title: Development and validation of a high-performance liquid chromatographic method using fluorimetric detection for the determination of the diarrhetic shellfish poisoning toxin okadaic acid without chlorinated solvents.
abstract: A modification of the high-performance liquid chromatographic method with fluorimetric detection method for the determination of diarrhetic shellfish poisoning toxins was developed to completely avoid the use of dangerous chlorinated solvents. The method was validated for the toxin okadaic acid (OA) over a period of 6 months where 12 calibrations were performed and 72 samples were analyzed. Analysis of toxic and non-toxic mussels, clams and scallops demonstrated its selectivity. Linearity was observed in the tested range of interest for monitoring purposes of edible shellfish, from the limit of detection (0.3 microg OA/g hepatopancreas) to 13 microg OA/g hepatopancreas. Intra-assay precision of the method was 7% RSD at the quantification limit (0.97 microg OA/g hepatopancreas at S/N=10). Accuracy was tested in triplicate recovery experiments from OA-spiked shellfish where recovery ranged from 92 to 106% in the concentration range of 0.8 to 3.6 microg OA/g hepatopancreas. Useful information on critical factors affecting calibration and reproducibility is also reported. Good correlation (R=0.87) was observed between the results of the method and those of the method of Lee, after the analysis of 45 samples of mussels from the galician rias.
authors.affiliation: Departamento de Farmacología, Universidad de Santiago de Compostela, Lugo, Spain.
authors.forename: J C
authors.initials: JC
authors.lastname: González
authors.forename: F
authors.initials: F
authors.lastname: Leira
authors.forename: M R
authors.initials: MR
authors.lastname: Vieytes
authors.forename: J M
authors.initials: JM
authors.lastname: Vieites
authors.forename: A M
authors.initials: AM
authors.lastname: Botana
authors.forename: L M
authors.initials: LM
authors.lastname: Botana
mesh_terms: D002138:Calibration; D017606:Chlorine Compounds / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003967:Diarrhea / Q000209:etiology; D005470:Fluorometry / Q000379:methods*; D006801:Humans; D008978:Mollusk Venoms / Q000737:chemistry*; D019319:Okadaic Acid / Q000032:analysis* / Q000031:analogs & derivatives; D011714:Pyrans / Q000032:analysis; D011786:Quality Control; D012015:Reference Standards; D015203:Reproducibility of Results; D012758:Shellfish; D012997:Solvents / Q000737:chemistry
chemical_list: D017606:Chlorine Compounds; D008978:Mollusk Venoms; D011714:Pyrans; D012997:Solvents; D019319:Okadaic Acid; C051904:dinophysistoxin 1; C076221:dinophysistoxin 2