METHOD FOR THE ISOLATION AND LIQUID-CHROMATOGRAPHIC DETERMINATION OF 8 SULFONAMIDES IN MILK

A method for the isolation and liquid chromatographic determination of eight sulfonamides in milk is presented. Fortified or blank milk samples (0.5 ml) were blended with octadecylsilyl (C18T) derivatized silica (2 g). A column made from the sample C18T matrix was first washed with hexane (8 ml) following which the sulfonamides were eluted with methylene chloride (8 ml). The eluate contained sulfonamide analytes which were free from interferences when analyzed by high-performance liquid chromatography (HPLC) utilizing UV detection (270 nm, photodiode array). Standard curve correlation coefficients (range, 0.998 +- 0.002 to 0.999 +- 0.001), average perentage recoveries (73.1 +- 7.4 to 93.7 +- 2.7%), and the inter- (3.9-9.6%) and intra-assay (2.2-6.7%) variabilities, were determined for the concentration range examined (62.5-2000 ng/ml) and resulted in a minimal detectable limit of 1.25 ng on column (62.5 ng/ml, 20 μl injection from a final sample volume of 0.5 ml). Savings in terms of time and solvent make this procedure attractive when compared to classical isolation techniques for sulfonamides. © 1990.