Simultaneous Determination of 21 N-Methylcarbamates and 12 Metabolites in Agricultural Products by HPLC
Simultaneous Determination of 21 N-Methylcarbamates and 12 Metabolites in Agricultural Products by HPLC
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HPLC同时测定农产品中21种N-甲基氨基甲酸酯和12种代谢物
DOI：
10.3358/shokueishi.39.6_357
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发表时间：
1998
期刊：
影响因子：
--
通讯作者：
T. Shibata
中科院分区：
文献类型：
--
作者：
Y. Tsumura;Yumiko Nakamura;K. Yoshii;Y. Tonogai;Mamiko Higo;T. Shibata
同时测定了农产品中21种N-甲基氨基甲酸酯（NMCs）和12种代谢物或异构体。由于用乙酸乙酯代替二氯甲烷完成萃取，因此具有硫醚基团的NMCs部分氧化为亚砜。将其定量为氧化和非氧化化合物的总量。用丙酮提取食品样品中的NMCs，然后蒸去丙酮，加入氯化钠，再用乙酸乙酯提取。蒸发萃取液，残留物在乙腈和正己烷之间分配。将乙腈层蒸发，并将残余物在Sep-Pak®氨基丙基柱上净化。通过HPLC结合柱后反应和荧光检测来测定匪C。在添加水平为0.1 ~ 1 ppm时，除丁羧肟亚砜外，大米、洋葱、苹果等10种农产品中NMCs的回收率为56.9 ~ 108.2%。主要NMCs的检测限为0.01 ppm。
Twenty-one N-methylcarbamates (NMCs) and 12 metabolites or isomers in agricultural products were simultaneously determined. As extraction was accomplished with ethyl actate instead of dichloromethane, NMCs possessing a thioether group were partly oxidized to sulfoxides. They were quantified as total amount of oxidized and non-oxidized compounds. NMCs in food samples were extracted with acetone, then the acetone was evaporated off and sodium chloride was added before extraction with ethyl acetate. The extract was evaporated and the residue was partitioned between acetonitrile and n-hexane. The acetonitrile layer was evaporated and the residue was cleaned up on a Sep-Pak® aminopropyl cartridge. NMCs were determined by HPLC with post-column reaction and fluorescence detection. Recoveries of NMCs from 10 kinds of agricultural products including rice, onion and apple were 56.9 to 108.2%, except for butocarboxim sulfoxide, at fortification levels of 0.1 to 1ppm. Detection limits were 0.01ppm for major NMCs.