Interlaboratory evaluation of multiple LC-MS/MS methods and a commercial ELISA method for determination of tetrodotoxin in oysters and mussels

Type Article
Date 2023-03
Language English
Author(s) Turner Andrew DORCID1, Dean Karl JORCID1, Dhanji-Rapkova MonikaORCID1, Dall’ara SoniaORCID2, Pino Florella2, McVey ClaireORCID3, Haughey SimonORCID3, Logan NatashaORCID3, Elliott ChristopherORCID3, Gago-Martinez AnaORCID4, Leao Jose ManuelORCID4, Giraldez JorgeORCID4, Gibbs RyanORCID5, Thomas KristaORCID6, Perez-Calderon RuthORCID6, Faulkner DermotORCID7, McEneny HughORCID7, Savar VeroniqueORCID8, Reveillon DamienORCID8, Hess PhilippORCID8, Arevalo FabiolaORCID9, Lamas J PabloORCID9, Cagide EvaORCID10, Alvarez MercedesORCID10, Antelo AlvaroORCID10, Klijnstra Mirjam DORCID11, Oplatowska-Stachowiak MichalinaORCID12, Kleintjens TimORCID12, Sajic NerminORCID12, Boundy Michael JORCID13, Maskrey Benjamin HORCID14, Harwood D TimORCID15, Jartín Jesús M GonzálezORCID16, Alfonso AmparoORCID16, Botana LuisORCID16
Affiliation(s) 1 : Centre for Environment, Fisheries and Aquaculture Science , Barrack Road, The Nothe, Weymouth, Dorset, DT4 8UB United Kingdom
2 : Fondazione Centro Ricerche Marine , Viale A. Vespucci, 2, 47042 kleintjens FC, Italy
3 : Queen’s University Belfast, Institute for Global Food Security , 19 Chlorine Gardens, Belfast, BT9 5DL United Kingdom
4 : University of Vigo , Department of Chemistry, Bloque E, Planta 2, Despacho 17, As Lagoas, Marcosende, 36310 Vigo, Spain
5 : Canadian Food Inspection Agency , 1992 Agency Drive, Dartmouth, NS, B3B 1Y9 Canada
6 : National Research Council of Canada , Biotoxin Metrology, 1411 Oxford Street, Halifax, NS, B3H 3Z1 Canada
7 : Agri-Food and Biosciences Institute, Veterinary Sciences Division , Stoney Road, Belfast, United Kingdom, BT4 3SD
8 : Ifremer, PHYTOX Unit , F-44000 Nante, s, France
9 : Instituto Tecnoloxico para o Control do Medio Mariño de Galicia , Peirao de Vilaxoan, s/n, 36611 Vilagarcia de Arousa, Pontevedra, Spain
10 : Laboratorio Cifga, Avenida Benigno Rivera , No. 56, 27003 Lugo, Spain
11 : Wageningen Food Safety Research, Wageningen University and Research , Akkermaalsbos 2, 6708WB Wageningen, The Netherlands
12 : R-Biopharm Nederland B.V , Beijerinckweg 18, 6827 BN Arnhem, The Netherlands
13 : Cawthron Institute , 98 Halifax Street East, Nelson 7010, Private Bag 2, Nelson, 7042 New Zealand
14 : CTL Ltd , Pakefield Road, Lowestoft, Suffolk, NR33 0HT United Kingdom
15 : CNC , 3 Elms Street, Stoke, 7011 New Zealand
16 : Universidade De Santiago De Compostela Deparamento de Farmacologa, Facultad de Veterinaria, , 27002 Lugo, Spain
Source Journal Of Aoac International (1060-3271) (Oxford University Press (OUP)), 2023-03 , Vol. 106 , N. 2 , P. 356-369
DOI 10.1093/jaoacint/qsad006
WOS© Times Cited 1

Background Given the recent detection of TTX in bivalve molluscs but the absence of a full collaborative validation study for TTX determination in a large number of shellfish samples, interlaboratory assessment of method performance was required to better understand current capabilities for accurate and reproducible TTX quantitation using chemical and immunoassay methods. Objective The aim was to conduct a collaborative study with multiple laboratories, using results to assess method performance and acceptability of different TTX testing methods Methods Homogenous and stable mussel and oyster materials were assessed by participants using a range of published and in-house detection methods to determine mean TTX concentrations. Data was used to calculate recoveries, repeatability and reproducibility, together with participant acceptability z-scores. Results Method performance characteristics were good, showing excellent sensitivity, recovery and repeatability. Acceptable reproducibility was evidenced by HorRat values for all LC-MS/MS and ELISA methods being less than the 2.0 limit of acceptability. Method differences between the LC-MS/MS participants did not result in statistically-different results. Method performance characteristics compared well with previously-published single-laboratory validated methods and no statistical difference was found in results returned by ELISA in comparison with LC-MS/MS. Conclusions The results from this study demonstrate that current LC-MS/MS methods and the ELISA are on the whole capable of sensitive, accurate and reproducible TTX quantitation in shellfish. Further work is recommended to expand the number of laboratories testing ELISA and to standardise an LC-MS/MS protocol to further improve interlaboratory precision. Highlights Multiple mass spectrometric methods and a commercial ELISA have been successfully assessed through collaborative study, demonstrating excellent performance.

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Turner Andrew D, Dean Karl J, Dhanji-Rapkova Monika, Dall’ara Sonia, Pino Florella, McVey Claire, Haughey Simon, Logan Natasha, Elliott Christopher, Gago-Martinez Ana, Leao Jose Manuel, Giraldez Jorge, Gibbs Ryan, Thomas Krista, Perez-Calderon Ruth, Faulkner Dermot, McEneny Hugh, Savar Veronique, Reveillon Damien, Hess Philipp, Arevalo Fabiola, Lamas J Pablo, Cagide Eva, Alvarez Mercedes, Antelo Alvaro, Klijnstra Mirjam D, Oplatowska-Stachowiak Michalina, Kleintjens Tim, Sajic Nermin, Boundy Michael J, Maskrey Benjamin H, Harwood D Tim, Jartín Jesús M González, Alfonso Amparo, Botana Luis (2023). Interlaboratory evaluation of multiple LC-MS/MS methods and a commercial ELISA method for determination of tetrodotoxin in oysters and mussels. Journal Of Aoac International, 106(2), 356-369. Publisher's official version : , Open Access version :