Kobayashi Maki, Nagayama Toshihiro, Takano Ichiro, Tamura Yasuhiro, Kimura Naoko, Kitayama Kyoko, Saito Kazuo
Tokyo Metropolitan Research Laboratory of Public Health: 3-24-1, Hyakunin-cho, Shinjuku-ku, Tokyo 169-0073, Japan.
Shokuhin Eiseigaku Zasshi. 2002 Jun;43(3):133-43. doi: 10.3358/shokueishi.43.133.
We investigated the determination of N-methylcarbamate pesticides and their metabolites in agricultural products by HPLC with post-column fluorescence detection after clean-up with an SPE cartridge. The homogenate of agricultural products 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 with a mixture of acetone and n-hexane, and purified by using Supelclean ENVI-Carb SPE, Bond Elut Extraction Cartridge PSA and SAX in series with a mixture of acetone and n-hexane. N-Methylcarbamate pesticide was analyzed by HPLC with post-column reaction and fluoresce detection. N-Methylcarbamate pesticide in citrus fruits and various kinds of agricultural products could be analyzed accurately by the presented method. Recoveries of N-methylcarbamate pesticides added to several agricultural products at the level of 0.10 ppm were mostly in the range of 60-110%. The limit of detection was 0.005 ppm.
我们研究了采用固相萃取小柱净化后,通过柱后荧光检测的高效液相色谱法测定农产品中氨基甲酸甲酯类农药及其代谢物的方法。农产品匀浆用丙酮提取。粗提取物在5%氯化钠溶液和二氯甲烷之间进行分配,二氯甲烷层浓缩至干。残渣用丙酮和正己烷的混合物溶解,并依次使用Supelclean ENVI-Carb固相萃取小柱、Bond Elut萃取小柱PSA和SAX,以丙酮和正己烷的混合物进行净化。氨基甲酸甲酯类农药通过柱后反应和荧光检测的高效液相色谱法进行分析。所提出的方法能够准确分析柑橘类水果和各类农产品中的氨基甲酸甲酯类农药。在几种农产品中添加浓度为0.10 ppm的氨基甲酸甲酯类农药,回收率大多在60%-110%范围内。检测限为0.005 ppm。