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Fit-for-purpose shellfish reference materials for internal and external quality control in the analysis of phycotoxins

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Abstract

The need for reference materials for quality control of analysis of foodstuffs has been stressed frequently. This has been particularly true in the phycotoxins field, where there is a great shortage of both pure calibration standards and reference materials. Worldwide there are very few independent bodies that produce certified reference materials for phycotoxins, the main producers currently being the National Research Council Canada and the Japanese Food Research Laboratory. Limited availability of contaminated shellfish and algae, as well as the time and knowledge necessary for the production of adequate reference materials, continuously lead to limited editions of certified reference materials and even more limited production of in-house reference materials. The restricted availability of in-house quality control materials promotes the rapid use of the limited certified reference materials, which in turn hampers the production of the suite of materials required globally for complete protection of public health. This paper outlines the various options that analysts can pursue in the use of reference materials for internal and external quality control, with a view to optimising the efforts of both reference materials users and reference materials producers. For this purpose, the logical sequence is reviewed from the discovery of a new bioactive compound in shellfish, through initial method development up to regulation for food safety purposes including accepted reference methods. Subsequently, the requirements for and efforts typically spent in the production and characterisation of laboratory reference materials, certified reference materials and other test materials used in inter-laboratory studies or proficiency testing, in the area of marine biotoxins are evaluated. Particular emphasis is put on practical advice for the preparation of in-house reference materials. The intricate link between reference material characterisation and method performance is outlined to give guidance on the appropriate in-house method validation in the rapidly developing field of phycotoxins.

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References

  1. Twiner MJ, Hess P, Bottein Dechraoui MY, McMahon T, Ramsdell JS, Samons MS, Satake M, Yasumoto T, Doucette GJ (2005) Cytotoxic and cytoskeletal effects of azaspiracid-1 on multiple mammalian cell lines. Toxicon 45:891–900

    CAS  Google Scholar 

  2. Van Egmond HP, Mouriño A, Burdaspal PA, Bustos J, Legarda T, Mesego A, Paulsch WE, Salgado C, van den Top HJ, Boenke A (1998) The certification of the mass fractions of saxitoxin and dc-saxitoxin in two mussel reference materials (CRMs 542 & 543), including the Identification of other PSP-toxins, and a spiking procedure based on an enrichment solution (CRM 663) with a certified mass concentration of saxitoxin. EUR report 18318, p 124. European Commission, DG Science, Research and Development, Brussels, Belgium

  3. Dell’Aversano C, Hess P, Quilliam MA (2005) Hydrophilic interaction liquid chromatography-mass spectrometry for the analysis of paralytic shellfish poisoning (PSP) toxins. J Chromatogr 1081:190–201

    Article  CAS  Google Scholar 

  4. Anon (2005) Report of the joint FAO/IOC/WHO ad hoc expert consultation on biotoxins in molluscan bivalves (Oslo, Norway, 26–30 September 2004), p 31. Rome, Italy: Food and Agriculture Organization. Website http://www.fao.org/es/esn/food/risk_biotoxin_en.stm (Accessed 17.01.2006)

  5. Hess P, Grune B, Anderson DB, Aune T, Botana LM, Caricato P, van Egmond HP, Halder M, Hall S, Lawrence JF, Moffat C, Poletti R, Richmond J, Rossini GP, Seamer C, Serratosa Vilageliu J (2006) Three Rs approaches in marine biotoxin testing - the report and recommendations of a joint ECVAM/DG SANCO workshop (ECVAM Workshop 55). Alternatives to Laboratory Animals (ATLA) 34, 193–224

  6. Van Egmond HP (2005) Validation issues and CRMs. Oral presentation at Wiley Award Symposium of the 2005 Annual Conference of the AOAC, Orlando, FL, US

  7. ISO (1993) International vocabulary of basic and general terms in metrology. Geneva, Switzerland, ISO/IEC

  8. Emons H, Linsinger TPJ, Gawlik BM (2004) Reference materials: terminology and use. Can’t one see the woods for the trees? TRAC 23:442–449

    CAS  Google Scholar 

  9. Emons H (2005) The ‘RM family’-identification of all of its members. Accredit Qual Assur 10:690–691

    Article  Google Scholar 

  10. Marine Institute, unpublished data

  11. Quilliam MA, Wright JLC (1989) The amnesic shellfish poisoning mystery. Anal Chem 61:1053A–1060A

    CAS  Google Scholar 

  12. McMahon T, Silke J (1996) Winter toxicity of unknown aetiology in mussels. Harmful Algal News 14:2

    Google Scholar 

  13. Anderson WA, Whelan P, Ryan M, McMahon T, James KJ (2001) Risk assessment of azaspiracids (AZAs) in shellfish. Food Safety Authority, Ireland

  14. Anon (2002) Commission Decision 2002/225/EC of 15 March 2002 laying down detailed rules for the implementation of Council Directive 91/492/EEC as regards the maximum levels and the methods of analysis of certain marine biotoxins in bivalve molluscs, echinoderms, tunicates and marine gastropods. Official J Eur Communities L75:62–64

  15. Anon (1997) Council Directive 97/61/EC of 20 October 1997 amending the Annex to Directive 91/492/EEC laying down the health conditions for the production and placing on the market of live bivalve molluscs. Official J Eur Communities L295:35–36

  16. Quevauviller P, Maier EA (1999) Interlaboratory studies and certified reference materials for environmental analysis, vol 22. In: Techniques and instrumentation in analytical chemistry. Elsevier Science B.V. p 558, ISBN: 0-444-82389-1

  17. Kramer KJM, Kramer GN, Muntau H (2003) Practical manual for the production of laboratory reference materials; 2nd edn of report initially prepared for EU Commission DG Sanco from project “Training on production and use of laboratory reference materials for use in quality control”, TRAP-LRM G6MA-CT2000-02006. Mermayde Publications, Bergen (Netherlands) P.O. Box 109, 1860 AC Bergen, The Netherlands

  18. Miles CO, Wilkins AL, Munday R, Dines MH, Hawkes AD, Briggs LR, Sanvik M, Jensen DJ, Cooney JM, Holland PT, Quilliam MA, MacKenzie AL, Beuzenberg V, Towers N (2004) Isolation of pectenotoxin-2 from dinophysis acuta and its conversion to pectenotoxin-2 seco acid and preliminary assessment of their acute toxicities. Toxicon 43:1–9

    Article  CAS  Google Scholar 

  19. Hess P, Nguyen L, Aasen J, Keogh M, Kilcoyne J, McCarron P, Aune T (2005) Tissue distribution, effects of cooking and parameters affecting the extraction of azaspiracids from mussels, Mytilus edulis, prior to analysis by liquid chromatography coupled to mass spectrometry. Toxicon 46:62–71

    Article  CAS  Google Scholar 

  20. McCarron P, Hess P (2006) Tissue distribution and effects of heat treatments on the content of domoic acid in blue mussels, Mytilus edulis. Toxicon 47:473–479

    Article  CAS  Google Scholar 

  21. Faure U, Wagstaffe PJ (1993) Stability of reference materials. Fresenius J Anal Chem 345:124–126

    Article  CAS  Google Scholar 

  22. McCarron P, Burrell S, Hess P (2006) Effect of addition of antibiotics and an antioxidant, on the stability of tissue reference materials for domoic acid, the amnesic shellfish poison. Anal Bioanal Chem (submitted June 2006)

  23. McCarron P, Emteborg H, Hess P (2006) Evaluation of freeze–drying as a stabilisation technique in comparison with wet frozen homogenates for mussel (Mytilus edulis) tissue reference materials containing hydrophilic and lipophilic phycotoxins. Anal Bioanal Chem (In preparation)

  24. NRC-CNRC Institute for Marine Biosciences. NRC CRM-ASP-Mus-c (2005) and NRC CRM-DSP-mus-b (2005). Certificates of analysis

  25. Quilliam MA, Reeves K, MacKinnon S, Craft C, Whyte H, Walter J, Stobo L, Gallacher S (2006) Preparation of reference materials for azaspiracids. In: (Deegan B, Butler C, Cusack C, Henshilwood K, Hess P, Keaveney S, McMahon T, O’Cinneide M, Silke J (eds) Proceedings of the 5th International Conference of Molluscan Shellfish Safety, 14–18 June 2004, Galway, Ireland. Marine Institute, Galway, Ireland (in press)

  26. Clancy V, Willie S (2004) Preparation and certification of a reference material for the determination of nutrients in seawater. Anal Bioanal Chem 378(5):1239–1242

    Article  CAS  Google Scholar 

  27. McCarron P, Kotterman M, de Boer J, Rehmann R, Hess P (2006) Feasibility of irradiation as a stabilisation technique in the preparation of tissue reference materials for a range of shellfish toxins. Anal Bioanal Chem (submitted June 2006)

  28. Bermudo E, Busquets R, Barcelo-Barrachina E, Puignou L, Santos FJ, Galceran MT (2003) Preparation of a beef extract as a laboratory reference material for the determination of heterocyclic amines. J Chromatogr B 802:61–68

    Article  Google Scholar 

  29. Lamberty A, Schimmel H, Pauwels J (1998) The study of the stability of reference materials by isochronous measurements. Fresenius J Anal Chem 360:359–361

    Article  CAS  Google Scholar 

  30. Venelinov T, Sahuquillo A (2006) Optimizing the uses and the costs of reference materials in analytical laboratories. TRAC 25:528–533

    CAS  Google Scholar 

  31. Anon (2002) Commission Decision 2002/226/EC of 15 March 2002 establishing special health checks for the harvesting and processing of certain bivalve molluscs with a level of amnesic shellfish poison (ASP) exceeding the limit laid down by Council Directive 91/492/EEC (notified under document number C(2002) 1009). Official J Eur Communities L75, 65–66

  32. QUASIMEME (2006) Report “DE-10 Shellfish Toxins Round 43-Exercise 696 November-December 2005”, report version 1.0 of 9 March 2006, accessed on sharepoint-part of the website: (http://www.quasimeme.org), last accessed: 02 June 2006

  33. Hess P, Scurfield J, Wells DE (2006) Proficiency testing for the quantitative determination of domoic acid, the amnesic shellfish poisoning toxin. In: Deegan B, Butler C, Cusack C, Henshilwood K, Hess P, Keaveney S, McMahon T, O’Cinneide M, Silke J (eds) Proceedings of the 5th International Conference of Molluscan Shellfish Safety, 14-18 June 2004, Galway, Ireland. Marine Institute, Galway, Ireland (in press)

  34. Hess P, Kilcoyne J, Swords D, Mulcahy N, McCarron M, Keogh M, Gibbons B, Ronan J (2006) Impact of HPLC-UV methods (solid-phase extraction/UV detection and photodiode-array detection) for the determination of domoic acid on quality of results and sample turn-around time. In: Deegan B, Butler C, Cusack C, Henshilwood K, Hess P, Keaveney S, McMahon T, O’Cinneide M, Silke J (eds) Proceedings of the 5th International Conference of Molluscan Shellfish Safety, 14–18 June 2004, Galway, Ireland. Marine Institute, Galway, Ireland (in press)

  35. European Commission (Standards, Measurement and Testing Programme) (1997) Guidelines for the production and certification of BCR reference materials. Doc BCR/01/97 1 September 1997

  36. ISO (2000) Guide 34 General requirements for the competence of reference materials producers, 2nd edn. Geneva, Switzerland, ISO

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Acknowledgements

The authors would like to acknowledge funding from the Marine Institute and the National Development Plan (NDP), Ireland, for funding of the ASTOX project (ST-02-02), 2003–2006. We also would like to acknowledge the contribution of the technical staff of the Biotoxin Chemistry Team at the Marine Institute to the preparation of the LRMs discussed in this paper.

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Hess, P., McCarron, P. & Quilliam, M.A. Fit-for-purpose shellfish reference materials for internal and external quality control in the analysis of phycotoxins. Anal Bioanal Chem 387, 2463–2474 (2007). https://doi.org/10.1007/s00216-006-0792-8

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