title: Comparison of different fluorimetric HPLC methods for analysis of acidic polyether toxins in marine phytoplankton.
abstract: The human toxic syndrome, diarrhetic shellfish poisoning (DSP), is caused by polyether toxins that are present in bivalve molluscs but originate from some species of marine phytoplankton. During the last few years different HPLC methods with fluorescence detection (FLD) have been proposed for analysis of marine toxins, including polyether toxins, in shellfish and phytoplankton. Several derivatization reagents have been proposed in the literature, with the aim of converting the acidic DSP toxins into their corresponding fluorescent derivatives. In this work we report results obtained from HPLC-FLD analysis of extracts from phytoplankton, including Dinophysis spp.,harvested off the south-west coast of Ireland. Three different reagents were used for fluorescent derivatization: 3-bromomethyl-6,7-dimethoxy-1-methyl-2(1H)-quinoxalinone (BrDMEQ), 9-chloromethylanthracene (CA), and "in situ" 9-anthracenyldiazomethane (ADAM). Derivatization was performed under conditions previously optimised. The DSP derivatives were cleaned using different SPE procedures then analysed by HPLC-FLD. In this study, the use of BrDMEQ, CA, and "in situ" ADAM was compared in terms of sensitivity and selectivity. Evaluation of HPLC methods for analysis of DSP toxin derivatives was also conducted; the presence of okadaic acid (OA), dinophysistoxin-2 (DTX-2), and pectenotoxin-2 seco acids (PTX1SAs) was detected in the sample extracts studied.
authors.affiliation: Departamento de Química Analítica y Alimentaria y Departamento de Química Orgánica, Campus Universitario Vigo, Universidad de Vigo, 36200 Vigo, España.
authors.forename: M J
authors.initials: MJ
authors.lastname: Nogueiras
authors.forename: Ana
authors.initials: A
authors.lastname: Gago-Martínez
authors.forename: Antonio I
authors.initials: AI
authors.lastname: Paniello
authors.forename: Marian
authors.initials: M
authors.lastname: Twohig
authors.forename: Kevin J
authors.initials: KJ
authors.lastname: James
authors.forename: James F
authors.initials: JF
authors.lastname: Lawrence
mesh_terms: D000818:Animals; D000873:Anthracenes / Q000737:chemistry; D001391:Azo Compounds / Q000737:chemistry; D049872:Bivalvia / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003967:Diarrhea / Q000209:etiology; D004987:Ethers / Q000032:analysis; D005470:Fluorometry / Q000379:methods*; D006801:Humans; D007494:Ireland; D008387:Marine Toxins / Q000032:analysis* / Q000737:chemistry; D010839:Phytoplankton / Q000737:chemistry*; D011810:Quinoxalines / Q000737:chemistry
chemical_list: C481027:9-anthracenyldiazomethane; D000873:Anthracenes; D001391:Azo Compounds; D004987:Ethers; D008387:Marine Toxins; D011810:Quinoxalines; C052465:3-bromomethyl-6,7-dimethoxy-1-methyl-2(1H)-quinoxalinone; C099162:9-chloromethylanthracene