Confirmatory assay for the simultaneous detection of penicillins and cephalosporins in milk using liquid chromatography/tandem mass spectrometry.
A high-performance liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the detection of residues of penicillins and cephalosporins in milk has been developed. After a simple extraction with acetonitrile, the extract was directly injected into the LC/MS/MS system on a C(18) column. A gradient consisting of acetonitrile and water, each containing 0.1% formic acid, was applied. The abundant parent ions [M + H](+) produced by positive electrospray ionisation were selected for fragmentation with argon. For each compound at least one fragment was recorded with multiple reaction monitoring. The limits of detection ranged from 1.5 to 25 microg/kg and the limits of quantification ranged from 4 to 50 microg/kg. Recoveries were examined at three levels (MRL, 0.5 x MRL, 2 x MRL) and ranged from 57 to 88%. The coefficients of variation obtained for the repeatability experiments were in agreement with those specified by the Horwitz equation. Linearity was checked by injecting extracts of samples spiked with increasing amounts of the different standards ranging from 0 to 150 microg/kg. The advantage of this method over existing methods is the very simple sample pre-treatment which makes the method very suitable for routine analysis.
Ministry of Small Enterprises, Traders and Agriculture, Agricultural Research Centre-Ghent, Animal Product Quality and Transformation Technology, Brusselsesteenweg 370, 9090 Melle, Belgium. e.daeseleire@clo.fgov.be
E
E
Daeseleire
H
H
De Ruyck
R
R
Van Renterghem
D000818:Animals; D002511:Cephalosporins / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D008892:Milk / Q000737:chemistry*; D010406:Penicillins / Q000032:analysis*; D015203:Reproducibility of Results
D002511:Cephalosporins; D007202:Indicators and Reagents; D010406:Penicillins