Single laboratory validation data and uncertainty estimation of a liquid chromatographic method for determination of aflatoxin B1 in animal feed
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In the present work we have validated an analytical method for the determination of aflatoxin B1 in dairy compound feeds and peanut meal. The method is based on a preliminary extraction with a mixture of methanol and water followed by a clean-up step with immunoaffinity column. The content of aflatoxin B1 is then established using reversed-phase high-performance liquid chromatography coupled with fluorescence detection. The method is fully validated by using Certified Reference Materials. Limit of detection is found to be 0.5x10-3 mg/kg. The Bartlett test has shown that the method is affected by a systematic error and as a consequence the results must be corrected for the recovery. The precision is found in all cases lower than those calculated by Horwitz equation. Uncertainty estimation has been performed taking into account the bottom-up approach as stated in the Eurachem/Citac guide. With this method the uncertainty is calculated by the addition of variances for a measurand M when the equation for the calculation of M is based only on multiplications and divisions. The bottom-up approach is a tool which identifies the parameters or working steps with an overly contribution to the total uncertainty, thus offering the chance to improve them. The final uncertainty budget has revealed that the main contributions to global uncertainty are those due to the recovery and to the calibration function.
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Barmark, A.L. and Larsson, K., 1994. Immunoaffinity Column Cleanup/Liquid Chromatographic determination of aflatoxins: an interlaboratory study. Journal of AOAC International 77: 46-53.
'Immunoaffinity Column Cleanup/Liquid Chromatographic determination of aflatoxins: an interlaboratory study ' () 77 Journal of AOAC International : 46 -53 .
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Barwick, V.J. and Ellison, L.R., 1999. Measurement uncertainty: approaches to the evaluation of uncertainty associated with recovery. Analyst 124: 981-990.
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'Assessment of quality performance parameters for straight line calibration curves related to the spread of the abscissa values around their mean ' () 584 Analytica Chimica Acta : 57 -65 .
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European Commission (EC), 2003. Commission Directive 2003/100/ EC of 31 October 2003 amending Annex I to Directive 2002/32/ EC of the European Parliament and of the Council on undesirable substances in animal feed. Official Journal of the European Union L 285: 33-37.
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European Commission (EC), 2006. Commission Regulation 401/2006 of 23 February 2006 laying down the methods of sampling and analysis for the official control of the levels of mycotoxins in foodstuffs. Official Journal of the European Union L 70: 12-34.
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Eurachem/Citac, 2000. Quantifying Uncertainty in Analytical Measurement. 2nd ed. Available at: http://www.eurachem.org. http://www.eurachem.org
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Eurachem/Citac, 1998. The Fitness for Purpose of Analytical methods. A Laboratory Guide to Method Validation and Related Topics edition 1.0 LGC. Available at: http://www.eurachem.org. http://www.eurachem.org
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Kok, W.T., 1994. Derivatization reaction for the determination of aflatoxins by liquid chromatography with fluorescence detection. Journal of Chromatography B 659: 127-137.
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| All Time | Past 365 days | Past 30 Days | |
|---|---|---|---|
| Abstract Views | 166 | 69 | 10 |
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Single laboratory validation data and uncertainty estimation of a liquid chromatographic method for determination of aflatoxin B1 in animal feed
In: World Mycotoxin JournalSearch for other papers by M. Nocentini in
Current site
Google Scholar
PubMed
Search for other papers by C. Focardi in
Current site
Google Scholar
PubMed
Search for other papers by S. Ninci in
Current site
Google Scholar
PubMed
Search for other papers by G. Biancalani in
Current site
Google Scholar
PubMed
In the present work we have validated an analytical method for the determination of aflatoxin B1 in dairy compound feeds and peanut meal. The method is based on a preliminary extraction with a mixture of methanol and water followed by a clean-up step with immunoaffinity column. The content of aflatoxin B1 is then established using reversed-phase high-performance liquid chromatography coupled with fluorescence detection. The method is fully validated by using Certified Reference Materials. Limit of detection is found to be 0.5x10-3 mg/kg. The Bartlett test has shown that the method is affected by a systematic error and as a consequence the results must be corrected for the recovery. The precision is found in all cases lower than those calculated by Horwitz equation. Uncertainty estimation has been performed taking into account the bottom-up approach as stated in the Eurachem/Citac guide. With this method the uncertainty is calculated by the addition of variances for a measurand M when the equation for the calculation of M is based only on multiplications and divisions. The bottom-up approach is a tool which identifies the parameters or working steps with an overly contribution to the total uncertainty, thus offering the chance to improve them. The final uncertainty budget has revealed that the main contributions to global uncertainty are those due to the recovery and to the calibration function.
| All Time | Past 365 days | Past 30 Days | |
|---|---|---|---|
| Abstract Views | 166 | 69 | 10 |
| Full Text Views | 22 | 1 | 0 |
| PDF Views & Downloads | 13 | 2 | 0 |
