title: Liquid chromatographic determination of okadaic acid and dinophysistoxin-1 in shellfish after derivatization with 9-chloromethylanthracene.
abstract: The reagent 9-chloromethylanthracene was evaluated for derivatization of the diarrhetic shellfish poisons, okadaic acid and dinophysistoxin-1 (DTX-1), to form fluorescent products separable by liquid chromatography. The toxins were reacted with the reagent in acetonitrile in the presence of tetramethylammonium hydroxide for 1 h at 90 degrees C. The products were purified by using two silica solid-phase extraction cartridges before being determined by reversed-phase liquid chromatography with fluorescence detection. The results are comparable to those obtained using 9-anthryldiazomethane (ADAM) for okadaic acid and DTX-1 in mussel tissue. Detection limits were estimated to be about 70-100 ng/g hepatopancreas (equivalent to 12-20 ng/g whole tissue) for each toxin.
authors.affiliation: Food Research Division, Health Canada, Ottawa, Ontario.
authors.forename: J F
authors.initials: JF
authors.lastname: Lawrence
authors.forename: S
authors.initials: S
authors.lastname: Roussel
authors.forename: C
authors.initials: C
authors.lastname: Ménard
mesh_terms: D000818:Animals; D000873:Anthracenes; D049872:Bivalvia; D002853:Chromatography, Liquid / Q000379:methods*; D003967:Diarrhea / Q000139:chemically induced; D004988:Ethers, Cyclic / Q000032:analysis*; D007202:Indicators and Reagents; D008387:Marine Toxins / Q000032:analysis*; D019319:Okadaic Acid / Q000031:analogs & derivatives; D011714:Pyrans / Q000032:analysis*; D012758:Shellfish / Q000032:analysis*
chemical_list: D000873:Anthracenes; D004988:Ethers, Cyclic; D007202:Indicators and Reagents; D008387:Marine Toxins; D011714:Pyrans; D019319:Okadaic Acid; C099162:9-chloromethylanthracene; C051904:dinophysistoxin 1