Determination of fumagillin in muscle tissue of rainbow trout using automated ion-pairing liquid chromatography.
A high-performance liquid chromatographic assay is described as a routine analytical method for the determination of fumagillin in rainbow trout muscle tissue. Muscle tissue samples (1 g) containing fumagillin were deproteinized with 8 ml of an acetonitrile-water mixture (2:6, v/v). The extracts were purified with a Bond Elut Octyl C8 cartridge column, washed with a water-methanol mixture (95:5, v/v; 4 ml) and fumagillin was eluted with acetonitrile (1 ml). Analytical separations were performed by reversed-phase HPLC with UV detection at 351 nm under gradient conditions. The mobile phase was acetonitrile-0.005 M tetrabutyl ammonium phosphate in water (pH 7.8). The assay is specific and reproducible within the fumagillin range of 20-1000 ng/g and recovery at 20 ng/g was 69.2%. Sample preparation involves the use of a robotic sample preparation system. Gravimetric validation of all operations enabled Good Laboratory Practices to be observed.
Guyonnet
J
J
Sanofi Santé Nutrition Animale, Department of Pharmacokinetics and Drug Metabolism, Libourne, France.
Richard
M
M
Hellings
P
P
D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003510:Cyclohexanes; D005231:Fatty Acids, Unsaturated / Q000032:analysis*; D007477:Ions; D009132:Muscles / Q000737:chemistry*; D017686:Oncorhynchus mykiss; D015203:Reproducibility of Results; D012717:Sesquiterpenes; D013056:Spectrophotometry, Ultraviolet
D000900:Anti-Bacterial Agents; D003510:Cyclohexanes; D005231:Fatty Acids, Unsaturated; D007477:Ions; D012717:Sesquiterpenes; C026211:fumagillin