Liquid chromatography with mass spectrometry: detection of lipophilic shellfish toxins
A rapid multiple toxin method based on liquid chromatography with mass spectrometry (LC/MS) was developed for the detection of okadaic acid (OA), dinophysistoxin-1 (DTX-1), DTX-2, yessotoxin (YTX), homoYTX, 45-hydroxy-YTX, 45-hydroxyhomo-YTX, pectenotoxin-1 (PTX-1), PTX-2, azaspiracid-1 (AZA-1), AZA...
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ftnrccanada:oai:cisti-icist.nrc-cnrc.ca:cistinparc:3538088 2023-05-15T15:58:58+02:00 Liquid chromatography with mass spectrometry: detection of lipophilic shellfish toxins Stobo, Lesley A. Lacaze, Jean-Pierre C. L. Scott, Alasdair C. Gallacher, Susan Smith, Elizabeth A. Quilliam, Michael A. 2005-09-01 text https://nrc-publications.canada.ca/eng/view/object/?id=f46ee715-e923-438e-99ad-73c1a658ec9a https://nrc-publications.canada.ca/fra/voir/objet/?id=f46ee715-e923-438e-99ad-73c1a658ec9a eng eng AOAC International Journal of Association of Official Analytical Chemists, Volume: 88, Issue: 5, Publication date: 2005-09-01, Pages: 1371–1382 Copyright © AOAC INTERNATIONAL 2007 All Rights Reserved liquid chromatography mass spectrometry shellfish toxins article 2005 ftnrccanada 2021-09-01T06:21:59Z A rapid multiple toxin method based on liquid chromatography with mass spectrometry (LC/MS) was developed for the detection of okadaic acid (OA), dinophysistoxin-1 (DTX-1), DTX-2, yessotoxin (YTX), homoYTX, 45-hydroxy-YTX, 45-hydroxyhomo-YTX, pectenotoxin-1 (PTX-1), PTX-2, azaspiracid-1 (AZA-1), AZA-2, and AZA-3. Toxins were extracted from shellfish using methanol–water (80%, v/v) and were analyzed using a C8 reversed-phase column with a 5 mM ammonium acetate–acetonitrile mobile phase under gradient conditions. The method was validated for the quantitative detection of OA, YTX, PTX-2, and AZA-1 in 4 species (mussels, Mytilus edulis; cockles, Cerastoderma edule; oysters, Crassostrea gigas; king scallop, Pecten maximus) of shellfish obtained from United Kingdom (UK) waters. Matrix interferences in the determination of the toxins in these species were investigated. The validated linear range of the method was 13–250 µg/kg for OA, PTX-2, and AZA-1 and 100–400 µg/kg for YTX. Recovery and precision ranged between 72–120 and 1–22%, respectively, over a fortification range of 40–160 µg/kg for OA, PTX-2, and AZA-1 and 100–400 µg/kg for YTX. The limit of detection, reproducibility, and repeatability of analysis showed acceptable performance characteristics. A further LC/MS method using an alkaline hydrolysis step was assessed for the detection of OA, DTX-1, and DTX-2 in their esterified forms. In combination with the LC/MS multiple toxin method, this allows detection of all toxin groups described in Commission Decision 2002/225/EC. Peer reviewed: Yes NRC publication: Yes Article in Journal/Newspaper Crassostrea gigas National Research Council Canada: NRC Publications Archive |
institution |
Open Polar |
collection |
National Research Council Canada: NRC Publications Archive |
op_collection_id |
ftnrccanada |
language |
English |
topic |
liquid chromatography mass spectrometry shellfish toxins |
spellingShingle |
liquid chromatography mass spectrometry shellfish toxins Stobo, Lesley A. Lacaze, Jean-Pierre C. L. Scott, Alasdair C. Gallacher, Susan Smith, Elizabeth A. Quilliam, Michael A. Liquid chromatography with mass spectrometry: detection of lipophilic shellfish toxins |
topic_facet |
liquid chromatography mass spectrometry shellfish toxins |
description |
A rapid multiple toxin method based on liquid chromatography with mass spectrometry (LC/MS) was developed for the detection of okadaic acid (OA), dinophysistoxin-1 (DTX-1), DTX-2, yessotoxin (YTX), homoYTX, 45-hydroxy-YTX, 45-hydroxyhomo-YTX, pectenotoxin-1 (PTX-1), PTX-2, azaspiracid-1 (AZA-1), AZA-2, and AZA-3. Toxins were extracted from shellfish using methanol–water (80%, v/v) and were analyzed using a C8 reversed-phase column with a 5 mM ammonium acetate–acetonitrile mobile phase under gradient conditions. The method was validated for the quantitative detection of OA, YTX, PTX-2, and AZA-1 in 4 species (mussels, Mytilus edulis; cockles, Cerastoderma edule; oysters, Crassostrea gigas; king scallop, Pecten maximus) of shellfish obtained from United Kingdom (UK) waters. Matrix interferences in the determination of the toxins in these species were investigated. The validated linear range of the method was 13–250 µg/kg for OA, PTX-2, and AZA-1 and 100–400 µg/kg for YTX. Recovery and precision ranged between 72–120 and 1–22%, respectively, over a fortification range of 40–160 µg/kg for OA, PTX-2, and AZA-1 and 100–400 µg/kg for YTX. The limit of detection, reproducibility, and repeatability of analysis showed acceptable performance characteristics. A further LC/MS method using an alkaline hydrolysis step was assessed for the detection of OA, DTX-1, and DTX-2 in their esterified forms. In combination with the LC/MS multiple toxin method, this allows detection of all toxin groups described in Commission Decision 2002/225/EC. Peer reviewed: Yes NRC publication: Yes |
format |
Article in Journal/Newspaper |
author |
Stobo, Lesley A. Lacaze, Jean-Pierre C. L. Scott, Alasdair C. Gallacher, Susan Smith, Elizabeth A. Quilliam, Michael A. |
author_facet |
Stobo, Lesley A. Lacaze, Jean-Pierre C. L. Scott, Alasdair C. Gallacher, Susan Smith, Elizabeth A. Quilliam, Michael A. |
author_sort |
Stobo, Lesley A. |
title |
Liquid chromatography with mass spectrometry: detection of lipophilic shellfish toxins |
title_short |
Liquid chromatography with mass spectrometry: detection of lipophilic shellfish toxins |
title_full |
Liquid chromatography with mass spectrometry: detection of lipophilic shellfish toxins |
title_fullStr |
Liquid chromatography with mass spectrometry: detection of lipophilic shellfish toxins |
title_full_unstemmed |
Liquid chromatography with mass spectrometry: detection of lipophilic shellfish toxins |
title_sort |
liquid chromatography with mass spectrometry: detection of lipophilic shellfish toxins |
publisher |
AOAC International |
publishDate |
2005 |
url |
https://nrc-publications.canada.ca/eng/view/object/?id=f46ee715-e923-438e-99ad-73c1a658ec9a https://nrc-publications.canada.ca/fra/voir/objet/?id=f46ee715-e923-438e-99ad-73c1a658ec9a |
genre |
Crassostrea gigas |
genre_facet |
Crassostrea gigas |
op_relation |
Journal of Association of Official Analytical Chemists, Volume: 88, Issue: 5, Publication date: 2005-09-01, Pages: 1371–1382 |
op_rights |
Copyright © AOAC INTERNATIONAL 2007 All Rights Reserved |
_version_ |
1766394752309133312 |