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TITLE:  Confirmation of gentamicin and neomycin in milk by weak cation-exchange extraction and electrospray ionization/ion trap tandem mass spectrometry
 
AUTHORS:  Heller DN;Clark SB;Righter HF;
 
YEAR:  2000
 
JOURNAL ABBREV:  J Mass Spectrom
 
MONTH:  Jan
 
TYPE:  JOUR
 
REFMAN INDEX:  19
 
JOURNAL FULL:  Journal of mass spectrometry : JMS
 
VOLUME:  35
 
ISSUE:  1
 
START PAGE:  39
 
END PAGE:  49
 
KEYWORDS:  Aminoglycosides;Animals;Anti-Bacterial Agents;Carbohydrate Sequence;Cattle;chemistry;Chromatography;Chromatography,Liquid;Food;Gentamicins;Ions;isolation & purification;Maryland;Mass Spectrometry;Methanol;methods;Milk;Molecular Sequence Data;Neomycin;Quality Control;Reproducibility of Results;Sodium;Solid Phase Extraction;standards;Tandem Mass Spectrometry;veterinary;Veterinary Medicine;
 
ABSTRACT:  A new procedure for the confirmation of two aminoglycoside antibiotics in milk was developed and validated. This work is among the early applications of ion trap mass spectrometry for regulatory methodology, and it incorporates a novel weak cation-exchange extraction. The procedure was validated for the confirmation of both gentamicin and neomycin at 30 ng ml(-1) and above. Milk is first treated with acid and centrifuged. The supernate, excluding the fat layer, is buffered with sodium citrate to neutral pH. The extract is applied to a weak cation-exchange solid-phase extraction column. Aminoglycosides are eluted with acidified methanol. Following separation by ion-pair liquid chromatography, analytes are ionized with an electrospray interface. Protonated molecular ions are selectively stored in an ion trap mass spectrometer, then collisionally dissociated to yield unique product ion spectra. Confirmation is based on matching spectral responses between samples and comparison standards consisting of a bona fide standard spiked into control extracts. Method performance was demonstrated with replicate samples of control milk, fortified milk, and milk containing incurred residues of each compound
 
AFFILIATIONS:  US Food and Drug Administration, Center for Veterinary Medicine, 8401 Muirkirk Road, Laurel, Maryland 20708, USA. dheller@cvm.fda.gov
 
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