Korean Journal of Fisheries and Aquatic Sciences (한국수산과학회지)

The Korean Society of Fisheries and Aquatic Science (한국수산과학회)
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Validation of Precolumn HPLC Oxidation Method for Analysis of Paralytic Shellfish Poison

마비성패류독소 분석을 위한 Precolumn HPLC Oxidation 법의 유효성 검증

  • 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)
  • 목종수 (국립수산과학원 남동해수산연구소) ;
  • 송기철 (국립수산과학원 서해수산연구소) ;
  • 이가정 (국립수산과학원 식품안전과) ;
  • 김지회 (국립수산과학원 식품안전과)
  • Received : 2013.01.30
  • Accepted : 2013.03.18
  • Published : 2013.04.30
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Abstract

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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References

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