넙치(Paralichthys olivaceus) 혈청 및 근육에서 세프티오퍼 및 대사체 분석을 위한 HPLC-MS/MS 방법 개발 및 검증
HPLC–MS/MS Method Development and Validation for Ceftiofur and Metabolites in Serum and Muscle of Olive Flounder (Paralichthys olivaceus)
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An economical and reliable HPLC-MS/MS method was developed and validated for quantifying ceftiofur residues in olive flounder (Paralichthys olivaceus) serum and muscle. QuEChERS extraction was used for muscle (LOQ 5 ng/g), while SPE with derivatization was employed for serum, achieving superior sensitivity (LOQ 10 ng/g) compared to QuEChERS (100 ng/g). Both methods showed recovery rates >90%, RSD ≤10%, and detection limits 40-fold lower than the maximum residue limit (0.4 mg/kg). The optimized SPE method reduced reagent consumption by 85% while maintaining perfor- mance. This matrix-specific approach enables direct comparison with countries using desfuroylceftiofur as a sole residue marker, contributing to international standardization of aquatic product safety monitoring.
Abstract
An economical and reliable HPLC-MS/MS method was developed and validated for quantifying ceftiofur residues in olive flounder (Paralichthys olivaceus) serum and muscle. QuEChERS extraction was used for muscle (LOQ 5 ng/g), while SPE with derivatization was employed for serum, achieving superior sensitivity (LOQ 10 ng/g) compared to QuEChERS (100 ng/g). Both methods showed recovery rates >90%, RSD ≤10%, and detection limits 40-fold lower than the maximum residue limit (0.4 mg/kg). The optimized SPE method reduced reagent consumption by 85% while maintaining perfor- mance. This matrix-specific approach enables direct comparison with countries using desfuroylceftiofur as a sole residue marker, contributing to international standardization of aquatic product safety monitoring.