| Download | - View accepted manuscript: Certification of nitrate in spinach powder reference material SPIN-1 by high-precision isotope dilution GC–MS (PDF, 1.4 MiB)
- View supplementary information part 1: Certification of nitrate in spinach powder reference material SPIN-1 by high-precision isotope dilution GC–MS (PDF, 228 KiB)
- View supplementary information part 2: Certification of nitrate in spinach powder reference material SPIN-1 by high-precision isotope dilution GC–MS (XLSM, 40 KiB)
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| DOI | Resolve DOI: https://doi.org/10.1007/s00216-019-01803-4 |
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| Author | Search for: Pagliano, Enea1; Search for: Meija, Juris1ORCID identifier: https://orcid.org/0000-0002-3349-5535; Search for: Campanella, Beatrice; Search for: Onor, Massimo; Search for: Iammarino, Marco; Search for: D’amore, Teresa; Search for: Berardi, Giovanna; Search for: D’imperio, Massimiliano; Search for: Parente, Angelo; Search for: Mihai, Ovidiu1; Search for: Mester, Zoltán1ORCID identifier: https://orcid.org/0000-0002-2377-2615 |
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| Affiliation | - National Research Council of Canada. Metrology Research Centre
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| Format | Text, Article |
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| Subject | certified reference material; dietary nitrate; leafy vegetable; isotope dilution |
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| Abstract | A high-precision exact-matching quadruple isotope dilution method (ID4MS) was employed for the quantitation of nitrate in an air-dried spinach powder Certified Reference Material (CRM). The analyte was extracted in hot water following addition of ¹⁵NO⁻₃ internal standard. The blend was then treated with sulfamic acid to remove nitrite and with triethyloxonium tetrafluoroborate to promote aqueous conversion of nitrate into volatile EtONO₂. The derivative was analyzed by headspace GC–MS with 3-min elution time. The method performance was validated with a series of tests which demonstrated adequate selectivity and ruggedness. This method supported the development of novel SPIN₋₁ CRM giving a modest contribution to its uncertainty (uchar = 0.85%). With respect to previous attempts, the SPIN was proven stable, homogeneous (uhom = 0.44%), and suitable for spinach monitoring under EU regulations. On dried basis, the nitrate content of SPINU regulations. On dried basis, the nitrate content of SPIN₋₁ was found to be 22.53 ± 0.43 mg/g (Uc = 1.9%, k = 2). The material was also used in an inter-laboratory study where four laboratories employed a total of ten measurement methods. |
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| Publication date | 2019-05-15 |
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| Publisher | Springer |
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| In | |
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| Language | English |
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| Peer reviewed | Yes |
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| Export citation | Export as RIS |
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| Report a correction | Report a correction (opens in a new tab) |
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| Record identifier | f4928323-dae5-41b9-9f2e-e4f876889f92 |
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| Record created | 2021-02-05 |
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| Record modified | 2024-09-24 |
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