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U.S. Department of Health and Human Services

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TITLE:  Confirmation of Chloramphenicol Residues in Bovine-Milk by Gas-Chromatography Mass-Spectrometry
 
AUTHORS:  Kijak PJ;
 
YEAR:  1994
 
JOURNAL ABBREV:  J AOAC Int
 
MONTH:  Jan
 
TYPE:  JOUR
 
REFMAN INDEX:  540
 
JOURNAL FULL:  Journal of AOAC International
 
VOLUME:  77
 
ISSUE:  1
 
START PAGE:  34
 
END PAGE:  40
 
KEYWORDS:  BOVINE-MILK;Chloramphenicol;confirmation;Ions;Mass Spectrometry;Meat;Methanol;Milk;Solid Phase Extraction;standards;TISSUES;Water;
 
ABSTRACT:  A gas chromatographic/mass spectrometric method was developed to confirm the presence of chloramphenicol (CAP) at 0.5 ng/mL in bovine milk meta-Nitrochloramphenicol (20 ng) is added to 10 mL milk as a surrogate standard. The milk is mixed with ethyl acetate and then loaded onto a diatomaceous earth-filled, solid-phase extraction (SPE) column; CAP is eluted with additional ethyl acetate. A solution of 4% NaCl in water is added to the eluant, and ethyl acetate is removed by evaporation under a flow of N-2. The sample is defatted with hexane and then loaded onto a C-18-SPE column. The column is washed with water, and CAP is eluted with methanol. The methanol is evaporated under a flow of Na, and the trimethylsilyl derivative is prepared with Sylon HTP (hexamethyldisilazane-trimethylchlorosilane-pyridine, 3 + 1 + 9). The excess reagent is evaporated under N-2, and the residue is taken up in cyclohexane-hexane (60 + 40). CAP is separated on a 30 m x 0.25 mm id methytsilicone column having a film thickness of 0.25 mu m and analyzed by methane negative chemical ionization with selected ion monitoring. The ions with m/z 304, 322, 358, 360, 466, and 468 are monitored. Confirmation is based on the presence of 5 ions with relative ion abundances within 10% of that obtained by using standards
 
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