P41: HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF SULFONAMIDES RESIDUES IN MILK SAMPLES

摘要

In this study, a highly selective molecular imprinted polymer (MIP) sorbent was used for the determination of six sulfonamides (sulfanilamide, sulfacetamide, sulfadiazine, sulfathiazole, sulfamerazine and sulfamethizole) from milk samples. MIPs particles were applied as sorbent in the solid phase microextraction (MIPSPE). The determination was achieved by an accurate and sensitive liquid chromatographic analytical method which was developed and validated according tothe European Union Decision 2002/657/EC. Several experimental parameters such as the amount of the MIP and milk, the amount and the type of the elution solvent, as well as time of absorption and extraction were investigated for the achieving optimal conditions. The study of validation is based on the investigation of the following parameters, linearity, selectivity, stability, limits of detection and quantitation, decision limit, detection capability, trueness, precision and ruggedness according to the Youden's approach. The decision limit (CCa) and the results for detection capability (CCb) in the milk were achieved from 101.9 to 113.5 μg kg~(-1) and from 114.4 to 135.4μg kg~(-1) respectively. The optimized protocol was successfully applied to milk samples from local markets as well as to breast milk sample.