Refinement of AOAC Official MethodSM 2005.06 Liquid Chromatography-Fluorescence Detection Method to Improve Performance Characteristics for the Determination of Paralytic Shellfish Toxins in King and Queen Scallops
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Notice bibliographique
Résumé
AOAC Official Method 2005.06 LC-fluorescence detection (FLD) method is an official alternative to the mouse bioassay for the determination of paralytic shellfish poisoning (PSP) toxins in bivalve shellfish. To validate the method for species of relevance to the UK official control monitoring program, the method performance characteristics were tested for whole king and queen scallops. Validation showed that, while the performance was generally acceptable for the quantitation of non-N-hydroxylated toxins, poor toxin recovery and sensitivity was evident for the analysis of N-hydroxylated toxins following periodate oxidation. These effects occurred in a range of scallop samples with variable temporal and spatial sources. The effects were also noted in other laboratories following a small interlaboratory study. As a result, the method was refined to improve the recovery and sensitivity of analysis following the periodate oxidation step in the PSP method for scallops. Performance improved through alterations to the preparation of the periodate oxidant, use of higher volumes for C18 cleanup, and injection volumes in combination with the use of a king scallop matrix modifier for oxidation of N-hydroxylated toxin calibration standards. A single-laboratory validation of the refined method showed that the selectivity, linearity, sensitivity, recovery, and precision were acceptable and similar to values reported previously for AOAC Official Method 2005.06 in other bivalve species. Results showed the method to be rugged for all parameters investigated, including small changes to the composition of the new periodate reagent utilized in the refined method. The refined scallops LC method was subsequently compared with the European reference method. PSP-positive scallops showed an excellent agreement between the methods for queen and Atlantic scallops, with a small level of positive bias in the LC results for whole king scallops. These differences were related solely to the use of the highest toxicity equivalence factors for toxin epimeric pairs, with gonyautoxin (GTX)1,4 and GTX2,3 in particular present at high concentrations in the king scallops. Overall, the refined LC-FLD method improved the performance characteristics of AOAC Official Method 2005.06 for the determination of PSP toxins in whole king and queen scallops, and showed a good overall agreement between the official methodologies. It is, therefore, recommended as a more appropriate option for the routine monitoring of PSP toxins in these species.
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Prédiction distillée sur la base complète
Imitation des enseignantsNi prévalence calibrée, ni vérité terrain. Validation humaine à venir. Apprise à partir de 10 348 étiquettes directes de Codex et de 10 348 étiquettes directes de Gemma. Le mode candidate est l'union des têtes enseignantes seuillées; le consensus est leur intersection. Ces sorties portent le statut machine_predicted_unvalidated et ne sont ni des étiquettes humaines ni des étiquettes directes de modèles de pointe.
Scores Codex et Gemma par catégorie
| Catégorie | Codex | Gemma |
|---|---|---|
| Métarecherche | 0,003 | 0,000 |
| Méta-épidémiologie (sens strict) | 0,000 | 0,000 |
| Méta-épidémiologie (sens large) | 0,000 | 0,000 |
| Bibliométrie | 0,000 | 0,000 |
| Études des sciences et des technologies | 0,000 | 0,000 |
| Communication savante | 0,000 | 0,000 |
| Science ouverte | 0,000 | 0,000 |
| Intégrité de la recherche | 0,000 | 0,000 |
| Charge utile insuffisante (le modèle a refusé de juger) | 0,000 | 0,000 |
Scores machine (provisoires)
Les deux têtes enseignantes du modèle étudiant, lues sur ce travail. Un score ordonne la base pour la relecture; il n'affirme jamais une catégorie, et le statut de validation accompagne chaque rangée tel quel.
Scores de référence d'un modèle non mature (critères de maturité non atteints, 7 itérations). Un score ordonne; il n'affirme jamais une catégorie.
score_only:v0-immature-baseline · tel quel depuis la passe de notation : score_only signifie que le nombre peut ordonner les travaux, et qu'aucune étiquette de catégorie n'en découle