Detection of residual bacitracin A, colistin A, and colistin B in milk and animal tissues by liquid chromatography tandem mass spectrometry

Eric Chun-hong Wan; Clare Ho; Della Wai-mei Sin; Yiu-chung Wong
May 2006
Analytical & Bioanalytical Chemistry;May2006, Vol. 385 Issue 1, p181
Academic Journal
Liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-MS/MS) was applied to the determination of residual bacitracin A, colistin A, and colistin B in milk and animal tissue samples. Prior to instrumental analysis, samples were subjected to acid extraction followed by solid-phase cleanup using Strata-X cartridges. Mass spectral acquisitions were performed under selective multiple reaction monitoring (MRM) mode at m/ z 199 and 670 from triply charged precursors of bacitracin A ( m/ z 475); m/ z 385 and 379 from triply charged precursors of colistin A ( m/ z 391); and m/ z 380 and 374 from triply charged precursors of colistin B ( m/ z 386). Method precision was evaluated from spike recovery of samples fortified at concentrations corresponding to 2/5 of the maximum residue limits (MRLs) for each of the analytes under study. Intra-day and inter-day variations were found to range from 90.9 to 104% with relative standard deviation (RSD) <6.5%, and from 90.1 to 106% with RSD <9.1%, respectively. Limits of quantification (LOQs) were defined as the spiking concentrations at 2/5 MRL, and limits of detection (LODs) were 10�47 �g kg-1 for bacitracin A, 1�16 �g kg-1 for colistin A, and 6�14 �g kg-1 for colistin B in milk and animal tissues. The presented method has good precision and high sensitivity and was applied as a fast screening protocol and a quantitative tool for monitoring of the concerned polypeptides in foods as part of a surveillance program. [Figure not available: see fulltext.]


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