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 major phase of work was to assign certified values and uncertainties to the toxin analogues representing 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 toxin concentration 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 uncertainties associated with homogeneity, stability and characterization. The commutability of CRM-FDMT1 was assessed by conducting a study of 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 the development and validation of analytical methods.
MCCARRON Pearse;
WRIGHT Elliott;
EMTEBORG Hakan;
QUILLIAM Michael;
2017-01-19
SPRINGER HEIDELBERG
JRC103569
1618-2642,
https://publications.jrc.ec.europa.eu/repository/handle/JRC103569,
10.1007/s00216-016-0004-0,
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