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  • Title: Surveillance study of novobiocin and phenylbutazone residues in raw bovine milk using liquid chromatography-tandem mass spectrometry.
    Author: Thompson TS, Noot DK, Kendall JD.
    Journal: Food Addit Contam Part A Chem Anal Control Expo Risk Assess; 2010 Aug; 27(8):1104-11. PubMed ID: 20496252.
    Abstract:
    A simple method permitting the simultaneous determination of trace residues of novobiocin and phenylbutazone in raw milk samples using liquid chromatography-tandem mass spectrometry was developed. Raw milk samples were mixed with acetonitrile to facilitate the concurrent precipitation of milk proteins and extraction of both veterinary drugs. Without additional clean-up or concentration of the resulting extract, the analytes could be quantified at concentrations as low as 0.0025 and 0.001 microg ml(-1) for phenylbutazone and novobiocin, respectively. The analysis of a series of fortified raw milk samples at analyte concentrations ranging from 0.005 to 0.1 microg ml(-1) and from 0.01 to 0.2 microg ml(-1) for phenylbutazone and novobiocin, respectively, yielded average recoveries ranging from 89.2% to 104.3% with standard deviations below 7%. The analytical method was applied to the analysis of raw milk samples collected from transport trucks upon delivery at dairy-processing plants throughout Alberta, Canada. Novobiocin was detected in 13 of 1072 samples tested at concentrations ranging from 0.001 to 0.007 microg ml(-1). Phenylbutazone was not detected in any of the samples tested.
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