高效液相色谱法同时测定畜禽废水中4种四环素类抗生素

Determination of Four Tetracycline Antibiotics in Swine Waste Water Using High-Performance Liquid Chromatography

目的利用高效液相色谱-二极管阵列检测器,建立同时检测畜禽废水中土霉素、四环素、金霉素、强力霉素的方法。方法选用Waters SunF ire C18色谱柱(250 mm×4.6 mm,5μm),乙腈-0.5%三氟乙酸(TFA)水溶液为流动相梯度洗脱,流速1.2ml/min,检测波长360nm,高效液相色谱仪测定。结果土霉素、四环素、金霉素和强力霉素4种抗生素质量浓度为0.1μg/ml^15.0μg/ml时有良好的线性关系,4种抗生素的检出限均为50ng/ml,方法回收率在83.82%~108.70%之间。结论高效液相色谱法方便、快速、准确,且重现性好,能够用于畜禽废水中四环素类抗生素的检测。

Objective To establish a method for determination of four tetracycline antibiotics in swine waste water by HPLC. Methods After filtration and acid-digestion, 20 μl samples were injected into an HPLC system. Acetonitrile and 0.5% TFA solution were applied in gradient elution using HPLC method. The total running time was 15 minutes. Results The standard curve of four compounds presented a good linearity（ R2 〉0.999） in the range of 0.1 to 15.0 μg/ml. The detection limits were 50 ng/ml. The recovery ranged from 83.82% to 108.70% with the relative standard deviation less than 9.30%. Conclusion The proposed method presents many advantages, such as quick speed, user-friendliness and reproducibility.