Analytical Sciences

Indirect Quantitation of Saxitoxin by HPLC with Post-column Oxidation and Fluorometric Detection

Ryuichi WATANABE,* Tomoko HARADA,* Ryoji MATSUSHIMA,* Hiroshi OIKAWA,** Yasukatsu OSHIMA,*** Masaki KANENIWA,* and Toshiyuki SUZUKI*

*National Research Institute of Fisheries Science, 2-12-4 Fukuura, Kanazawa, Yokohama 236-8648, Japan
**National Research Institute of Fisheries and Environment of Inland Sea, 2-12-4 Maruishi, Hatsukaichi, Hiroshima 739-0452, Japan
***School of Marine Bioscience, Kitasato University, 1-15-1 Kitasato, Minami, Sagamihara 252-0373, Japan

The indirect identification and quantification of saxitoxin (STX) using other STX analogues by high-performance liquid chromatography with post-column oxidation and fluorescent detection (HPLC-FD) was investigated. Decarbamoylsaxitoxin (dcSTX) among the many STX analogues was selected as an external standard to identify and quantify STX. The retention time of STX in shellfish extracts by HPLC-FD was reproducibly estimated by using the retention time of dcSTX and the separation factor (α) between STX and dcSTX. Almost all of the columns tested to setup the method were useful to identify STX. Because a molar fluorescent coefficient of dcSTX was slightly different from that of STX, a factor used to correct the fluorescent coefficient in STX/dcSTX was determined to be 1.30. The indirect quantification of STX in scallop extracts by using the correction factor agreed to 80 – 100% precision with direct quantification using STX as an external standard.

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