作者: Kazuaki AKASAKA , Hiroshi OHRUI , Hiroshi MEGURO , Takeshi YASUMOTO
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摘要: A highly sensitive HPLC method for the determination of acid dinophysis toxins-3 (DTX-3s; 7-O-acyl-35-methylokadaic acids) by labeling 2-(anthracene-2, 3-dicarboximido)ethyl trifluoromethanesulfonate (AE-OTf) has been reported. The digestive glands mussels or scallops were homogenized with 2-propanol, followed extraction hexane/ethyl acetate. After evaporation solvent, they labeled AE-OTf in dry acetonitrile. Then, after cleaning up a silica-gel short column, fluorescent derivatives injected into an system. In this system, at first separated on phenylated silicagel column; then, only target fraction was introduced separation column (an ODS column) valve device switching column. 7-O-palmitoyl DTX-3 derivative could be determined range 1.4-284fmol (1.5-300pg) detection limit 0.57fmol (0.6pg, S/N=3).