固相萃取-超高效液相色谱法测定水中四环素类抗生素

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。

Determination of 4 Tetracycline Antibiotics in Water by. SPE-UPLC

The determination of 4 tetracycline antibiotics in water by UPLC was investigated in this study. Solid phase extraction was carried out to concentrate and purify the water samples. HLB cartridge was conditioned with methanol and then equilibrated with water. The analytes were finally eluted by methanol. Methanol, acetonitrile, and citric acid solution （0.01 mol/L） were applied in gradient elution in UPLC method. Total running time was only 4.5 minutes. The standard curve of each compound presented a good linearity （r2 〉 0.999）. The recoveries of three spiked levels of samples were 56.0%-86.3% （Low）, 68.0%- 78.5% （Middle）, 73.8%-80.4% （High）, respectively. The method detection limits （MDLs） were 0.71, 0.36, 0.47, 0.88 μg/L for oxytetracycline, tetracycline, chlortetracycline and doxycycline, respectively. The method is simple, quick, and reproductive and is suitable for high-throughput analysis of tetracycline antibiotics in water samples.