title: Extension of the validation of AOAC Official Method 2005.06 for dc-GTX2,3: interlaboratory study.
abstract: AOAC Official Method(SM) 2005.06 for the determination of saxitoxin (STX)-group toxins in shellfish by LC with fluorescence detection with precolumn oxidation was previously validated and adopted First Action following a collaborative study. However, the method was not validated for all key STX-group toxins, and procedures to quantify some of them were not provided. With more STX-group toxin standards commercially available and modifications to procedures, it was possible to overcome some of these difficulties. The European Union Reference Laboratory for Marine Biotoxins conducted an interlaboratory exercise to extend AOAC Official Method 2005.06 validation for dc-GTX2,3 and to compile precision data for several STX-group toxins. This paper reports the study design and the results obtained. The performance characteristics for dc-GTX2,3 (intralaboratory and interlaboratory precision, recovery, and theoretical quantification limit) were evaluated. The mean recoveries obtained for dc-GTX2,3 were, in general, low (53.1-58.6%). The RSD for reproducibility (RSD(r)%) for dc-GTX2,3 in all samples ranged from 28.2 to 45.7%, and HorRat values ranged from 1.5 to 2.8. The article also describes a hydrolysis protocol to convert GTX6 to NEO, which has been proven to be useful for the quantification of GTX6 while the GTX6 standard is not available. The performance of the participant laboratories in the application of this method was compared with that obtained from the original collaborative study of the method. Intralaboratory and interlaboratory precision data for several STX-group toxins, including dc-NEO and GTX6, are reported here. This study can be useful for those laboratories determining STX-group toxins to fully implement AOAC Official Method 2005.06 for official paralytic shellfish poisoning control. However the overall quantitative performance obtained with the method was poor for certain toxins.
authors.affiliation: European Union Reference Laboratory for Marine Biotoxins (EURLMB), CITEXVI, Campus Universitario de Vigo, Fonte das Abelleiras SN, 36310 Vigo, Spain.
authors.forename: Begoña
authors.initials: B
authors.lastname: Ben-Gigirey
authors.forename: María L
authors.initials: ML
authors.lastname: Rodríguez-Velasco
authors.forename: Ana
authors.initials: A
authors.lastname: Gago-Martínez
mesh_terms: D000465:Algorithms; D000818:Animals; D049872:Bivalvia; D002851:Chromatography, High Pressure Liquid; D006868:Hydrolysis; D007202:Indicators and Reagents; D008387:Marine Toxins / Q000032:analysis*; D010125:Ostreidae; D010084:Oxidation-Reduction; D010504:Periodic Acid / Q000737:chemistry; D010545:Peroxides / Q000737:chemistry; D012015:Reference Standards; D015203:Reproducibility of Results; D012530:Saxitoxin / Q000032:analysis*; D057096:Shellfish Poisoning; D013050:Spectrometry, Fluorescence / Q000379:methods
chemical_list: D007202:Indicators and Reagents; D008387:Marine Toxins; D010545:Peroxides; D010504:Periodic Acid; D012530:Saxitoxin