A new ECD [electron capture detector] gas chromatographic determination of kanamycin in beef

A new ECD gas chromatographic determination method for kanamycin (KM) is proposed. KM in beef was extracted with 10% trichloroacetic acid, and the extract was washed with ether twice before being absorbed on an Amberlite CG-50 (H form) resin column and eluted with 0.1N hydrochloric acid. The eluate was concentrated to dryness and dissolved in methyl alcohol-water (1:1) mixture to prepare a test solution. A portion of the test solution was dried, and N-acylation of KM in the residue was carried out with heptafluorobutylyl-imidazole, followed by trimethylsilylation with trimethylsilylimidazole. The resulting derivative was determined by ECD-gas chromatography on a glass column (1.5m×3mm id) packed with 4% OV-101 coated onto Gaschrom Q. A linear calibration curve was obtained in the range from 0.05 to 1.0μg of KM. Recoveries of KM added to beef at levels of 0.2, 0.5 and 1.0ppm were 74%, 86% and 83%, respectively. The limit of detection was 0.1μg/g.