Browse > Article
http://dx.doi.org/10.5657/KFAS.2020.0174

Validation of LC-MS/MS Method for Analysis of Paralytic Shellfish Toxins in Shellfish and Tunicates  

Cho, Sung Rae (Food Safety and Processing Research Division, National Institute of Fisheries Science)
Kim, Dong Wook (Food Safety and Processing Research Division, National Institute of Fisheries Science)
Yu, Hean Jae (Food Safety and Processing Research Division, National Institute of Fisheries Science)
Cho, Seong Hae (Food Safety and Processing Research Division, National Institute of Fisheries Science)
Ryu, Ara (Food Safety and Processing Research Division, National Institute of Fisheries Science)
Lee, Ka Jeong (Food Safety and Processing Research Division, National Institute of Fisheries Science)
Mok, Jong Soo (Food Safety and Processing Research Division, National Institute of Fisheries Science)
Publication Information
Korean Journal of Fisheries and Aquatic Sciences / v.53, no.2, 2020 , pp. 174-180 More about this Journal
Abstract
The mouse bioassay has been used widely for the monitoring of paralytic shellfish toxins (PSTs) in many countries. However, this method shows low sensitivity and high limit of detection (LOD), as well as it cannot confirm toxic profiles. Recently, LC-MS/MS method was studied for the quantitative of PSTs, however, the method has any problems with unstable retention times by ionization suppression caused by high salt concentration in shellfish extracts. To establish an alternative method for PSTs analysis, we tried to original LC-MS/MS methods adding desalting operation using amorphous graphitized polymer carbon solid-phase extraction cartridges. The method validation was conducted to determine linearity, limit of detection, limit of quantification (LOQ), accuracy, and precision in quantifying PSTs. The correlation coefficients for all tested PSTs maintained over 0.999. The LODs and LOQs for all PSTs were about 0.19-1.05 ㎍/kg and 0.58-3.18 ㎍/kg, respectively. The accuracies for PSTs were 95.4-107.7% for saxitoxin group, 97.1-100.9% for gonyautoxin group, 99.0-100.8% for N-sulfocarbamoyl toxin group, and 96.8-104.6% for decarbamoyl toxin group. These results indicate that the modified LC-MS/MS method was appropriate for analyzing the PSTs in shellfish and tunicates.
Keywords
Paralytic shellfish toxin; Solid-phase extraction; LC-MS/MS; Shellfish; Tunicate;
Citations & Related Records
Times Cited By KSCI : 5  (Citation Analysis)
연도 인용수 순위
1 AOAC (Association of Official Methods of Analysis). 2013. Appendix K: Guidelines for dietary supplements and botanicals. AOAC International, Gaithersburg, MS, U.S.A, 8-9.
2 Barbera-Sanchez AL, Soler JF, Astudillo LR and Chang-Yen I. 2004. Paralytic shellfish poisoning (PSP) in Margarita island, Venezuela. Rev Biol Trop 52, 89-98.
3 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.
4 Chang DS, Shin IS, Kim JH, Pyeun JH and Choe WK. 1989. Detoxification of PSP and relationship between PSP toxicity and Protogonyaulax sp. Bull Kor Fish Soc 22, 177-188.
5 Codex Alimentarius Commission. 2014. Principle for the establishment of Codex methods of analysis. In: Procedural manual, twenty-first edition. Rome, Italy, 63-73.
6 KMFDS (Korea Ministry of Food and Drug Safety). 2019a. Korea food code. Retrieved from https://www.foodsafetykorea.go.kr/portal/safefoodlife/food/foodRvlv/foodRvlv.do on Sep 24, 2019.
7 Dell’Aversano CD, Hess P and Quilliam MA. 2005. Hydrophilic interaction liquid chromatography-mass spectrometry for the analysis of paralytic shellfish poisoning (PSP) toxins. J Chromatogr A 1081, 190-201. https://doi.org/10.1016/j.chroma.2005.05.056.   DOI
8 Hall S. 1991. Natural toxins. In: Microbiology of marine food products. Ward DR and Hackney CR, eds. Van Nostrand Reinhold, New York, NY, U.S.A., 301-330.
9 Jang JH, Yun SM and Lee JS. 2005. Paralytic shellfish poison profile in commercial shellfishes. J Korean Soc Food Sci Nutr 34, 924-928. https://doi.org/10.3746/jkfn.2005.34.6.924.   DOI
10 KMFDS (Korea Ministry of Food and Drug Safety). 2019b. Korea food code. Retrieved from https://www.foodsafetykorea.go.kr/foodcode/01_03.jsp?idx=12 on Sep 27, 2019.
11 Lee KJ, Kwon SJ, Jung YJ, Son KT, Ha KS, Mok JS and Kim JH. 2017. Comparison of analytical methods for the detection of paralytic shellfish toxins. Korean J Fish Aquat Sci 50, 669-674. https://doi.org/10.5657/KFAS.2017.0669.   DOI
12 Luckas B, Hummert C and Oshima Y. 2003. Analytical methods for paralytic shellfish poisons. In: Manual on harmful marine microalgae, Hallegfaeff GM, Andersen DM, Cembella DA and Enevoldsen HO, eds. UNESCO, Paris, France, 191-209.
13 Mok JS, Oh EG, Son KT, Lee TS, Lee KJ, Song KC and Kim JH. 2012. Accumulation and depuration of paralytic shellfish poison in marin organisms. Korean J Fish Aquat Sci 45, 465-471. http://dx.doi.org/10.5657/KFAS.2012.0465.   DOI
14 Oshima Y. 1995. Post-column derivatization liquid-chromatograpic method for paralytic shellfish toxins. J AOAC Int 78, 528-532.   DOI
15 Mok JS, Song KC, Lee KJ and Kim JH. 2013. Validation of precolumn HPLC oxidation method for analysis of paralytic shellfish poison. Korean J Fish Aquat Sci 46, 147-153. https://doi.org/10.5657/KFAS.2013.0147.   DOI
16 Murakami R and Noguchi T. 2000. Paralytic shellfish poison. J Food Hyg Soc Jan 41, 1-10. https://doi.org/10.3358/shokueishi.41.1.
17 Noguchi T. 2003. Marine toxins. Nippon Suisan Gakkaishi 69, 895-909. https://doi.org/10.2331/suisan.69.895.   DOI
18 Rey V, Botana AM and Botana AM. 2017. Quantification of PSP toxins in toxic shellfish matrices using post-column oxidation liquid chromatography and pre-column oxidation liquid chromatography methods suggests post-column oxidation liquid chromatography as a good monitoring method of choice. Toxicon 129, 28-35. https://doi.org/10.1016/j.toxicon.2017.02.003.   DOI
19 Park MJ, Lee HJ, 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 Safe 15, 293-296.
20 Quilliam MA, Thomson BA, Scott GJ and Siu KW. 1989. Ion spray mass spectrometry of marine neurotoxins. Rapid Commun Mass Spectrom 3, 145-150. https://doi.org/10.1002/rcm.1290030508.   DOI
21 Song KC, Lee KJ, Yu HS, Mok JS, Kim JH, Lim KS and Lee MA. 2013. Paralytic shellfish poisoning (PSP) analysis using liquid chromatography-tandem mass spectrometry. Korean J Fish Aquat Sci 46, 154-159. https://doi.org/10.5657/KFAS.2013.0154.   DOI
22 Toyofuku H. 2006. Joint FAO/WHO/IOC activities to provide scientific advice on marine biotoxins(research report). Mar Pol Bull 52, 1735-1745. https://doi.org/10.1016/j.marpolbul.2006.07.007.   DOI
23 Yang X, Zhou L, Tan Y, Shi X, Zhao Z, Nie D, Zhou C and Liu H. 2017. Development and validation of a liquid chromatography-tandem mass spectrometry method coupled with dispersive solid-phase extraction for simultaneous quantification of eight paralytic shellfish poisoning toxins in shellfish. Toxins 9, 206. https://doi.org/10.3390/toxins9070206.   DOI
24 Turner AD, Hatfield RG, Maskrey BH, Algoet M and Lawrence JF. 2019. Evaluation of the new European Union reference method for paralytic shellfish toxins in shellfish: A review of twelve years regulatory monitoring using pre-column oxidation LC-FLD. Trend Anal Chem 113, 124-139. https://doi.org/10.1016/j.trac.2019.02.005.
25 Turner AD, McNabb PS, Harwood DT, Selwood AI and Boundy MJ. 2015. Single-laboratory validation of a multitoxin ultra performance LC-hydrophilic interaction LC-MS/MS method for quantitation of paralytic shellfish toxins in bivalve shellfish. J AOAC Int 98, 609-621. https://doi.org/10.5740/jaoacint.14-275.   DOI