. Morino;Masako Ito;Y. Tamura
研究了柱后荧光衍生高效液相色谱法同时测定农产品中n -甲基氨基甲酸酯类农药。用丙酮提取食品样品匀浆。将粗提物在5%氯化钠溶液和二氯甲烷溶液中分装，二氯甲烷层浓缩干燥。将残留物溶于甲醇中，加入稀盐酸，柱后荧光衍生液相色谱分析。柱后反应系统采用两步反应：n -甲基氨基甲酸酯水解NaOH溶液裂解甲胺，甲胺与邻苯二醛和2-巯基乙醇反应。得到的荧光衍生物在445nm处检测（激发在339nm处）。在0.1ppm水平下，回收率约为90%，变异系数约为5%。样品的检出限为0.005ppm。本方法适用于食品中n -甲基氨基甲酸酯及其代谢物残留量的测定。
Simultaneous determination of N-methylcarbamate pesticides in agricultural products by high performance liquid chromatography with post-column fluorescence derivatization was investigated.The food sample homogenate was extracted with acetone. The crude extract was partitioned between 5% sodium chloride solution and dichloromethane, and the dichloromethane layer was concentrated to dryness. The residue was dissolved in methanol, dilute hydrochloric acid was added and the solution was analyzed by liquid chromatography with post-column fluorescence derivatization. The post-column reaction system uses a two-step reaction: N-methylcarbamate hydrolysis by NaOH solution cleaves off methylamine, which reacts with o-phthalaldehyde and 2-mercaptoethanol. The resulting fluorescent derivative was detected at 445nm (excitation at 339nm). Recovery at the 0.1ppm levels was around 90% with a coefficient of variation of about 5%. The detection limit was 0.005ppm in samples. The method is recommended for determination of residues of N-methylcarbamate and its metabolites in foods.