OPTIMIZATION OF THE ANALYTICAL PERFORMANCE OF THE MAGNETIC-SECTOR MASS-SPECTROMETER FOR THE IDENTIFICATION OF RESIDUAL CHLORAMPHENICOL IN SHRIMP

Chemical noise limits mass spectrometric detection of chloramphenicol (CAP) with electron capture ionization at low resolution, and makes CAP identification at concentrations of 5 parts per billion (ppb) difficult. Increasing the resolution from 1000 to 3500, however, was sufficient to separate the analyte signals from the noise signals, and resulted in a 100 times higher analytical sensitivity. The introduction of sweep gas in the ion source decreased the scattering of the quantitative results on average by a factor of 7, and thereby improved the precision of the analyses to an acceptable level (CV < 10%). Under such conditions, CAP residues of 1.5 and 2.1 ppb in shrimp as determined by electron capture gas chromatography/mass spectrometry can readily be identified by monitoring four diagnostic ions.