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本研究建立了测定水中四种四环素类抗生素的超高效液相色谱(ultra-high performance liquid chromatography,UPLC)分析方法。采用固相萃取法提取水中的四环素类抗生素,分别以甲醇和水活化、平衡HLB小柱,用甲醇进行洗脱。在UPLC条件中采用甲醇、乙腈及0.01mol/L柠檬酸溶液作为流动相进行梯度洗脱,外标法定量,分析时间仅为4.5分钟。四种四环素类抗生素的线性关系良好,线性相关系数大于0.999。低中高三个浓度加标回收率分别为56.0%-86.3%,68.0%-78.5%,73.8%-80.4%。土霉素、四环素、金霉素和强力霉素的方法检出限分别为0.71,0.36,0.47,0.88μg/L,与HPLC-MS方法相当。该方法重现性较好,操作简单,分析时间短,可用于高通量水体样品中四环素类抗生素的测定。
This study established a method for the determination of four tetracycline antibiotics in water by ultra-high performance liquid chromatography (UPLC). The tetracycline antibiotics were extracted by solid-phase extraction and activated by methanol and water respectively. The HLB cartridges were equilibrated and eluted with methanol. In the UPLC conditions methanol, acetonitrile and 0.01mol / L citric acid solution as the mobile phase gradient elution, external standard method, the analysis time is only 4.5 minutes. The four tetracycline antibiotics had a good linear relationship with a linear correlation coefficient of greater than 0.999. The low, medium and high concentrations of the three spiked recoveries were 56.0% -86.3%, 68.0% -78.5%, 73.8% -80.4%. The detection limits of oxytetracycline, tetracycline, chlortetracycline and doxycycline were 0.71, 0.36, 0.47 and 0.88 μg / L, respectively, which were comparable with HPLC-MS method. The method has good reproducibility, simple operation and short analysis time, and can be used for the determination of tetracycline antibiotics in high-throughput water samples.