CHROMATOGRAPHY, Vol. 23 (2002), No. 2, pp. 73-78

Highly Sensitive Time-Resolved Fluorometric Determination for Alkylphenols by High Performance Liquid Chromatography Using -Diketonate Europium Chelate
Takeshi Matsuya1*, Kazuhiko Ohtake1, Nobuhiro Hoshino1, Minoru Ogasawara1, Tatsuyuki Harita1, Shinsuke Arao1 and Kazuko Matsumoto2
1 Iatron Laboratories, Inc. 1460-6, Mitodai, Mito, Takomachi, Katori-gun, Chiba 289-2247, Japan
2 Department of Chemistry, Advanced Research Center for Science & Engineering, Waseda University 3-4-1, Ohkubo, Shinjuku-ku, Tokyo 169-8555, Japan

A time-resolved fluorescence detection system by HPLC for alkylphenols has been developed using a europium chelate fluorescent labeling reagent, 4-(1,1,1,2,2-pentafluoro-3,5-dioxo-pentyl)-[1,11'-biphenyl]-4'-sulfonyl-chloride (PDB-SCl). The labeling reaction was on to phenolic hydroxyl group of alkylphenols, and the derivatized alkylphenols were separated on a HPLC column. After separation, EuCl3, TOPO (tri-n-octylphosphine oxide), and Triton X-100 were introduced to the eluent, and the fluorescence of the europium chelate was measured with the time-resolved phosphorescence detector. The detection limit for 4-nonylphenol in the time-resolved fluorometric HPLC method was 4 to 65 times lower than that of the commonly used LC-MS method. The detection limits for 4-nonylphenol in the river water sample was 0.99 ng/L. The average recovery from river water samples was 64.8%. The precision of the method ranged from 2.5 to 5.9%. Using this method, the concentration of 4-nonylphenol in a river water sample was 4.8 ng/L.
Keywords: alkylphenols; time-resolved fluorescence; HPLC; Eu chelate; river water

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