HPLC를 이용한 축,수산 식품 중 잔류 노보비오신의 분석

Abstract

A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in bovine, porcine, chicken, flatfish and japanese eel muscle has been developed and validated. The separation condition for HPLC/UV was optimized with phenyl hexyl (4.6.Ｘ150 mm, 5 μm) column with 10 mM monobasic sodium phosphate buffer (pH 2.5)/acetonitrile (50/50, v/v) as the mobile phase at a flow rate of 1.0 mL/min and detection wavelength was set at 254 nm. Residues were extracted from tissue by blending with methanol and lipid materials were removed with n-hexane. Then, the methanol extract was evaporated to dryness under a nitrogen stream, reconstituted in the mobile phase. Aliquot of the organic extract was decanted and filtered through 0.45 μm syringe filter. The 20 μL of the resulting solution was injected into the HPLC system. The calibration ranges were 0.5. 5 μg/g and calibration curves were linear with coefficients of correlation better than 0.95. The limits of quantification were 0.5 μg/g for all muscles. The recoveries of bovine, porcine, chicken, flatfish and japanes eel muscles were 99.8 %, 102.4 %, 91.0 %, 104.0 % and 93.0 %, respectively. The procedures were validated according to the CODEX guideline, determining specificity, linearity, accuracy, precision, quantitation limit and recovery.