title: High-throughput analysis of amnesic shellfish poisoning toxins in shellfish by ultra-performance rapid resolution LC-MS/MS.
abstract: The application of ultra-performance rapid resolution LC on a 1.8 microm particle-size column coupled with tandem MS (RRLC-MS/MS) is described for the analysis of amnesic shellfish poisoning (ASP) toxins in shellfish. Complete resolution among domoic acid (DA) and the isomers was achieved in less than 3 min. The method was intralaboratory validated for direct analysis of crude extracts without further cleanup. It showed LODs ranging from 0.05 to 0.09 mg/kg and a working range that complied with the current regulatory level for DA of 20 mg/kg, and with the level of 4.5 mg/kg recently proposed by the European Food Safety Authority. Confirmatory capabilities were demonstrated according to the Commission Decision 2002/657/EC criteria. The results obtained by RRLC-MS/MS agreed with those provided by the reference LC-UV method, both intralaboratory for the analysis of blind samples (R2 = 0.9751) and interlaboratory through participation in the proficiency test for ASP toxins during 2009 (z-score = -0.962 and 0.177 for low- and high-contaminated samples, respectively). RRLC-MS/MS provided fast analysis and additional confirmatory capabilities for direct analysis of crude extracts while the performance and reliability of the results were maintained, even in very complex matrixes.
authors.affiliation: Institut de Recerca i Tecnologia Agroalimentàries (IRTA), Ctra. Poble Nou, km, 5.5, 43540, Sant Carles de la Ràpita, Tarragona, Spain. pablo.delaiglesia@irta.cat
authors.forename: Pablo
authors.initials: P
authors.lastname: de la Iglesia
authors.forename: Esther
authors.initials: E
authors.lastname: Barber
authors.forename: Gemma
authors.initials: G
authors.lastname: Giménez
authors.forename: María Luisa
authors.initials: ML
authors.lastname: Rodríguez-Velasco
authors.forename: Adriano
authors.initials: A
authors.lastname: Villar-González
authors.forename: Jorge
authors.initials: J
authors.lastname: Diogène
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D006801:Humans; D015394:Molecular Structure; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012758:Shellfish / Q000032:analysis*; D057096:Shellfish Poisoning / Q000517:prevention & control*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013997:Time Factors; D014118:Toxins, Biological / Q000737:chemistry*
chemical_list: D014118:Toxins, Biological