Fisheries and Aquatic Sciences

한국수산과학회 (The Korean Society of Fisheries and Aquatic Science)
권호 표지
DOI QR코드

DOI QR Code

Comparison of MBA and HPLC Post-column Oxidation Methods for the Quantification of Paralytic Shellfish Poisoning Toxins

  • Yu, Hongsik (Food Safety Division, National Fisheries Research and Development Institute) ;
  • Lim, Keun Sik (Food Safety Division, National Fisheries Research and Development Institute) ;
  • Song, Ki Cheol (West Sea Fisheries Institute, National Fisheries Research and Development Institute) ;
  • Lee, Ka Jeong (Food Safety Division, National Fisheries Research and Development Institute) ;
  • Lee, Mi Ae (Food Safety Division, National Fisheries Research and Development Institute) ;
  • Kim, Ji Hoe (Food Safety Division, National Fisheries Research and Development Institute)
  • 투고 : 2013.08.12
  • 심사 : 2013.08.23
  • 발행 : 2013.09.30
PDF 다운로드
⟨ 이전 논문 다음 논문 ⟩

초록

The mouse bioassay and high performance liquid chromatography (HPLC) post-column oxidation method are different methods of quantifying paralytic shellfish poisoning toxins. In this study, we compared their ability to accurately quantify the toxicity levels in two types of field sample (oysters and mussels) with different toxin profiles for routine regulatory monitoring. A total of 72 samples were analyzed by both methods, 44 of which gave negative results, with readings under the limit of detection of the mouse bioassay ($40{\mu}g/100g$ saxitoxin [STX] eq). In 14 oysters, the major toxin components were gonyautoxin (GTX) 1, -2, -3, -4, -5, decarbamoylgonyautoxin-2 (dcGTX2), and decarbamoylsaxitoxin (dcSTX), while 14 mussels tested positive for dcSTX, GTX2, -3, -4, -5, dcGTX2, neosaxitoxin (NEO), STX, and dcSTX. When the results obtained by both methods were compared in two matrices, a better correlation ($r^2=0.9478$) was obtained for mussels than for oysters ($r^2=0.8244$). Additional studies are therefore needed in oysters to investigate the differences in the results obtained by both methods. Importantly, some samples with toxin levels around the legal limit gave inconsistent results using HPLC-based techniques, which could have a strong economic impact due to enforced harvest area closure. It should therefore be determined if all paralytic shellfish poisoning toxins can be quantified accurately by HPLC, and if the uncertainties of the method lead to doubts regarding regulatory limits.

키워드

참고문헌

  1. Association of Official Analytical Chemists. 2005. AOAC Official Method 959.08. Paralytic shellfish poison. Biological method. In: AOAC Official Methods of Analysis. 18th ed. Truckses MW, ed. AOAC International, Gaithersburg, MD, US, pp. 79-80.
  2. Association of Official Analytical Chemists. 2006. Paralytic shellfish poisoning toxins in shellfish. Prechromatographic oxidation and liquid chromatography with fluorescence detection. First action 2005, official method 2005.06. In: Official Methods of Analysis of AOAC International. Horwitz W and Latimer GW, eds. AOAC International, Gaithersburg, MD, US, p. 83.
  3. Balls MB, Goldburg AM, Fentem JH, Broadhead CL, Burch RL, Festing MFW, Frazier JM, Hendricksen CFM, Jennings M, van der Kamp MDO, Morton DB, Rowan AX, Russell C, Russell WMS, Spielmann H, Stephens ML, Stokes WS, Straughan DW, Yager JD, Zurlo JD and van Zutphen BFM. 1995. The three Rs: the way forward: the report and recommendation of ECVAM Workshop 11. Altem Lab Anim 23, 883-866.
  4. Ben-Gigirey B, Rodriguez-Velasco ML and Gago-Martinez A. 2012. Interlaboratory study for the extension of the validation of 2005.06 AOAC Official Method for dc-GTX-2,3. J AOAC 95, 1-13.
  5. Botana LM, Rodriguez-Vieytes M, Alfonso A and Louzao MC. 1996. Phycotoxins: paralytic shellfish poisoning and diarrhetic shellfish poisoning. In: Handbook of Food Analysis. Nollet LML, ed. Marcel Dekker Inc., New York, US, pp. 1147-1169.
  6. DeGrasse SL, van de Riet J, Hatfield R and Turner A. 2011. Pre- versus post-column oxidation liquid chromatography fluorescence detection of paralytic shellfish toxins. Toxicon 57, 619-624. http://dx.doi.org/10.1016/j.toxicon.2010.12.017.
  7. Diener M, Erler K, Hiller S, Christian B and Luckas B. 2006. Determination of paralytic shellfish poisoning (PSP) toxins in dietary supplements by application of a new HPLC/FD method. Eur Food Res Technol 224, 147-151. http://dx.doi.org/10.1007/s00217-006-0302-4.
  8. 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 and Vilageliu JS. 2006. Three Rs approaches in marine biotoxin testing: the report and recommendations of a Joint ECVAM/DG SANCO Workshop (ECVAM Workshop 54). Altem Lab Aanim 34, 193-224.
  9. Korea Food and Drug Administration. 2013. Korean Food Standard. Chapter 2. Korea Food and Drug Administration, Cheongwon, KR, pp. 2-26.
  10. Luckas B, Hummert C and Oshima Y. 2004. Analytical methods for paralytic shellfish poisons. In: Manual on Harmful Marine Microalgae. Hallegraeff GM, Anderson DM and Cembella AD, eds. UNESCO Publishing, Paris, FR, pp. 191-209.
  11. Park DL, Adams WN, Graham SL and Jackson RC. 1986. Variability of mouse bioassay for determination of paralytic shellfish poisoning toxins. J Assoc Off Anal Chem 69, 547-550.
  12. Rourke WA, Murphy CJ, Pitcher G, van de Riet JM, Burns G, Thomas KM and Quilliam MA. 2008. Rapid postcolumn methodology for determination of paralytic shellfish toxins in shellfish tissue. J AOAC Int 91, 589-597.
  13. Song KC, Lee KJ, Yu HS, Mok JS, Kim JH, Lim KS, Lee MA and Kim MH. 2013. Intra-laboratory validation of an HPLC post-column oxidation method for the analysis of PSP toxins in oysters and mussels. Korean J Food Sci Technol 45, 241-247. http://dx.doi.org/10.9721/KJFST.2013.45.2.241.
  14. Turner AD, Hatfield RG, Rapkova-Dhanji M, Norton DM, Algoet M and Lees DN. 2010. Single-laboratory validation of a refined AOAC HPLC method 2005.06 for oysters, cockles and clams in U.K. shellfish. J AOAC Int 93, 1482-1493.
  15. Turner AD, Dhanji-Rapkova M, Algoet M, Suarez-Isla BA, Cordova M, Caceres C, Murphy CJ, Casey M and Lees DN. 2012. Investigations into matrix components affecting the performance of the official bioassay reference method for quantitation of paralytic shellfish poisoning toxins in oysters. Toxicon 59, 215-230. http://dx.doi.org/10.1016/j.toxicon.2011.11.013.
  16. US Food and Drug Administration. 2009. Guide for the Control of Molluscan Shellfish, 2007 revision. Food and Drug Administration, Center for Food Safety and Applied Nutrition, Washington DC, US.
  17. Wiese M, D'Agostino PM, Mihali TK, Moffitt MC and Neilan BA. 2010. Neurotoxic alkaloids: saxitoxin and its analogs. Mar Drugs 8, 2185-2211. http://dx.doi.org/10.3390/md8072185.