PMID- 36668847 OWN - NLM STAT- MEDLINE DCOM- 20230124 LR - 20231118 IS - 2072-6651 (Electronic) IS - 2072-6651 (Linking) VI - 15 IP - 1 DP - 2022 Dec 30 TI - A Feasibility Study into the Production of a Mussel Matrix Reference Material for the Cyanobacterial Toxins Microcystins and Nodularins. LID - 10.3390/toxins15010027 [doi] LID - 27 AB - Microcystins and nodularins, produced naturally by certain species of cyanobacteria, have been found to accumulate in aquatic foodstuffs such as fish and shellfish, resulting in a risk to the health of the seafood consumer. Monitoring of toxins in such organisms for risk management purposes requires the availability of certified matrix reference materials to aid method development, validation and routine quality assurance. This study consequently targeted the preparation of a mussel tissue reference material incurred with a range of microcystin analogues and nodularins. Nine targeted analogues were incorporated into the material as confirmed through liquid chromatography with tandem mass spectrometry (LC-MS/MS), with an additional 15 analogues detected using LC coupled to non-targeted high resolution mass spectrometry (LC-HRMS). Toxins in the reference material and additional source tissues were quantified using LC-MS/MS, two different enzyme-linked immunosorbent assay (ELISA) methods and with an oxidative-cleavage method quantifying 3-methoxy-2-methyl-4-phenylbutyric acid (MMPB). Correlations between the concentrations quantified using the different methods were variable, likely relating to differences in assay cross-reactivities and differences in the abilities of each method to detect bound toxins. A consensus concentration of total soluble toxins determined from the four independent test methods was 2425 +/- 575 microg/kg wet weight. A mean 43 +/- 9% of bound toxins were present in addition to the freely extractable soluble form (57 +/- 9%). The reference material produced was homogenous and stable when stored in the freezer for six months without any post-production stabilization applied. Consequently, a cyanotoxin shellfish reference material has been produced which demonstrates the feasibility of developing certified seafood matrix reference materials for a large range of cyanotoxins and could provide a valuable future resource for cyanotoxin risk monitoring, management and mitigation. FAU - Turner, Andrew D AU - Turner AD AUID- ORCID: 0000-0003-1390-0924 AD - Centre for Environment Fisheries and Aquaculture Science, Barrack Road, Weymouth DT4 8UB, UK. FAU - Beach, Daniel G AU - Beach DG AUID- ORCID: 0000-0002-5680-2112 AD - Biotoxin Metrology, National Research Council Canada, Halifax, NS B3H 3Z1, Canada. FAU - Foss, Amanda AU - Foss A AUID- ORCID: 0000-0003-0412-3879 AD - Greenwater Laboratories, 205 Zeagler Drive, Suite 302, Palatka, FL 32177, USA. FAU - Samdal, Ingunn A AU - Samdal IA AUID- ORCID: 0000-0001-5225-2494 AD - Norwegian Veterinary Institute, 1431 As, Norway. FAU - Lovberg, Kjersti L E AU - Lovberg KLE AD - Norwegian Veterinary Institute, 1431 As, Norway. FAU - Waack, Julia AU - Waack J AD - Centre for Environment Fisheries and Aquaculture Science, Barrack Road, Weymouth DT4 8UB, UK. AD - CyanoSol, School of Pharmacy and Life Sciences, Robert Gordon University, Aberdeen AB10 7GJ, UK. FAU - Edwards, Christine AU - Edwards C AD - CyanoSol, School of Pharmacy and Life Sciences, Robert Gordon University, Aberdeen AB10 7GJ, UK. FAU - Lawton, Linda A AU - Lawton LA AD - CyanoSol, School of Pharmacy and Life Sciences, Robert Gordon University, Aberdeen AB10 7GJ, UK. FAU - Dean, Karl J AU - Dean KJ AUID- ORCID: 0000-0002-7803-6690 AD - Centre for Environment Fisheries and Aquaculture Science, Barrack Road, Weymouth DT4 8UB, UK. FAU - Maskrey, Benjamin H AU - Maskrey BH AD - Centre for Environment Fisheries and Aquaculture Science, Barrack Road, Weymouth DT4 8UB, UK. FAU - Lewis, Adam M AU - Lewis AM AD - Centre for Environment Fisheries and Aquaculture Science, Barrack Road, Weymouth DT4 8UB, UK. LA - eng GR - BB/S004211/1/BB_/Biotechnology and Biological Sciences Research Council/United Kingdom PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20221230 PL - Switzerland TA - Toxins (Basel) JT - Toxins JID - 101530765 RN - 77238-39-2 (microcystin) RN - 0 (Microcystins) RN - 0979BIK2QU (nodularin) RN - 0 (Cyanobacteria Toxins) SB - IM MH - Animals MH - *Microcystins/analysis MH - Cyanobacteria Toxins MH - Chromatography, Liquid/methods MH - Feasibility Studies MH - Tandem Mass Spectrometry/methods MH - *Bivalvia/chemistry MH - Shellfish/analysis PMC - PMC9867187 OTO - NOTNLM OT - LC-HRMS OT - LC-MS/MS OT - microcystins OT - mussels OT - nodularins OT - quality control OT - reference materials OT - shellfish COIS- The authors declare no conflict of interest. EDAT- 2023/01/21 06:00 MHDA- 2023/01/25 06:00 PMCR- 2022/12/30 CRDT- 2023/01/20 15:33 PHST- 2022/11/16 00:00 [received] PHST- 2022/12/15 00:00 [revised] PHST- 2022/12/23 00:00 [accepted] PHST- 2023/01/20 15:33 [entrez] PHST- 2023/01/21 06:00 [pubmed] PHST- 2023/01/25 06:00 [medline] PHST- 2022/12/30 00:00 [pmc-release] AID - toxins15010027 [pii] AID - toxins-15-00027 [pii] AID - 10.3390/toxins15010027 [doi] PST - epublish SO - Toxins (Basel). 2022 Dec 30;15(1):27. doi: 10.3390/toxins15010027.