| Téléchargement | - Voir le manuscrit accepté : Determination of thiocyanate in saliva by headspace gas chromatography-mass spectrometry, following a single-step aqueous derivatization with triethyloxonium tetrafluoroborate (PDF, 1.2 Mio)
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| DOI | Trouver le DOI : https://doi.org/10.1016/j.chroma.2015.04.040 |
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| Auteur | Rechercher : Ammazzini, Sara; Rechercher : Onor, Massimo; Rechercher : Pagliano, Enea1; Rechercher : Mester, Zoltán1Identifiant ORCID : https://orcid.org/0000-0002-2377-2615; Rechercher : Campanella, Beatrice; Rechercher : Pitzalis, Emanuela; Rechercher : Bramanti, Emilia; Rechercher : D'Ulivo, Alessandro |
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| Affiliation | - Conseil national de recherches du Canada. Science des mesures et étalons
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| Format | Texte, Article |
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| Sujet | thiocyanate; saliva; smokers and nonsmokers; triethyloxonium tetrafluoroborate derivatization; GC/MS; isotope dilution |
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| Résumé | A novel method for the determination of salivary thiocyanate is presented. Thiocyanate was converted into ethyl thiocyanate by single-step aqueous derivatization based on triethyloxonium tetrafluoroborate and measured by gas chromatography-mass spectrometry (15min runtime). The ethyl thiocyanate derivative is volatile and can be sampled from the headspace. The derivatization chemistry proposed allows for separation of the analyte from saliva matrix whose introduction in the measurement system is avoided. Quantitation of the analyte was obtained by isotope dilution, employing a 13C-enriched thiocyanate as internal standard. Technical details and fundamental aspects of derivatization chemistry and calibration strategy are presented.The method was validated by comparison with a standard method based on ion chromatography. The two independent methodologies produced results in agreement within 3%. Also a three level spike recovery test was carried out for validation purpose and quantitative recoveries were attained. The method is fast, simple, safe, and sensitive. Measurement of a 1. mL volume 50. ng/g of thiocyanate standard produced a signal-to-noise ratio of 250 for the analytical peak. This method is therefore suitable for ultra-trace determination of thiocyanate (low part-per-billion range). For the application described the full detection potential of the method was not required and the sample preparation presented has been designed for quantitation of saliva samples containing 1-400. μg/g of thiocyanate with a combined standard uncertainty of 2% relative for saliva samples containing 25. μg/g of thiocyanate. This method was applied for the determination of thiocyanate in human saliva samples. |
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| Date de publication | 2015-06-26 |
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| Maison d’édition | Elsevier |
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| Dans | |
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| Langue | anglais |
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| Publications évaluées par des pairs | Oui |
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| Numéro NPARC | 21275825 |
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| Exporter la notice | Exporter en format RIS |
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| Signaler une correction | Signaler une correction (s'ouvre dans un nouvel onglet) |
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| Identificateur de l’enregistrement | a8070629-de69-4fa5-83d8-5d59b7dd0f78 |
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| Enregistrement créé | 2015-07-14 |
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| Enregistrement modifié | 2020-06-04 |
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