Analysis of synthetic antioxidants in salmon silage using QuEChERS extraction method followed by determination by LC-MS/MS; a single-laboratory validation study
| Autor: | K. Zahlsen, T. Holten, M. Sandrød, J.B. Øiaas, T.S. Guldberg, H.F. Kvitvang |
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| Rok vydání: | 2020 |
| Předmět: |
Calibration curve
Clinical Biochemistry Quechers Mass spectrometry 030226 pharmacology & pharmacy 01 natural sciences Biochemistry Antioxidants Analytical Chemistry Matrix (chemical analysis) 03 medical and health sciences chemistry.chemical_compound 0302 clinical medicine Limit of Detection Salmon Tandem Mass Spectrometry media_common.cataloged_instance Animals European union media_common Detection limit Silage Chromatography 010401 analytical chemistry Extraction (chemistry) Reproducibility of Results Cell Biology General Medicine 0104 chemical sciences chemistry Linear Models Butylated hydroxyanisole Chromatography Liquid |
| Zdroj: | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences. 1174 |
| ISSN: | 1873-376X |
| Popis: | A new method was developed and in-house validated to determined ethoxyquin (EQ), butylated hydroxyanisole (BHA) and propyl gallate (PG) in fish silage and fish oil used for production of animal feed. Sample pre-treatment comprises use of QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction and gives extracts for liquid chromatography-triple quadrupole mass spectrometry analysis without matrix interferences. The results allow quantification of the antioxidants in all matrices by using deuterated internal standards and calibration curves made in solvent, as well as establishing low detection limits (0.012–0.015 mg/kg) and quantification limits (0.040–0.050 mg/kg) needed regarding the recent suspension of EQ as feed additive within the European Union. The proposed method was validated in terms of linearity, accuracy (relative error, ±1.4%), precision (RSD, ≤2.7%) and recovery (matrix effect, 97–101%) where all the parameters show acceptable results according to recognized guidelines (including EuraChem) within method validation. Combined expanded measurement uncertainty was estimated with a coverage factor of 2 by including all contributors to analytical variation, showing results of ±15% or better. The combined QuEChERS and LC-MS/MS method was successfully applied to salmon silage samples and their corresponding aqueous and oil fractions. |
| Databáze: | OpenAIRE |
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