Mass fraction assignment of Amino Acids in acidic aqueous solution (CCQM-K78.a)
Notice bibliographique
Résumé
The CCQM-K78.a comparison was coordinated by the BIPM on behalf of the CCQM Organic Analysis Working Group for NMIs and DIs which provide measurement services in organic analysis under the CIPM MRA. The key comparison forms part of the OAWG 10-year strategic plan of comparisons. CCQM-K78.a underpins the demonstration of capabilities for value assignment of high polarity calibration solutions. The model system selected was amino acids in aqueous solution. Participants were required to assign the mass fractions, expressed in μg/g, of phenylalanine (Phe), leucine (Leu), isoleucine (Ile) and proline (Pro) present in solution in 0.01 N hydrochloric acid. The content and analytical challenges of the selected analytes are representative of those for typical calibration solutions for polar organic analytes in aqueous solution. Participation in CCQM-K78, a benchmarked measurement capability for assigning the mass fraction content of polar organic compounds (pK ow > -2) present at a mass fraction range between 50 μg/g and 500 μg/g in an aqueous solution. It also tested capabilities for the quantitative assignment of isomeric polar compounds of similar chromatographic retention time properties. A satisfactory level of agreement of the results was obtained between participants and with gravimetric values for amino acid content. In the cases where the agreement was not satisfactory, the participants were able to identify a technical cause for the inconsistency. The comparison demonstrated the trueness and precision of double IDMS-based methods as a primary measurement procedure for the quantification of polar analytes in aqueous solution when an isotopically labelled version of the analyte is available as the internal standard. It also demonstrated that amino acid quantification using pre- or post-column derivatization with UV or FLD detection can provide results with comparable levels of performance. In this case, where the purity of the primary calibrators had been assigned with a relative standard uncertainty below 0.2%, results consistent with the KCRV within a relative expanded uncertainty in the range 1% - 2% could be realized and levels of 2%-4% were routinely achieved. KEY WORDS FOR SEARCH Amino acid quantification, leucine, isoleucine, proline, phenylalanine, calibration solution, standard solution, IDMS, primary measurement procedure, polar solution, peptide quantification Main text To reach the main text of this paper, click on Final Report . Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/ . The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).
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Comment cette classification a été obtenuedéplier
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 | 0,000 | 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) | 0,002 | 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 découleClassification
machine, non validéePrédiction automatique; un appel candidat d’une seule tête enseignante, pas un consensus.
Le détail, modèle par modèle et score par score, se trouve en fin de page sous « Comment cette classification a été obtenue ».