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目的:建立水产品中氯霉素、四环素、土霉素、金霉素残留的高效液相色谱法同时检测方法。方法:样品(有鳍鱼、虾、蟹、贝壳类)经5%高氯酸溶液沉淀蛋白质,以HPLC同时检测其中四种抗生素含量,色谱柱:ZORBAX SB-C18 4.6×250 mm 5μm,流动相:甲醇+乙腈+0.01 mol/L草酸溶液梯度洗脱,流速1.0 ml/min,检测波长270 nm。结果:本法四种抗生素的最低检出浓度均为0.01 mg/kg,在0.01 mg/kg～1 mg/kg范围内线性良好,加标回收率96.0%～102%,RSD<1.0%(n=6)。结论:该法具有准确、灵敏、简便等优点,适用于同时检测水产品中上述四种抗生素。
Objective: To establish a method for simultaneous determination of chloramphenicol, tetracycline, oxytetracycline and chlortetracycline in aquatic products by high performance liquid chromatography. Methods: Samples (finfish, shrimp, crab and shellfish) were precipitated by 5% perchloric acid solution and four antibiotics were detected by HPLC simultaneously. Column: ZORBAX SB-C18 4.6 × 250 mm 5μm, mobile phase : Methanol + acetonitrile +0.01 mol / L oxalic acid gradient elution, flow rate 1.0 ml / min, detection wavelength 270 nm. Results: The minimum detectable concentrations of the four antibiotics in this method were both 0.01 mg / kg. The linearity was good in the range of 0.01 mg / kg ~ 1 mg / kg. The recoveries were 96.0% -102% with RSD <1.0% = 6). Conclusion: The method is accurate, sensitive, simple and so on, suitable for simultaneous detection of the above four antibiotics in aquatic products.