title: Quantitative determination of marine toxins associated with diarrhetic shellfish poisoning by liquid chromatography coupled with mass spectrometry.
abstract: Quantitative determination by liquid chromatography (LC) coupled with mass spectrometry (MS) was achieved for the following 10 toxins found in association with diarrhetic shellfish poisoning: okadaic acid (OA), dinophysistoxin-1 (DTX1), 7-O-palmitoylokadaic acid (palOA), 7-O-palmitoyldinophysistoxin-1 (pa1DTX1), pectenotoxin-1 (PTX1), pectenotoxin-2 (PTX2), pectenotoxin-2 seco acid (PTX2SA), pectenotoxin-6 (PTX6), yessotoxin (YTX), and 45-hydroxyyessotoxin (YTXOH). Toxins in 2 g of the adductor muscle or the digestive glands of scallops, Patinopecten yessoensis, were extracted with 18 ml of methanol-water (9:1, v/v), freed of polar contaminants by partition between chloroform and water, and treated by solid-phase extraction on a silica cartridge column. Samples containing YTXOH were purified separately on a buffered reversed-phase column. Chromatographic separation was achieved by the following combinations of columns and mobile phases: a Symmetry C18 column with acetonitrile-0.05% acetic acid (7:3, v/v) for OA, DTX1, PTX6 and PTX2SA; a Develosil ODS column with the same mobile phase for PTX1 and PTX2; a Capcellpak column with methanol-2.5% acetic acid (98:2, v/v) for palOA and palDTX1; and an Inertsil ODS column with methanol-0.2 M ammonium acetate (8:2, v/v) for YTX and YTXOH. Carboxylic acid toxins were selectively monitored on [M-H]- ions, sulfated toxins on [M-Na]-ions, and neutral toxins on [M+NH4]+ ions. Average recoveries of the toxins spiked to tissue homogenates ranged from 70 to 134%. Detection limits in the muscle ranged from 5 to 40 ng/g and those in the digestive glands from 10 to 80 ng/g.
authors.affiliation: Japan Food Research Laboratories, Tama Laboratory, Tokyo, Japan.
authors.forename: H
authors.initials: H
authors.lastname: Goto
authors.forename: T
authors.initials: T
authors.lastname: Igarashi
authors.forename: M
authors.initials: M
authors.lastname: Yamamoto
authors.forename: M
authors.initials: M
authors.lastname: Yasuda
authors.forename: R
authors.initials: R
authors.lastname: Sekiguchi
authors.forename: M
authors.initials: M
authors.lastname: Watai
authors.forename: K
authors.initials: K
authors.lastname: Tanno
authors.forename: T
authors.initials: T
authors.lastname: Yasumoto
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D003967:Diarrhea / Q000139:chemically induced*; D008387:Marine Toxins / Q000032:analysis* / Q000506:poisoning; D013058:Mass Spectrometry / Q000379:methods*; D012680:Sensitivity and Specificity
chemical_list: D008387:Marine Toxins