title: New method for the analysis of lipophilic marine biotoxins in fresh and canned bivalves by liquid chromatography coupled to high resolution mass spectrometry: a quick, easy, cheap, efficient, rugged, safe approach.
abstract: A new method for the analysis of lipophilic marine biotoxins (okadaic acid, dinophysistoxins, azaspiracids, pectenotoxins, yessotoxins, spirolids) in fresh and canned bivalves has been developed. A QuEChERS methodology is applied; i.e. the analytes are extracted with acetonitrile and clean-up of the extracts is performed by dispersive solid phase extraction with C18. The extracts are analyzed by ultra-high performance liquid chromatography coupled to a hybrid quadrupole-Orbitrap mass spectrometer, operating in tandem mass spectrometry mode, with resolution set at 70,000 (m/z 200, FWHM). Separation of the analytes, which takes about 10min, is carried out in gradient elution mode with a BEH C18 column and mobile phases based on 6.7mM ammonia aqueous solution and acetonitrile mixtures. For each analyte the molecular ion and 1 or 2 product ions are acquired, with a mass accuracy better than 5ppm. The quantification is performed using surrogate matrix matched standards, with eprinomectin as internal standard. The high-throughput method, which has been successfully validated, fulfills the requirements of European Union legislation, and has been implemented as a routine method in a public health laboratory.
authors: Laboratori de l'Agència de Salut Pública de Barcelona, Avinguda Drassanes 13-15, 08001, Barcelona, Spain; CIBER of Epidemiology and Public Health (CIBERESP), Madrid, Spain. Electronic address: arubies@aspb.cat.
authors: A
authors: A
authors: Rúbies
authors: Laboratori de l'Agència de Salut Pública de Barcelona, Avinguda Drassanes 13-15, 08001, Barcelona, Spain; CIBER of Epidemiology and Public Health (CIBERESP), Madrid, Spain.
authors: E
authors: E
authors: Muñoz
authors: Department of Analytical Chemistry, University of Barcelona, Martí Franquès 1-11, 08028, Barcelona, Spain.
authors: D
authors: D
authors: Gibert
authors: Laboratori de l'Agència de Salut Pública de Barcelona, Avinguda Drassanes 13-15, 08001, Barcelona, Spain; Mass Spectrometry Laboratory/Organic Pollutants, IDAEA-CSIC, c/Jordi Girona, 18-26, 08034 Barcelona, Spain.
authors: N
authors: N
authors: Cortés-Francisco
authors: Department of Analytical Chemistry, University of Barcelona, Martí Franquès 1-11, 08028, Barcelona, Spain.
authors: M
authors: M
authors: Granados
authors: Mass Spectrometry Laboratory/Organic Pollutants, IDAEA-CSIC, c/Jordi Girona, 18-26, 08034 Barcelona, Spain.
authors: J
authors: J
authors: Caixach
authors: Laboratori de l'Agència de Salut Pública de Barcelona, Avinguda Drassanes 13-15, 08001, Barcelona, Spain; CIBER of Epidemiology and Public Health (CIBERESP), Madrid, Spain.
authors: F
authors: F
authors: Centrich
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D000641:Ammonia / Q000737:chemistry; D000818:Animals; D049872:Bivalvia / Q000737:chemistry* / Q000378:metabolism; D002851:Chromatography, High Pressure Liquid; D005504:Food Analysis / Q000379:methods*; D008387:Marine Toxins / Q000032:analysis* / Q000302:isolation & purification; D008978:Mollusk Venoms; D019319:Okadaic Acid / Q000032:analysis / Q000302:isolation & purification; D035964:Oxocins / Q000032:analysis / Q000302:isolation & purification; D052616:Solid Phase Extraction; D013141:Spiro Compounds / Q000032:analysis / Q000302:isolation & purification; D053719:Tandem Mass Spectrometry; D000095702:Polyether Toxins
chemical_list: D000097:Acetonitriles; D000641:Ammonia; D008387:Marine Toxins; D008978:Mollusk Venoms; D019319:Okadaic Acid; D035964:Oxocins; D013141:Spiro Compounds; C406592:azaspiracid; D000095702:Polyether Toxins; C066632:yessotoxin; C032159:acetonitrile
keywords: Bivalve samples; High resolution mass spectrometry; Lipophilic marine biotoxins; Liquid chromatography