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TITLE:  Procedure for detecting and confirming pentobarbital residues in dog food by gas chromatography/mass spectrometry
 
AUTHORS:  Adam LA;Reeves VB;
 
YEAR:  1998
 
JOURNAL ABBREV:  J AOAC Int
 
MONTH:  Mar
 
TYPE:  JOUR
 
REFMAN INDEX:  160
 
JOURNAL FULL:  Journal of AOAC International
 
VOLUME:  81
 
ISSUE:  2
 
START PAGE:  359
 
END PAGE:  367
 
KEYWORDS:  Alkylation;analysis;Animal Feed;Animals;Dogs;Drug Residues;Food;Gas Chromatography-Mass Spectrometry;Hypnotics and Sedatives;Meat;Methanol;Nitrogen;Pentobarbital;Reproducibility of Results;Solid Phase Extraction;Solutions;veterinary;Veterinary Medicine;
 
ABSTRACT:  The method described detects and confirms presence of pentobarbital residues in dry, extruded feeds at concentrations of 5-20 ppb. Dried feed is ground to a uniform powder and shaken overnight in methanol. A portion of the methanolic extract is evaporated, and the residue is reconstituted in phosphate-buffered saline. The aqueous extract is cleaned with a solid-phase extraction cartridge designed to extract barbiturate residues from biological matrixes. Dimethyl sulfoxide, tetramethylammonium hydroxide, and iodomethane are added to derivatize pentobarbital, 1,3-Dimethyl-pentobarbital is then acidified with dilute hydrochloric acid and extracted with isooctane. The organic layer is transferred and evaporated under a stream of nitrogen. The residue is reconstituted in a small volume of ethyl acetate for analysis by gas chromatography/mass spectrometry. The limit of detection is approximately 0.7 ppb. The method was validated with pentobarbital-fortified feed samples containing high concentrations of meat and bone meal
 
AFFILIATIONS:  U.S. Food and Drug Administration, Center for Veterinary Medicine, Laurel, MD 20708, USA
 
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