Development and validation of a multi-residue and multiclass ultra-high-pressure liquid chromatography-tandem mass spectrometry screening of antibiotics in milk

Abstract

A multi-residue screening method for 33 antibiotics from five different families was employed to simultaneously determine sulphonamide, tetracycline, macrolide, quinolone and chloramphenicol antibiotics using ultra high pressure liquid chromatography tandem mass spectrometry. A simple sample preparation method was developed using protein precipitation, centrifugation and solid phase extraction and was optimised to achieve the best recovery for all compounds. The methodology was validated for quantitative screening methods, by evaluating the detection capability (CCβ), specificity, selectivity, precision, applicability and ruggedness. Precision, in terms of relative standard deviation, was under 21% for all compounds. Because CCβ was determined for screening purposes and, according to maximum residue limit, the limit of detection of the method was calculated and ranged from 0.010 μg kg−1 to 3.7 μg kg−1. This validation provided evidence that the method is suitable to be applied in routine analysis for the detection of antibiotics in bovine, caprine and ovine milk.