A mussel tissue certified reference material for multiple phycotoxins. Part 4: certification.
A freeze-dried mussel tissue (Mytilus edulis) reference material (CRM-FDMT1) was produced containing multiple groups of shellfish toxins. Homogeneity and stability testing showed the material to be fit for purpose. The next phase of work was to assign certified values and uncertainties to 10 analytes from six different toxin groups. Efforts involved optimizing extraction procedures for the various toxin groups and performing measurements using liquid chromatography-based analytical methods. A key aspect of the work was compensating for matrix effects associated with liquid chromatography-mass spectrometry through standard addition, dilution, or matrix-matched calibration. Certified mass fraction values are reported as mg/kg of CRM-FDMT1 powder as bottled for azaspiracid-1, -2, and -3 (4.10 ± 0.40; 1.13± 0.10; 0.96 ± 0.10, respectively), okadaic acid, dinophysistoxin-1 and -2 (1.59 ± 0.18; 0.68 ± 0.07; 3.57± 0.33, respectively), yessotoxin (2.49 ± 0.28), pectenotoxin-2 (0.66 ± 0.06), 13-desmethylspirolide-C (2.70 ± 0.26), and domoic acid (126 ± 10). Combined uncertainties for the certified values include contributions from homogeneity, stability, and characterization experiments. The commutability of CRM-FDMT1 was assessed by examining the extractability and matrix effects for the freeze-dried material in comparison with its equivalent wet tissue homogenate. CRM-FDMT1 is the first shellfish matrix CRM with certified values for yessotoxins, pectenotoxins or spirolides, and is the first CRM certified for multiple toxin groups. CRM-FDMT1 is a valuable tool for quality assurance of phycotoxin monitoring programs and for analytical method development and validation. Graphical Abstract CRM-FDMT1 is a multi-toxin mussel tissue certified reference material (CRM) to aid in development and validation of analytical methods for measuring the levels of algal toxins in seafood.
Measurement Science and Standards, National Research Council Canada, 1411 Oxford Street, Halifax, Nova Scotia, B3H 3Z1, Canada. pearse.mccarron@nrc-cnrc.gc.ca.
Pearse
P
McCarron
Measurement Science and Standards, National Research Council Canada, 1411 Oxford Street, Halifax, Nova Scotia, B3H 3Z1, Canada.
Elliott
E
Wright
European Commission, Joint Research Centre, Directorate F - Health, Consumers, and Reference Materials, Retieseweg 111, 2440, Geel, Belgium.
Håkan
H
Emteborg
Measurement Science and Standards, National Research Council Canada, 1411 Oxford Street, Halifax, Nova Scotia, B3H 3Z1, Canada.
Michael A
MA
Quilliam
D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D005612:Freeze Drying; D005663:Furans / Q000032:analysis; D007608:Kainic Acid / Q000031:analogs & derivatives / Q000032:analysis; D018942:Macrolides; D008387:Marine Toxins / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D008978:Mollusk Venoms; D049880:Mytilus edulis / Q000737:chemistry*; D019319:Okadaic Acid / Q000032:analysis / Q000031:analogs & derivatives; D035964:Oxocins / Q000032:analysis; D011714:Pyrans / Q000032:analysis; D012015:Reference Standards; D017747:Seafood / Q000032:analysis*; D013141:Spiro Compounds / Q000032:analysis; D000095702:Polyether Toxins
D005663:Furans; D007608:Kainic Acid; D018942:Macrolides; D008387:Marine Toxins; D008978:Mollusk Venoms; D019319:Okadaic Acid; D035964:Oxocins; D011714:Pyrans; D013141:Spiro Compounds; C517170:13-desmethylspirolide C; C406592:azaspiracid; D000095702:Polyether Toxins; C051904:dinophysistoxin 1; C098380:pectenotoxin 2; C012301:domoic acid; C066632:yessotoxin
Azaspiracid; CRM-FDMT1; Dinophysistoxin; Domoic acid; Mytilus edulis; Okadaic acid; Pectenotoxin; Spirolide; Yessotoxin