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TITLE:  Development and validation of a gas chromatography/mass spectrometry procedure for confirmation of para-toluenesulfonamide in edible fish fillet tissue
 
AUTHORS:  Idowu OR;Kijak PJ;Meinertz JR;Schmidt LJ;
 
YEAR:  2004
 
JOURNAL ABBREV:  J AOAC Int
 
MONTH:  Sep
 
TYPE:  JOUR
 
REFMAN INDEX:  179
 
JOURNAL FULL:  Journal of the AOAC International
 
VOLUME:  87
 
ISSUE:  5
 
START PAGE:  1098
 
END PAGE:  1108
 
KEYWORDS:  analogs & derivatives;analysis;Animals;Drug Residues;Fishes;Food;Gas Chromatography-Mass Spectrometry;Meat;Potassium;Sodium;Solid Phase Extraction;Sulfonamides;Toluene;veterinary;Veterinary Medicine;
 
ABSTRACT:  Chloramine-T is a disinfectant being developed as a treatment for bacterial gill disease in cultured fish. As part of the drug approval process, a method is required for the confirmation of chloramine-T residues in edible fish tissue. The marker residue that will be used to determine the depletion of chloramine-T residues from the edible tissue of treated fish is para-toluenesulfonamide (p-TSA), a metabolite of chloramine-T. The development and validation of a procedure for the confirmation of p-TSA is described. Homogenized fish tissue is dried by mixing with anhydrous sodium sulfate, and the mixture is extracted with methylene chloride. The extract is passed through a silica gel solid-phase extraction column, from which p-TSA is subsequently eluted with acetonitrile. The acetonitrile extract is evaporated, and the oily residue is dissolved in hexane. The hexane solution is shaken with fresh acetonitrile. The acetonitrile solution is evaporated and the residue is redissolved in dilute potassium hydroxide solution. The aqueous solution is extracted with methylene chloride to further remove more of the fat co-extractive. The aqueous solution is reacted with pentafluorobenzyl bromide in presence of tetrabutylammonium hydrogensulfate. The resulting di-(pentafluorobenzyl) derivative of p-TSA is analyzed by gas chromatography/mass spectrometry. This method permits the confirmation of p-TSA in edible fish tissue at 20 ppb
 
AFFILIATIONS:  U.S. Food and Drug Administration, Center for Veterinary Medicine, 8401 Muirkirk Rd, Laurel, MD 20708, USA. oidowu@cvm.fda.gov
 
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