کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
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1216898 | 1494174 | 2008 | 5 صفحه PDF | دانلود رایگان |

An LC–ESI–MS–MS method for the analysis of metabolites of four nitrofurans (furazolidone, furaltadone, nitrofurazone and nitrofurantoin) in raw milk has been developed. The samples were achieved by hydrolysis of the protein-bound drug metabolites, derivatization with 2-nitrobenzaldehyd (2-NBA) and clean-up extraction liquid–liquid with ethyl acetate. LC separation was achieved by using a Phenomenex Luna C-18 column. The mass spectrometer operated in multiple reaction monitoring mode (MRM) with positive electro-spray interface (ESI). The method validation was done according to the criteria laid down in Commission Decision No. 2002/657 EC. The validation includes the determination of linearity, repeatability, within-laboratory reproducibility, accuracy, decision limit (CCα) and detection capability (CCβ). The calibration curves were linear, with typical (R2) values higher than 0.991. The coefficient of variation (CV, %) was lower than 9.3% and the accuracy (RE, %) ranged from −9.0% to 7.0%. CV within-laboratory reproducibility was lower than 13%. The limits of decision (CCα) and detection capability (CCβ) were 0.12–0.29 μg/kg and 0.15–0.37 μg/kg, thus below the minimum required performance limit (MRPL) set at 1 μg/kg by the UE. This validated method was successfully applied for the determination of nitrofuran metabolites in a large number of milk samples.
Journal: Journal of Chromatography B - Volume 864, Issues 1–2, 15 March 2008, Pages 156–160