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This paper describes the validation of an LC-MS/MS-based method for the quantification of > 500 secondary microbial metabolites. Analytical performance parameters have been determined for seven food matrices using seven individual samples per matrix for spiking. Apparent recoveries ranged from 70 to 120% for 53–83% of all investigated analytes (depending on the matrix). This number increased to 84–94% if the recovery of extraction was considered. The comparison of the fraction of analytes for which the precision criterion of RSD ≤ 20% under repeatability conditions (for 7 replicates derived from different individual samples) and intermediate precision conditions (for 7 technical replicates from one sample), respectively, was met (85–97% vs. 93–94%) highlights the contribution of relative matrix effects to the method uncertainty. Statistical testing of apparent recoveries between pairs of matrices exhibited a significant difference for more than half of the analytes, while recoveries of the extraction showed a much better agreement. Apparent recoveries and matrix effects were found to be constant over 2–3 orders of magnitude of analyte concentrations in figs and maize, whereas the LOQs differed less than by a factor of 2 for 90% of the investigated compounds. Based on these findings, this paper discusses the applicability and practicability of current guidelines for multi-analyte method validation. Investigation of (apparent) recoveries near the LOQ seems to be insufficiently relevant to justify the enormous time-effort for manual inspection of the peaks of hundreds of analytes. Instead, more emphasis should be put on the investigation of relative matrix effects in the validation procedure.
Michael Sulyok; David Stadler; David Steiner; Rudolf Krska. Validation of an LC-MS/MS-based dilute-and-shoot approach for the quantification of > 500 mycotoxins and other secondary metabolites in food crops: challenges and solutions. Analytical and Bioanalytical Chemistry 2020, 412, 2607 -2620.
AMA StyleMichael Sulyok, David Stadler, David Steiner, Rudolf Krska. Validation of an LC-MS/MS-based dilute-and-shoot approach for the quantification of > 500 mycotoxins and other secondary metabolites in food crops: challenges and solutions. Analytical and Bioanalytical Chemistry. 2020; 412 (11):2607-2620.
Chicago/Turabian StyleMichael Sulyok; David Stadler; David Steiner; Rudolf Krska. 2020. "Validation of an LC-MS/MS-based dilute-and-shoot approach for the quantification of > 500 mycotoxins and other secondary metabolites in food crops: challenges and solutions." Analytical and Bioanalytical Chemistry 412, no. 11: 2607-2620.
Deoxynivalenol (DON), a frequent contaminant of flour, can be partially degraded by baking. It is not clear: (i) How the choice of processing parameter (i.e., ingredients, leavening, and baking conditions) affects DON degradation and thus (ii) how much DON can be degraded during the large-scale industrial production of bakery products. Crackers, biscuits, and bread were produced from naturally contaminated flour using different processing conditions. DON degradation during baking was quantified with the most accurate analytical methodology available for this Fusarium toxin, which is based on liquid chromatography tandem mass spectrometry. Depending on the processing conditions, 0–21%, 4–16%, and 2–5% DON were degraded during the production of crackers, biscuits, and bread, respectively. A higher NaHCO3 concentration, baking time, and baking temperature caused higher DON degradation. NH4HCO3, yeast, vinegar, and sucrose concentration as well as leavening time did not enhance DON degradation. In vitro cell viability assays confirmed that the major degradation product isoDON is considerably less toxic than DON. This proves for the first time that large-scale industrial baking results in partial detoxification of DON, which can be enhanced by process management.
David Stadler; Francesca Lambertini; Lydia Woelflingseder; Heidi Schwartz-Zimmermann; Doris Marko; Michele Suman; Franz Berthiller; Rudolf Krska. The Influence of Processing Parameters on the Mitigation of Deoxynivalenol during Industrial Baking. Toxins 2019, 11, 317 .
AMA StyleDavid Stadler, Francesca Lambertini, Lydia Woelflingseder, Heidi Schwartz-Zimmermann, Doris Marko, Michele Suman, Franz Berthiller, Rudolf Krska. The Influence of Processing Parameters on the Mitigation of Deoxynivalenol during Industrial Baking. Toxins. 2019; 11 (6):317.
Chicago/Turabian StyleDavid Stadler; Francesca Lambertini; Lydia Woelflingseder; Heidi Schwartz-Zimmermann; Doris Marko; Michele Suman; Franz Berthiller; Rudolf Krska. 2019. "The Influence of Processing Parameters on the Mitigation of Deoxynivalenol during Industrial Baking." Toxins 11, no. 6: 317.