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Determination of the Chloramphenicol residues in milk and milk products using LC/MS/MS

0.1 μg/L concentration (n=6x3) and it was < 9%. The interferences in the chromatogram from different milk samples were investigated and eliminated using an appropriate HPLC column with guard column and using appropriate product ions. The product ions used are listed in Table 2.

For the chromatographic separation, the deviation of the retention time between standard and samples were inside of 2.5%the average retention time of the standard was 2.54 minutes and 2.56 minutes for the milk samples. For the relative ion intesities of mass spectrometric detection the deviation of relative ion intensity in spiked milk samples vs. standard was lower than 10%

Conclusion

The presented method is able to detect and to quantify chloramphenicol residues in milk and milk products in the lower ppb concentration range. With the excellent sensitivity of the API 3000 system, the limit of decision (ccα) and the limit of detection (cc) were calculated to be 0.03 μg/L and 0.1 μg/L respectively. This method along with the proven reliability and stability of the API 3000 system provides for a dependable and consistent determination of CAP as demonstrated by the precision of the correlation coefficients (r2) at > 0.99 for the 4 calibration curves and the < 9% variability in the intra-day reproducibility calculations. Due to its high specificity, sensitivity, and stability this LC/MS/MS assay on the API 3000 system fulfills the criteria of the EU regulation 2002/657/EC.

References

1D. Arnold and A. Somogyi, J. AOAC 68 (1985) 984.

2G. Balizs and D. Arnold, Chromatographia, 27 (1989) 489.

3P. Frst, C. Krger, H.A. Meemken and W. Groebel: D. Lebensmittel Rundschau 84 (1988) 108.

4P.J. Kijak, J. AOAC 77 (1994) 34.

5A. Pfenning, S. Turni
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