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A simple and reliable method using liquid chromatographyῌelectrospray ionizationῌmass spectrometry (LC/ESI-MS) has been developed for the determination of the macrolide antibiotics spiramycin and tilmicosin in meat and fish. The drugs were extracted from meat and fish with 0.2 metaphosphoric acidῌmethanol (6 : 4), and the extracts were cleaned up on an Oasis HLB cartridge (60 mg). Positive ionization produced the molecular related ions, (Mΐ2H) 2ῌ , at m/z 350.2, 422.3 and 435.3 for neospiramycin I, spiramycin I and tilmicosin, respectively. The LC separation was performed on a Capcell Pak MG-C18 column (1502 mm

or (M H). The recoveries of the drugs from milk fortified at a level 0.1 µg/g were 63.8 95.9 with high precision. The limits of detection of the drugs in milk were 0.01 µg/g.