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A rapid confirmatory liquid chromatographic/tandem mass spectrometic method was developed for determination of chloramphenicol in bovine milk. Chloramphenicol was extracted directly from milk by solid-phase extraction on a C18 cartridge. The extract was further cleaned up on neutral aluminium oxide. Three transition products were monitored in negative ion mode after atmospheric pressure chemical ionization. The detection capability related to the transition product of lowest abundance was 0.03 μg/kg. The mean recovery was 90% at levels of 0.1–0.2 μg/kg. The relative repeatability standard deviations were 4.3, 3.8, and 2.8% at levels of 0.1, 0.2, and 1.0 μg/kg, respectively.

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