한국수산과학회지 (Korean Journal of Fisheries and Aquatic Sciences)

  • 제46권2호
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  • Pages.147-153
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  • 2013
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  • 0374-8111(pISSN)
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  • 2287-8815(eISSN)
한국수산과학회 (The Korean Society of Fisheries and Aquatic Science)
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마비성패류독소 분석을 위한 Precolumn HPLC Oxidation 법의 유효성 검증

Validation of Precolumn HPLC Oxidation Method for Analysis of Paralytic Shellfish Poison

  • 목종수 (국립수산과학원 남동해수산연구소) ;
  • 송기철 (국립수산과학원 서해수산연구소) ;
  • 이가정 (국립수산과학원 식품안전과) ;
  • 김지회 (국립수산과학원 식품안전과)
  • Mok, Jong-Soo (Southeast Sea Fisheries Research Institute, National Fisheries Research & Development Institute) ;
  • Song, Ki-Cheol (West Sea Fisheries Research Institute, National Fisheries Research & Development Institute) ;
  • Lee, Ka-Jeong (Food Safety Research Division, National Fisheries Research & Development Institute) ;
  • Kim, Ji-Hoe (Food Safety Research Division, National Fisheries Research & Development Institute)
  • 투고 : 2013.01.30
  • 심사 : 2013.03.18
  • 발행 : 2013.04.30
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초록

To prevent paralytic shellfish poisoning (PSP) due to the consumption of shellfish contaminated with PSP toxins, the quantitative analysis of these toxins is very crucial. The AOAC International mouse bioassay (MBA) has been used widely for the routine monitoring of PSP toxins for more than 50 years. However, this method has low sensitivity and high limit of quantification (LOQ) and interferences from other components in the extract, and it cannot determine toxic profiles. Ethical problems also exist with the continued use of this live mouse assay. To establish an alternative method to the MBA used for PSP toxins analysis, we attempted to optimize the analysis conditions of a precolumn high-performance liquid chromatography (HPLC) oxidation method and succeeded in validating its accuracy and precision in quantifying PSP toxins. A clear peak and the isolation of PSP toxins were obtained by injecting the working standards of Certified Reference Materials using HPLC. The LOQ of the precolumn HPLC oxidation method for PSP toxins was about $0.1002{\mu}g/g$, which represented an approximately fourfold improvement in detection capability versus the AOAC MBA. The intra-accuracy and precision for PSP toxins in oysters were 77.0-103.3% and 2.0-5.7%, respectively, while the respective inter-accuracy and precision were 77.3-100.7% and 2.4-6.0%. The mean recoveries of PSP toxins from oysters were 75.2-112.1%. The results of a comparison study showed good correlation between the results of the precolumn HPLC oxidation method and those of MBA, with a correlation factor of 0.9291 for mussels. The precolumn HPLC oxidation method may be used as an alternative to, or supplementary method with, MBA to monitor the occurrence of PSP toxins and to analyze the profiles of these toxins in shellfish.

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참고문헌

  1. AOAC. 2002. AOAC Guidelines for single laboratory validation of chemical methods for dietary supplements and botanicals. Gaithersburg, MD, USA, 1-38.
  2. AOAC. 2005. AOAC Official Method 959.08. Paralytic shellfish poison. Biological method. Final action. In: AOAC official methods of analysis, 18th ed. AOAC International, Gaithersburg, MD, USA. 79-80.
  3. Asp TN, Larsen S and Aune T. 2004. Analysis of PSP toxins in Norwegian mussels by a post-column derivatization HPLC method. Toxicon 43, 319-327. http://dx.doi.org/10.1016/j.toxicon.2004.01.004.
  4. Balls MB, Goldburg AM, Fentem JH, Broadhead CL, Bursch RL, Festing MFW, Frazier JM, Hendrickson CFM, Jennings M, van der Kamp MDO, Morton DB, Rowan AX, Russell C, Russel WMS, Spielman H, Stephens ML, Stokes WS, Straughan DW, Yager JD, Zurlo J and van Zutphen BFM. 1995. The report and recommendation of ECVAM workshop 11, ATLA. 23, 883-866.
  5. Chang DS, Shin IS, Kim JH, Pyun JH and Choe WK. 1989. Detoxification of PSP and relationship between PSP toxicity and Protogonyaulax sp. Bull Kor Fish Soc 22, 177-188.
  6. Chang DS, Shin IS, Pyeun JH and Park YH. 1987. A Study on paralytic shellfish poison of sea mussel, Mytilus edulis. Food poisoning accident in Gamchun Bay, Pusan, Korea, 1986. Bull Kor Fish Soc 20, 293-299.
  7. Determan M. 2003. Paralytic shellfish poisoning (PSP) patterns in Puget Sound shellfish in 2001. Washington State Department of Health, Olympia, WA, USA, 1-12.
  8. Franco JM and Fernandez-Villa P. 1993. Separation of paralytic shellfish toxins by reversed phase high performance liquid chromatography with postcolumn reaction and fluorometric detection. Chromatographia 35, 613-620. https://doi.org/10.1007/BF02267925
  9. Gawley RE, Pinet S, Cardona CM, Datta PK, Ren T, Guida WC, Nydick J and Leblanc RM. 2002. Chemosensors for the marine toxin saxitoxins. J Am Chem Soc 124, 13448-13453. http://dx.doi.org/10.1021/ja027507p.
  10. Hall S, Strichartz GR, Moczydlowski E, Ravindran A and Reichardt PB. 1990. The saxitoxins: sources, chemistry, and pharmacology. In: Marine Toxins. Hall S and Strichartz GR, eds. ACS Symposium Series 418, American Chemical Society, Washington, DC, USA, 29-65.
  11. Hall S. 1991. Natural toxins. In: Microbiology of Marine Food Products. Ward DR and Hackney CR, eds. Van Nostrand Reinhold, New York, USA, 301-330.
  12. Hess P, Grune B, Anderson DB, Anne T, Botana LM, Caricato E, van Egmond HE, Halder M, Hall S, Lawrence JF, Moffat C, Poletti R, Richmond J, Rossini GE, Seamer C and Vilageliu JS. 2006. Three Rs approaches in marine biotoxin testing, The report and recommendations of a joint ECVAMIDG SANCO Workshop (ECVAM Workshop 55). ATLA 34, 193-224.
  13. Jellett JF, Roberts RL, Laycock MV, Quilliam MA and Barrett RE. 2002. Detection of paralytic shellfish poisoning (PSP) toxins in shellfish tissue using MIST Alert, a new rapid test, in parallel with the regulatory AOAC mouse bioassay. Toxicon 40, 1407-1425. http://dx.doi.org/10.1016/S0041-0101(02)00153-8.
  14. Kim HG, Lee SG, Lim WA, Lee JS and Kim JH. 1996. Environmental physiology of Alexandrium tamarense isolated from Chinhae Bay, the south sea of Korea. In: Harmful and toxic algal blooms.
  15. Lawrence JF, Menard C and Cleroux C. 1995. Evaluation of prechromatographic oxidation for liquid chromatographic determination of paralytic shellfish poisons in shellfish. J AOAC Int 78, 514-520.
  16. Lawrence JF and Niedzwiadek B. 2001. Quantitative determination of paralytic shellfish poisoning toxins in shellfish using prechromatographic oxidation and liquid chromatography with fluorescence detection. J AOAC Int 84, 1099-1108.
  17. Lawrence JF, Niedzwiadek B and Menard C. 2005. Quantitative determination of paralytic shellfish poisoning toxins in shellfish using prechromatographic oxidation and liquid chromatography with fluorescence detection: collaborative study. J AOAC Int 88, 1714-1732.
  18. Lee JS, Shin IS, Kim YM and Chang DS. 1997. Paralytic shellfish toxins in the mussel, Mytilus edulis, caused the shellfish poisoning accident at Geoje, Korea, in 1996. J Kor Fish Soc 30, 158-160.
  19. Louzao MC, Vieytes MR, Cabado AG, Baptista de Sousa JMV and Botana LMA. 2003. A fluorimetric microplate assay for detection and quantitation of toxins causing paralytic shellfish poisoning. Chem Res Toxicol 16, 433-438. http:// dx.doi.org/10.1021/tx025574r.
  20. Manger RL, Leja LS, Lee SY, Hungerford JM, Kirkpatrick MA, Yasumoto T and Wekel MM. 2003. Detection of paralytic shellfish poison by rapid cell bioassay: antagonism of voltage- gated sodium channel active toxins in vitro. J AOAC Int 86, 540-543.
  21. Mons MN, Van Egmond HP and Speijers GJA. 1998. Paralytic shellfish poisoning: A review. RIVM Report 388802005, 1-60.
  22. Noguchi T. 2003. Marine toxins. Nippon Suisan Gakkaishi 69, 895-909. http://dx.doi.org/10.2331/suisan.69.895.
  23. Oshima Y. 1995. Post-column derivatization liquid-chromatograpic method for paralytic shellfish toxins. J AOAC Int 78, 528-532.
  24. Park DL, Adams WN, Graham SL and Jackson RC. 1986. Variability of mouse bioassay for determination of paralytic shellfish poisoning toxins. J AOAC Int 69, 547-550.
  25. Park MJ, Lee HJ, Lee TS, Son KT, Byun HS, Park JH and Jang DS. 2000. Comparison of paralytic shellfish poison contents and components in the different bivalve species. J Fd Hyg Safety 15, 293-296.
  26. Rodriguez DC, Etzel RA, Hall SE, de Porras E, Velasquez OH, Tauxe RV, Kilbourne EM and Blake PA. 1990. Lethal Paralytic Shellfish Poisoning in Guatemala. Am J Trop Med Hyg 42, 267-271. https://doi.org/10.4269/ajtmh.1990.42.267
  27. Rourke WA, Murphy CJ, Pitcher G, Riet JM, Burns BG, Thomas KM and Quilliam MA. 2008. Rapid postcolumn methodology for determination of paralytic shellfish toxins in shellfish tissue. J AOAC Int 91, 589-597.
  28. Sayfritz SJ, Aasen JAB and Aune T. 2008. Determination of paralytic shellfish poisoning toxins in Norwegian shellfish by liquid chromatography with fluorescence and tandem mass spectrometry detection. Toxicon 52, 330-340. http://dx.doi. org/10.1016/j.toxicon.2008.06.001.
  29. Schantz EJ, McFarren EF, Schafer ML and Lewis KH. 1958. Purified shellfish poison for bioassay standardization. J AOAC Int 41, 160-168.
  30. Shon MB, Kim YS and Kim CH. 2009. Paralytic shellfish poisoning of Mediterranean mussels from Jinhae Bay in Korea. Kor J Fish Aquat Sci 42, 366-372. http://dx.doi.org/10.5657/ kfas.2009.42.4.366.
  31. Silvert W and Rao DVS. 1992. Dynamic model of the flux of domoic acid, a neuro toxin, through a Mytilus edulis population. Can J Fish Aquat Sci 49, 400-405. https://doi.org/10.1139/f92-045
  32. Takata K, Takatsuji H and Seno M. 2008. Detoxification of the oyster Crassostrea gigas contaminated with paralytic shellfish poison (PSP) by cultivation in filtered seawater. Nippon Suisan Gakkaishi 74, 78-80. http://dx.doi.org/10.2331/suisan.74.78.
  33. Thibault E, Pleasance S and Laycock MV. 1991. Analysis of paralytic shellfish poisons by capillary electrophoresis. J Chromatogr A 542, 483-501. https://doi.org/10.1016/S0021-9673(01)88783-5
  34. Thomas K, Chung S, Ku J, Reeves K and Quilliam MA. 2006. Analysis of PSP toxins by liquid chromatography with post column oxidation and fluorescence detection. In: Molluscan Shellfish Safety. Henshilwood K, Deegan B, McMahon T, Cusack C, Keaveney S, Silke J, O'Cinneide M, Lyons D and Hess P. eds. The Marine Institute, Galway, Ireland. 132 -138.
  35. Toyofuku H. 2006. Joint FAO/WHO/IOC activities to provide scientific advice on marine biotoxins (research report). Mar Pol Bull 52, 1735-1745. http://dx.doi.org/10.1016/j.marpolbul.2006.07.007.
  36. Usleber E, Dietrich R, Burk C, Schneider E and Martlbauer E. 2001. Immunoassay methods for paralytic shellfish poisoning toxins. J AOAC Int 84, 1649-1656.
  37. Van de Riet JM, Gibbs RS, Chou FW, Muggah PM, Rourke WA, Burns G, Thomas K and Quilliam MA. 2009. Liquid chromatographic post-column oxidation method for analysis of paralytic shellfish toxins in mussels, clams, scallops, and oysters: single-laboratory validation. J AOAC Int 92, 1690-1704.
  38. Wekell JC, Hurst J and Lefebvre KA. 2004. The origin of regulatory limits for PSP and ASP toxins in shellfish. J Sellfish Res 23, 927-930.

피인용 문헌

  1. Variation and Profile of Paralytic Shellfish Poisoning Toxins in Jinhae Bay, Korea vol.16, pp.3, 2013, https://doi.org/10.5657/FAS.2013.0137