Ion‐spray mass spectrometry of marine neurotoxins

Quilliam, Michael A.; Thomson, Bruce A.; Scott, George J.; Siu, Kin Wai Michael

doi:10.1002/rcm.1290030508

Cited by 128 publications

(40 citation statements)

References 21 publications

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“…Several laboratories have reported improvements to the method, such as the in situ method for preparation of the reagent (Yoshida et al, 1988;Quilliam et al, 1998) and better cleanup procedures (Quilliam, 1995;Stabell et al, 1991). LC combined with mass spectrometry (LC/ MS) is another method that is gaining acceptance as a good quantitative and confirmatory method for toxins (Quilliam, 1995;Quilliam et al, 1989).…”

Section: Introductionmentioning

confidence: 99%

Further Studies on the Analysis of DSP Toxin Profiles in Galician Mussels

Leão

Gago-Martı́nez

Vázquez

et al. 1999

J. Agric. Food Chem.

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Vous avez des questions? Nous pouvons vous aider. Pour communiquer directement avec un auteur, consultez la première page de la revue dans laquelle son article a été publié afin de trouver ses coordonnées. Si vous n'arrivez pas à les repérer, communiquez avec nous à PublicationsArchive-ArchivesPublications@nrc-cnrc.gc.ca. Questions? Contact the NRC Publications Archive team atPublicationsArchive-ArchivesPublications@nrc-cnrc.gc.ca. If you wish to email the authors directly, please see the first page of the publication for their contact information. NRC Publications Archive Archives des publications du CNRCThis publication could be one of several versions: author's original, accepted manuscript or the publisher's version. / La version de cette publication peut être l'une des suivantes : la version prépublication de l'auteur, la version acceptée du manuscrit ou la version de l'éditeur. NRC Publications Record / Notice d'Archives des publications de CNRC:http://nparc.cisti-icist.nrc-cnrc.gc.ca/eng/view/object/?id=339aafca-a308-4ddf-b8d4-528ff1d1093d http://nparc.cisti-icist.nrc-cnrc.gc.ca/fra/voir/objet/?id=339aafca-a308-4ddf-b8d4-528ff1d1093d Further studies on mussel samples from Galicia, Spain, have revealed the presence of okadaic acid (OA), dinophysistoxin 2 (DTX2), and the fatty acid acyl esters of both of these toxins as the "DTX3" complex. Measurements were performed with an improved in situ method for the formation of 9-anthryldiazomethane (ADAM) derivatives followed by liquid chromatography with fluorescence detection. Base hydrolysis of DTX3 toxins gave free OA and DTX2, which were determined following ADAM derivatization. Results were confirmed by liquid chromatography/mass spectrometry analyses, and in most of the samples, free DTX2 was the most abundant toxin. However, the OA/DTX2 ratio in the DTX3 conjugated form was different, with OA being the most abundant in all cases. This difference could be due to different rates of metabolism of OA and DTX2 to the acyl esters or due to contamination of the shellfish by the two toxins at different points in time, resulting in less acyl ester formation for one toxin versus the other. The second possibility would be reasonable if two different source organisms were producing the toxins. Further Studies on the Analysis of DSP Toxin Profiles in Galician Mussels

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Section: Introductionmentioning

confidence: 99%

Further Studies on the Analysis of DSP Toxin Profiles in Galician Mussels

Leão

Gago-Martı́nez

Vázquez

et al. 1999

J. Agric. Food Chem.

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“…15 This acid is volatile and is compatible with HPLC/MS. It has been shown that a low concentration of a volatile buffer at low pH maximizes ionization efficiency and sensitivity for ISP-MS. 16 Our current study applies HPLC with ionspray ionization and a tandem mass spectrometry strategy (HPLC/ISP-MS/MS) to the detection of paraquat and diquat in water samples. Multiple reaction monitoring (MRM) was chosen because of the added selectivity that it provides.…”

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confidence: 99%

A Simple High Performance Liquid Chromatography/Ionspray Tandem Mass Spectrometry Method for the Direct Determination of Paraquat and Diquat in Water

Marr¹,

King²

1997

Rapid Commun. Mass Spectrom.

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A method has been developed for the direct determination of paraquat and diquat in water samples. No sample preparation was required and analysis was done using high performance liquid chromatography coupled with ionspray tandem mass spectrometry. Heptafluorobutyric acid was used as the ion-pair agent. Further improvements in this method included the incorporation of an internal standard (caffeine). Using this method, detection limits of 5 and 1 µg/L were obtained for paraquat and diquat respectively. Recoveries were consistently > 90% with relative standard deviations of < 10% over the concentration range 5-100 µg/L. To our knowledge, this method is the first application of ionspray tandem mass spectrometry, and the first to use heptafluorobutyric acid as an ion-pair reagent, for the analysis of paraquat and diquat.

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“…Recently, the U.S. Food and Drug Administration increased the permissible level of DA in Dungeness et al, Grimmelt et a]., 19901, direct detection-UV HPLC [Lawrenceet al, 1989a[Lawrenceet al, , 1991Quilliametal., 1989a1, chemical and fluorescence derivative HPLC [Lawrence et a]., 1989b; Pockington et al, 19901, LC or GC-MS [Quilliam et al, 1989b;Pleasance et a]., 1990; Musser et al, 19921, radio immunoassay (RIA), and enzyme-linked immunosorbant assay (ELISA) [Newsome et al, 19911. Of these methods, HPLC with direct detection of DA at 242 nm (A max) combined with a solid phase extraction (SPE) clean-up procedure has evolved as the method of choice for rapid monitoring purposes.…”

Section: Introductionmentioning

confidence: 99%

Salt clean‐up procedure for the determination of domoic acid by HPLC

et al. 1994

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Domoic acid (DA) was first reported in mussels from Prince Edward Island, Canada, in 1987. It reappeared in anchovies and pelicans from Monterey Bay, California, in 1991. Later that year, domoic acid was found in razor clams and Dungeness crabs along the Washington and Oregon coasts. Since the initial outbreak, a variety of analytical methods for the detection of this neurotoxin have been developed. Here, we describe a modification to the solid phase extraction (SPE) clean-up step in Quilliam's HPLC-UV method (1991: NRCC No. 33001). The standard 10% acetonitrile (MeCN) wash and 0.5M ammonium citrate buffer (ACB) in 10% MeCN (pH = 4.5) eluting solution have been replaced with a 0.1M sodium chloride (NaCl) in 10% MeCN wash and a 0.5M NaCl in 10% MeCN eluting solution. This modification allows the analysis to work equally well on both clam and crab viscera and meat. Chromatograms of visceral samples no longer contain interfering or late eluting peaks; and all chromatograms are free of the large solvent peak tailing associated with the ACB eluent. The newly modified method allows for an improved and more versatile domoic acid analysis.

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Ion‐spray mass spectrometry of marine neurotoxins

Cited by 128 publications

References 21 publications

Further Studies on the Analysis of DSP Toxin Profiles in Galician Mussels

Further Studies on the Analysis of DSP Toxin Profiles in Galician Mussels

A Simple High Performance Liquid Chromatography/Ionspray Tandem Mass Spectrometry Method for the Direct Determination of Paraquat and Diquat in Water

Salt clean‐up procedure for the determination of domoic acid by HPLC

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