Sensitive method for the determination of lipophilic marine biotoxins in extracts of mussels and processed shellfish by high-performance liquid chromatography-tandem mass spectrometry based on enrichment by solid-phase extraction.
J Chromatogr A
; 1216(21): 4529-38, 2009 May 22.
Article
in En
| MEDLINE
| ID: mdl-19362722
ABSTRACT
A solid-phase extraction (SPE) method for the enrichment and clean-up of lipophilic marine biotoxins from extracts of different species of bivalve molluscs and processed shellfish products was developed. Okadaic acid (OA), pectenotoxin2 (PTX2), azaspiracid1 (AZA1) and yessotoxin (YTX) were determined by LC-MS/MS in hydrolyzed and non-hydrolyzed extracts. Applying a concentration factor of 10 the limit of quantification for the four toxins was determined to be 1 microg/kg. An organized in-house ring trial proved transferability of the method protocol and satisfactory results for all four toxins with a relative standard deviation (RSD) of 5-12%. The precision of the whole method including LC-MS detection was determined by processing seven independent extractions analyzed in independent sequences. RSD ranged between 12% and 24%. This SPE method was tested within a concentration range corresponding to the range of the current European Union regulatory limits (up to 160 microg/kg for the OA group), but it would also be applicable to a lower microg/kg range which is important in view of a possible decrease of regulatory limits as proposed by a working group of the European Food Safety Authority. The potential of SPE as a cleaning tool to cope with matrix effects in LC-MS/MS was studied and compared to liquid-liquid portioning.
Full text:
1
Collection:
01-internacional
Database:
MEDLINE
Main subject:
Shellfish
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Tissue Extracts
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Bivalvia
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Solid Phase Extraction
/
Food Analysis
/
Marine Toxins
Type of study:
Diagnostic_studies
Limits:
Animals
Language:
En
Journal:
J Chromatogr A
Year:
2009
Document type:
Article
Affiliation country: