Results of a European interlaboratory method validation study for the quantitative determination of lipophilic marine biotoxins in raw and cooked shellfish based on high-performance liquid chromatography-tandem mass spectrometry. Part I: collaborative study.
A European interlaboratory collaborative study was conducted to validate a method for the quantitative determination of lipophilic marine biotoxins based on high-performance liquid chromatography-tandem mass spectrometry. During this study, the diarrhetic shellfish poisoning toxins okadaic acid, dinophysis toxin1 and 2 including their esters, the azaspiracids 1-3, pectenotoxin2, and the yessotoxins were investigated at concentration levels near the limit of quantification and near the legal limit. Naturally contaminated blue mussels, both raw and cooked and spiked extracts of clams and oysters were studied and results were obtained for 16 test samples from 16 laboratories representing eight different countries. This article summarizes the study outcome concerning validation key parameters like specificity, linearity, limit of detection, accuracy/recovery, and precision. Further, influences of cooking of mussels before homogenization or hydrolysis on method robustness have been evaluated.
Federal Institute for Risk Assessment-National Reference Laboratory for Marine Biotoxins Germany, Thielallee 88-92, 14195 Berlin, Germany. anja.these@bfr.bund.de
Anja
A
These
Christine
C
Klemm
Ingo
I
Nausch
Steffen
S
Uhlig
D000818:Animals; D002851:Chromatography, High Pressure Liquid; D003296:Cooking; D005060:Europe; D005504:Food Analysis / Q000379:methods*; D007391:International Cooperation; D008387:Marine Toxins / Q000032:analysis*; D019319:Okadaic Acid / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012758:Shellfish / Q000032:analysis*; D053719:Tandem Mass Spectrometry
D008387:Marine Toxins; D019319:Okadaic Acid