Multiresidue LS-MS analysis of ASP and DSP toxins in shellfish: Validation and laboratory QA/QC data

P.T. Holland; P.S. McNabb; A.I. Selwood; R. Van Ginkel

Multiresidue LS-MS analysis of ASP and DSP toxins in shellfish: Validation and laboratory QA/QC data

in Mycotoxins and phycotoxins

Autor:innen:

P.T. Holland

P.T. Holland Cawthron Institute, 98 Halifax Street East, Nelson 7001, New Zealand; patrick.holland@cawthron.org.nz

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P.S. McNabb

P.S. McNabb Cawthron Institute, 98 Halifax Street East, Nelson 7001, New Zealand; patrick.holland@cawthron.org.nz

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A.I. Selwood

A.I. Selwood Cawthron Institute, 98 Halifax Street East, Nelson 7001, New Zealand; patrick.holland@cawthron.org.nz

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, und

R. Van Ginkel

R. Van Ginkel Cawthron Institute, 98 Halifax Street East, Nelson 7001, New Zealand; patrick.holland@cawthron.org.nz

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Art:: Kapitel

Seiten:: 333–343

DOI:: https://doi.org/10.3920/9789086865857_035

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Progress is reviewed with validation and routine application of an LC-MS/MS method for highly sensitive and specific determination of ASP, DSP and other lipophilic algal toxins and metabolites in shellfish. Tissue homogenates are blended with 90% aqueous methanol and the centrifuged extracts cleaned-up with a hexane wash. LC-MS uses reversed phase gradient elution with an acidic buffer, electrospray (+ & - ion modes) and triple quadrupole MS-MS detection. The method is quantitative for six key toxins where reference standards are available: azaspiracid-1 (AZA1), domoic acid (DA), gymnodimine (GYM), okadaic acid (OA and OA-esters, following hydrolysis), pectenotoxin-2 (PTX2) and yessotoxin (YTX). Relative response factors are used to estimate concentrations for a range of related toxins and metabolites. The extensive within-lab validation of the method was augmented by comparative studies on toxin extractability and stability, and a small inter-laboratory study. Successive extractions showed that a single extraction with 90% methanol was more effective than a single extraction with 80% methanol for AZA1, YTX and esters of OA and DTX2. There was little effect of time between homogenisation and extraction on levels of most toxins (6 min to 22 hours at 20 oC). However, low levels of PTX2 and 7-epiPTX2 seco acid significantly increased with time. Steaming shellfish prior to tissue homogenisation caused a 2-fold decrease in measured YTX. Eight laboratories generally obtained consistent inter-lab data for toxins in shellfish extracts. Between-lab reproducibility was satisfactory for seven key toxins (HORRAT 0.8 – 1.9). The new method is fit for the purpose of regulating ASP and DSP toxins in shellfish and has been in routine use for over two years. QA/QC data is summarised for 259 batches of shellfish samples from New Zealand public health and industry monitoring programmes. The precision of the method was sustained over extended periods and was consistent with estimates of the uncertainty of measurement from the validations.

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Mycotoxins and phycotoxins

Advances in determination, toxicology and exposure management

ISBN:: 9789086865857

Verleger:: Wageningen Academic

Print-Publikationsdatum:: 30 Oct 2006

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Multiresidue LS-MS analysis of ASP and DSP toxins in shellfish: Validation and laboratory QA/QC data

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Mycotoxins and phycotoxins

Advances in determination, toxicology and exposure management

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