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U.S. Department of Health and Human Services

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TITLE:  Confirmation of oxytetracycline, tetracycline and chlortetracycline residues in milk by particle beam liquid chromatography/mass spectrometry
AUTHORS:  Kijak PJ;Leadbetter MG;Thomas MH;Thompson EA;
YEAR:  1991
JOURNAL ABBREV:  Biol Mass Spectrom
JOURNAL FULL:  Biological mass spectrometry
ISSUE:  12
END PAGE:  795
KEYWORDS:  analysis;Animals;Chlortetracycline;Drug Residues;Food;Gas Chromatography-Mass Spectrometry;Maryland;Methanol;methods;Milk;Molecular Weight;Oxytetracycline;Research;Tetracycline;Tetracyclines;veterinary;Water;
ABSTRACT:  A method using particle beam liquid chromatography/mass spectrometry was developed for the confirmation of oxytetracycline, tetracycline and chlortetracycline residues in bovine milk. This method is one of the first to apply particle beam technology to the confirmation of animal drug residues in food products for regulatory purposes. The milk is centrifuged, using molecular weight cut-off filters to remove components of 25,000 daltons and above from the milk. The filtrate is passed through a C-18 sample preparation cartridge which retains the tetracyclines. After the columns are washed with water, the tetracyclines are eluted with 0.1 M oxalic acid in methanol and concentrated. The compounds are separated on a Novapak C-18 column with a methanol-oxalic acid-acetonitrile mobile phase. Negative chemical ionization with selective ion monitoring is used to identify the tetracyclines. The procedure was used to confirm the presence of each tetracycline at 100 ng ml-1 in fortified and incurred milk samples
AFFILIATIONS:  Food and Drug Administration, Division of Veterinary Medical Research, Beltsville, Maryland 20705