BS EN 16204:2012
Current
The latest, up-to-date edition.
Foodstuffs. Determination of lipophilic algal toxins (okadaic acid group toxins, yessotoxins, azaspiracids, pectenotoxins) in shellfish and shellfish products by LC-MS/MS
Hardcopy , PDF
English
31-05-2012
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Foreword
Introduction
1 Scope
2 Normative references
3 Principle
4 Reagents
5 Apparatus
6 Procedure
7 HPLC-MS/MS analysis
8 Calculation
9 Precision
10 Test report
Annex A (informative) - Precision data
Annex B (informative) - Examples for suitable
MS detection conditions
Annex C (informative) - Typical chromatogram
Bibliography
Defines a multi-reference method for the determination of lipophilic algal toxins (fatsoluble algal toxins produced by some dinoflagellates) in raw shellfish and shellfish products including cooked shellfish, by liquid chromatography coupled to tandem mass spectrometry LC-MS/MS [1], [2], [3].
| Committee |
AW/275
|
| DevelopmentNote |
Supersedes 10/30234561 DC. (05/2012) Reviewed and confirmed by BSI, April 2018. (04/2018)
|
| DocumentType |
Standard
|
| Pages |
44
|
| PublisherName |
British Standards Institution
|
| Status |
Current
|
| Supersedes |
This European Standard specifies a multi-reference method for the determination of lipophilic algal toxins (fat-soluble algal toxins produced by some dinoflagellates) in raw shellfish and shellfish products including cooked shellfish, by liquid chromatography coupled to tandem mass spectrometry LC-MS/MS [1], [2], [3]. This method has been validated in an inter-laboratory study consisting of three parts via the analysis of both naturally contaminated homogenates of blue mussel and spiked extracts of blue mussel, oyster and clam. For further information on the validation, see Annex A. Additional studies have investigated further matrices (see [4], [5]). The detection limit for toxins of the okadaic acid group, azaspiracids and pectenotoxins was determined to be 6 µg/kg shellfish meat and for yessotoxins 10 µg/kg shellfish meat. Quantitative determination of okadaic acid (OA), pectenotoxin 2 (PTX-2), azaspiracid-1 (AZA-1) and yessotoxin (YTX) can be carried out directly by means of standard substances available commercially. Assuming an equal response factor, okadaic acid is used for the indirect quantitative determination of the two dinophysistoxins dinophysistoxin-1 (DTX-1) and dinophysistoxin 2 (DTX-2); likewise azaspiracid 1 (AZA-1) is used for the indirect quantitative determination of azaspiracid-2 (AZA-2) and azaspiracid-3 (AZA-3), while YTX is used for homo-yessotoxin, 45-OH-yessotoxin and 45-OH-homo-yessotoxin, and PTX-2 for pectenotoxin-1 (PTX-1). The limit of quantification (LOQ) for toxins of the okadaic acid group, azaspiracids and pectenotoxins was determined to be 20 µg/kg shellfish meat and for yessotoxins 35 µg/kg shellfish meat. By means of hydrolysis [6], the esters of okadaic acid, DTX-1 and DTX-2 can also be determined quantitatively as the corresponding free acids.
| Standards | Relationship |
| EN 16204:2012 | Identical |
| ISO 5725-6:1994 | Accuracy (trueness and precision) of measurement methods and results — Part 6: Use in practice of accuracy values |
| ISO 5725-4:1994 | Accuracy (trueness and precision) of measurement methods and results Part 4: Basic methods for the determination of the trueness of a standard measurement method |
| ISO 5725-2:1994 | Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method |
| EN ISO 3696:1995 | Water for analytical laboratory use - Specification and test methods (ISO 3696:1987) |
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