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Issue 5, 2005
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Determination of nifursol metabolites in poultry muscle and liver tissue. Development and validation of a confirmatory method

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Abstract

A method is described for the identification and quantitative determination of 3,5-dinitrosalicylic acid hydrazide (DSH), the marker residue of nifursol metabolites in poultry (turkey, broiler) muscle and liver tissue. The method is based on the acid-catalysed hydrolysis of tissue-bound metabolites to free DSH and in situ derivatisation with 2-nitrobenzaldehyde to the corresponding nitrophenyl derivative NPDSH. A structural analogue of DSH, 4-hydroxy-3,5-dinitrobenzoic acid hydrazide (HBH) was synthesised to serve as an internal standard. The analytes were isolated from the matrix by liquid–liquid extraction with ethyl acetate. Determination was performed by LC-MS/MS with negative electrospray ionisation. The [M − H]+ ions of NPDSH and NPHBH at m/z 374 were fragmented by collision induced dissociation (CID) producing transition ions at m/z 182, 183 and 226. The transition ions at m/z 182 and 226 were selected for monitoring of NPDSH while the transition ion at m/z 183 was selected for NPHBH. The method has been validated according to the EU criteria of Commission Decision 2002/657/EC at 0.5, 1.0 and 1.5 µg kg−1 in muscle and liver tissue. A decision limit (CCα) was obtained of 0.04 and 0.025 µg kg−1 in muscle and liver, respectively. Similarly a detection capability (CCβ) was obtained of 0.10 and 0.05 µg kg−1 in muscle and liver, respectively. The introduction of HBH as an internal standard did not lead to a significant improvement of the quantitative performance of the method. In fact for liver better performance characteristics were obtained when the IS was not taken into account. Nevertheless, as a qualitative marker for recovery, HBH could still be very useful in the analysis of unknown samples.

Graphical abstract: Determination of nifursol metabolites in poultry muscle and liver tissue. Development and validation of a confirmatory method

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Article information


Submitted
16 Sep 2004
Accepted
25 Feb 2005
First published
21 Mar 2005

Analyst, 2005,130, 763-771
Article type
Paper

Determination of nifursol metabolites in poultry muscle and liver tissue. Development and validation of a confirmatory method

P. P. J. Mulder, T. Zuidema, N. G. M. Keestra, P. J. F. Kooij, I. J. W. Elbers and J. A. van Rhijn, Analyst, 2005, 130, 763
DOI: 10.1039/B414320E

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