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 residue in salmon muscle and skin tissues by ion-pair reversed-phase liquid chromatography (LC) with electrochemical detection at +0.9 V. Lincomycin was extracted from tissues by homogenizing with 0.01 M KH2PO4 buffer (pH 4.5) and centrifuging the mixture. Water-soluble proteins were precipitated by adding sodium tungstate and sulfuric acid and removed by centrifugation. The buffer extract was then passed through a C18 solid-phase extraction cartridge. Lincomycin was eluted with 50% acetonitrile in water, and the eluate containing lincomycin was extracted with ethyl acetate. After the solvent had evaporated, the residue was redissolved 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 salmon 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 > or = 85% for salmon muscle and > or = 80% for salmon skin.
Luo
W
W
US Food Drug Administration, National Center for Toxicological Research, Division of Chemistry, Jefferson, AR 72079-9502, USA.
Hansen
E B
EB
Ang
C Y
CY
Thompson
H C
HC
D000097:Acetonitriles / Q000737:chemistry; D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis / Q000378:metabolism*; D002021:Buffers; D002851:Chromatography, High Pressure Liquid; D004350:Drug Residues / Q000032:analysis* / Q000378:metabolism; D004563:Electrochemistry; D008034:Lincomycin / Q000032:analysis* / Q000378:metabolism; D009132:Muscles / Q000378:metabolism*; D012474:Salmon / Q000378:metabolism*; D012867:Skin / Q000378:metabolism*; D014018:Tissue Distribution; D014867:Water / Q000737:chemistry
D000097:Acetonitriles; D000900:Anti-Bacterial Agents; D002021:Buffers; D014867:Water; D008034:Lincomycin; C032159:acetonitrile