Optimization of sample cleanup procedure for determination of diarrhetic shellfish poisoning toxins by use of experimental design

In routine monitoring of diarrhoeic shellfish poison (dinophysistoxin-1 and okadaic acid) there appeared to be an inconsistency between the mouse bioassay and existing chemical analysis based on liquid chromatography. The sample cleanup procedure has been subject to minor modifications in an effort...

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Published in	Journal of Chromatography A Vol. 764; no. 2; pp. 223 - 231
Main Authors	Aase, Brit, Rogstad, Astri
Format	Journal Article
Language	English
Published	Amsterdam Elsevier B.V 14.03.1997 Elsevier
Subjects	Anthryldiazomethane Biological and medical sciences Dinophysistoxin Fish and seafood industries Food industries Food toxicology Fundamental and applied biological sciences. Psychology Medical sciences Okadaic acid Toxicology Toxins Sample preparation Shellfish Experimental analysis Okadaic acid Dinophysistoxin Anthryldiazomethane Toxins Solid phase extraction Chemical analysis Mussel HPLC chromatography Foodstuff Derivatization Optimization Toxin Bivalvia Experimental design Food poisoning Invertebrata Mollusca Quantitative analysis
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ISSN	0021-9673
DOI	10.1016/S0021-9673(96)00938-7

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Abstract	In routine monitoring of diarrhoeic shellfish poison (dinophysistoxin-1 and okadaic acid) there appeared to be an inconsistency between the mouse bioassay and existing chemical analysis based on liquid chromatography. The sample cleanup procedure has been subject to minor modifications in an effort to overcome the problem. However, further studies have appeared necessary and in this study all experimental factors that can influence the sample cleanup using solid-phase extraction columns prior to the LC analysis have been evaluated by use of experimental statistical design in order to understand the effect of the various factors and to optimize the conditions for recovery of the toxins. Based on our experiments we suggest using a solid-phase extraction silica column of 100 mg in the sample cleanup procedure and washing solvents composed of dichloromethane instead of chloroform to minimize the effect of stabilizing alcohol. It is sufficient to apply 7.5 ml hexane–dichloromethane (1:1) to the column in the first washing step and 2.5 ml of dichloromethane in the final washing. Elution is complete by use of 2.5 ml chloroform with 3.5% methanol. Toxic shellfish tested by this procedure confirmed the mouse bioassay.
AbstractList	In routine monitoring of diarrhoeic shellfish poison (dinophysistoxin-1 and okadaic acid) there appeared to be an inconsistency between the mouse bioassay and existing chemical analysis based on liquid chromatography. The sample cleanup procedure has been subject to minor modifications in an effort to overcome the problem. However, further studies have appeared necessary and in this study all experimental factors that can influence the sample cleanup using solid-phase extraction columns prior to the LC analysis have been evaluated by use of experimental statistical design in order to understand the effect of the various factors and to optimize the conditions for recovery of the toxins. Based on our experiments we suggest using a solid-phase extraction silica column of 100 mg in the sample cleanup procedure and washing solvents composed of dichloromethane instead of chloroform to minimize the effect of stabilizing alcohol. It is sufficient to apply 7.5 ml hexane–dichloromethane (1:1) to the column in the first washing step and 2.5 ml of dichloromethane in the final washing. Elution is complete by use of 2.5 ml chloroform with 3.5% methanol. Toxic shellfish tested by this procedure confirmed the mouse bioassay.
Author	Rogstad, Astri Aase, Brit
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Keywords	Sample preparation Shellfish Experimental analysis Okadaic acid Dinophysistoxin Anthryldiazomethane Toxins Solid phase extraction Chemical analysis Mussel HPLC chromatography Foodstuff Derivatization Optimization Toxin Bivalvia Experimental design Food poisoning Invertebrata Mollusca Quantitative analysis
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References_xml	– reference: H.P. van Egmond, T. Aune, P. Lassus, G.J.A. Speijers and M. Waldock, J. Natural Toxins, 2 (1993) 41–83. – reference: F. Zonta, B. Stancher, P. Bogoni and P. Masotti, J. Chromatogr., 594 (1992) 137–144. – reference: O.B. Stabell, V. Hormazabal, I. Steffenak and K. Pedersen, Toxicon, 29 (1991) 21–29. – reference: T. Aune, Ø. Strand, B. Aase, J. Weidemann, E. Dahl and P. Hovgaard, Abstracts of 7th International Conference on Toxic Phytoplankton, Sendai, Japan, 1995, p. 4. – reference: J.L. Shen, C. Hummert, G. Ganzlin and B. Lukas, in W. Baltes, T. Eklund, R. Fenswick, W. Pfannhauser, A. Ruiter and H.P. Thier (Editors), Proceedings of European Conference on Food Chemistry, B. Behr, Hamburg, 1991, pp. 821–827. – reference: K. Akasaka, H. Ohrui, H. Meguro and T. Yasumoto, J. Chromatogr. A, 729 (1996) 381–386. – reference: B. Luckas, C. Hummert, G. Thielert, J. Kirschbaum and A. Boenke, BCR information, EUR15339, European Commission, Brussels, 1994, pp. 1–85. – reference: A. Pereira, D. Klein, K. Sohet, G. Houvenaghel and J.C. Braekman, in P. Lassus, G. Arzul, E. Erard, P. Gentien and C. Marcaillou (Editors), Harmful Marine Algal Blooms, Lavoisier, Intercept, 1995, pp. 333–338 and references cited therein. – reference: N. Ileby and A. Fiksdahl, in S.S. Bates and J. Worms (Editors), Proceedings of the First Canadian Workshop on Harmful Marine Algae, Canadian Technical Report of Fisheries and Aquatic Sciences, Moncton, 1712 (1989) 19–20. – reference: R.W. Dickey, H.R. Granade and F.A. Bencsath, in T.J. Smayda and Y. Shimizu (Editors), Toxic Phytoplankton Blooms in the Sea, Elsevier, Amsterdam, 1993, pp. 495–499. – reference: C. Hummert, J.L. Shen and B. Luckas, J. Chromatogr. A, 729 (1996) 387–392. – reference: M.A. Quilliam, J. AOAC Int., 78 (1995) 555–570. – reference: Marine Analytical Chemistry Standards Program, Reference Material Documentation: MUS-2, Halifax, Canada, version 1993, pp. 1–19. – reference: J.S. Lee, K. Tangen, E. Dahl, P. Hovgaard and T. Yasumoto, Nippon Suisan Gakkaishi, 54 (1988) 1953–1957. – reference: T. Yasumoto, Shokuhin Eiseigaku Zasshi, 31 (1981) 515–522. – reference: J.S. Lee, T. Yanagi, R. Kenma and T. Yasumoto, Agric. Biol. Chem., 51 (1987) 877–881. – ident: 10.1016/S0021-9673(96)00938-7_BIB6 doi: 10.1016/0041-0101(91)90036-Q – ident: 10.1016/S0021-9673(96)00938-7_BIB2 doi: 10.2331/suisan.54.1953 – ident: 10.1016/S0021-9673(96)00938-7_BIB3 – ident: 10.1016/S0021-9673(96)00938-7_BIB8 doi: 10.1016/0021-9673(95)01261-3 – ident: 10.1016/S0021-9673(96)00938-7_BIB5 – ident: 10.1016/S0021-9673(96)00938-7_BIB16 – ident: 10.1016/S0021-9673(96)00938-7_BIB4 – ident: 10.1016/S0021-9673(96)00938-7_BIB13 doi: 10.1016/0021-9673(95)00890-X – ident: 10.1016/S0021-9673(96)00938-7_BIB14 – ident: 10.1016/S0021-9673(96)00938-7_BIB15 – ident: 10.1016/S0021-9673(96)00938-7_BIB1 – ident: 10.1016/S0021-9673(96)00938-7_BIB11 – ident: 10.1016/S0021-9673(96)00938-7_BIB12 – ident: 10.1016/S0021-9673(96)00938-7_BIB10 – ident: 10.1016/S0021-9673(96)00938-7_BIB9 – ident: 10.1016/S0021-9673(96)00938-7_BIB7
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Snippet	In routine monitoring of diarrhoeic shellfish poison (dinophysistoxin-1 and okadaic acid) there appeared to be an inconsistency between the mouse bioassay and...
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SubjectTerms	Anthryldiazomethane Biological and medical sciences Dinophysistoxin Fish and seafood industries Food industries Food toxicology Fundamental and applied biological sciences. Psychology Medical sciences Okadaic acid Toxicology Toxins
Title	Optimization of sample cleanup procedure for determination of diarrhetic shellfish poisoning toxins by use of experimental design
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