Determination of Brevetoxins in Shellfish by LC/MS/MS: Single-Laboratory Validation

A single-laboratory validation is reported for an LC/MS/MS quantification of six brevetoxins in four matrixes (Greenshell mussel, eastern oyster, hard clam, and Pacific oyster). Recovery and precision data were collected from seven analytical batches using shellfish flesh at 0.05 mg/kg. Method recov...

Full description

Saved in:
Bibliographic Details
Published in:Journal of AOAC International 2012-07, Vol.95 (4), p.1097-1105
Main Authors: MCNABB, Paul S, SELWOOD, Andrew I, VAN GINKEL, Roel, BOUNDY, Michael, HOLLAND, Patrick T
Format: Article
Language:English
Subjects:
Animals
Biological and medical sciences
Biological Assay - methods
Bivalvia
Chemical properties
Chromatography, Liquid - methods
Fish and seafood industries
Food Analysis - methods
Food Contamination
Food industries
Fundamental and applied biological sciences. Psychology
Laboratories
Liquid chromatography
Marine Toxins - analysis
Mass spectrometry
Methods
Mice
Ostreidae
Oxocins - analysis
Physiological aspects
Reference Values
Reproducibility of Results
Shellfish
Shellfish Poisoning - prevention & control
Tandem Mass Spectrometry - methods
Toxins, Biological - analysis
Citations: Items that cite this one
Online Access:Get full text
Tags: Add Tag
No Tags, Be the first to tag this record!
Description
Summary:A single-laboratory validation is reported for an LC/MS/MS quantification of six brevetoxins in four matrixes (Greenshell mussel, eastern oyster, hard clam, and Pacific oyster). Recovery and precision data were collected from seven analytical batches using shellfish flesh at 0.05 mg/kg. Method recoveries and within-laboratory reproducibility ranged from 73 to 112%, with an RSD between 14 and 18% for brevetoxin-3, brevetoxin B5, brevetoxin B2, and S-desoxy brevetoxin B2. The recovery and within-laboratory reproducibility for brevetoxin-2 was 61%, with an RSD of 27%. Brevetoxin B1 gave an RSD of 12%, but no reference material was available and this toxin was only recorded in a hard clam sample naturally contaminated with brevetoxins. One naturally contaminated sample of each shellfish matrix, with brevetoxin levels ranging from 0.012 to 9.9 mg/kg, was tested in multiple batches, and the RSDs were similar to those for fortified samples at 0.05 mg/kg. Comparisons with limited data for the neurotoxic shellfish poisoning mouse bioassay for four naturally contaminated shellfish samples showed that the regulatory action limit of 0.8 mg/kg is conservative with respect to the bioassay regulatory limit of 20 mouse units/100 g.
ISSN:1060-3271
1944-7922
DOI:10.5740/jaoacint.11-272