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Muscarella M, Lo Magro S, Palermo C, Centonze D.
Validation according to European
Commission Decision 2002/657/EC of a confirmatory method for
aflatoxin M1 in milk based on immunoaffinity columns and high
performance liquid chromatography with fluorescence detection.
Anal Chim Acta. 2007 Jul 2;594(2):257-64.
Istituto Zooprofilattico Sperimentale della Puglia e della
Basilicata, Foggia, via Manfredonia 20, 71100 Foggia, Italy.
A high performance liquid chromatographic method with
fluorimetric detection for the determination of aflatoxin M1
in milk has been optimized and validated according to Commission
Decision 2002/657/EC by using the conventional validation
approach. The procedure for determining selectivity, recovery,
precision, decision limit (CC(alpha)), detection capability
(CC(beta)) and ruggedness of the method has been reported. The
results of the validation process demonstrate the agreement of
the method with the provisions of Commission Regulation
401/2006/EC. The mean recovery calculated at three levels of
fortification (0.5, 1.0, and 1.5-fold the MRL) was 91% and the
maximum relative standard deviation value for the
within-laboratory reproducibility was 15%. Limit of detection
(LOD) and limit of quantitation (LOQ) values were 0.006 microg
kg(-1) and 0.015 microg kg(-1) while the CC(alpha) and CC(beta)
values were 0.058 microg kg(-1) and 0.065 microg kg(-1),
respectively. The relative expanded measurement uncertainty of
the method was 7%. The method was not affected by slight
variations of some critical factors (ruggedness minor changes)
as pre-treatment and clean-up of milk samples, thermal treatment
and different storage conditions, as well as by major changes
valued in terms of milk produced by different species (buffalo,
goat and sheep). The method allowed accurate confirmation
analyses of milk samples, resulted positive by the screening
method. In fact, the Z-score values attained in a proficiency
test round were well below the reference value of 1, proving the
excellent laboratory performances.
PMID: 17586123
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