Quantitation and confirmation of sulfamethazine residues in swine muscle and liver by LC and GC/MS.
The present paper describes a liquid chromatographic (LC) method for purification of crude swine tissue extracts before gas chromatographic/mass spectrometric (GC/MS) quantitation and confirmation of sulfamethazine at low ppb levels. Fractions corresponding to sulfamethazine were collected, evaporated to dryness, N-methylated with diazomethane, concentrated, and analyzed by GC/MS. A mass spectrometer was set to selected ion monitoring (SIM) mode. Ions 233, 227, 228, and 92 m/z were detected. Ratio 227/233 m/z (sulfamethazine/internal standard, [phenyl 13C6] sulfamethazine) was used for quantitation, while ratios 228/227 and 92/227 m/z, respectively, were used for confirmation. Quantitation in spiked blank muscle tissue was tested from 100 to 1 ppb and found acceptable at all concentrations studied; coefficients of variations ranged from 4.9 to 14.4%. Similar results were obtained for liver tissue from 5 to 20 ppb; coefficients of variation ranged from 1.2 to 9.1%.
Carignan
G
G
Health and Welfare Canada, Bureau of Drug Research, Ottawa, Ontario.
Carrier
K
K
D000818:Animals; D002853:Chromatography, Liquid; D004350:Drug Residues / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry; D007202:Indicators and Reagents; D008099:Liver / Q000737:chemistry; D008460:Meat / Q000032:analysis*; D009132:Muscles / Q000737:chemistry; D013418:Sulfamethazine / Q000032:analysis*; D013552:Swine
D007202:Indicators and Reagents; D013418:Sulfamethazine