DETERMINATION OF LINCOMYCIN RESIDUE IN SALMON TISSUES BY ION-PAIR REVERSED-PHASE LIQUID-CHROMATOGRAPHY WITH ELECTROCHEMICAL DETECTION

A method is described for detecting and quantitating lincomycin residu e in salmon muscle and skin tissues by ion-pair reversed-phase liquid chromatography (LC) with electrochemical detection at +0.9 V. Lincomyc in was extracted from tissues by homogenizing with 0.01M KH2PO4 buffer (pH 4.5) and centrifuging the mixture. Water-soluble proteins were pr ecipitated by adding sodium tungstate and sulfuric acid and removed by centrifugation, The buffer extract was then passed through a C-18 sol id-phase extraction cartridge, Lincomycin was eluted with 50% acetonit rile in water, and the eluate containing lincomycin was extracted with ethyl acetate, After the solvent had evaporated, the residue was redi ssolved in mobile phase and analyzed by LC, The method had a limit of detection of 7 ng/g lincomycin for salmon muscle and 12 ng/g for salmo n skin, The limit of quantitation was 17 ng/g for salmon muscle and 24 ng/g for salmon skin, Average recoveries of lincomycin spiked at 50, 100, and 200 ng/g were greater than or equal to 85% for salmon muscle and greater than or equal to 80% for salmon skin.