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采用固相萃取/高效液相色谱/串联质谱法测定自然水体中的5种磺胺类抗生素。试验过程中比较了两种萃取柱(HLB和C18)的富集效果,并对水样的pH值、萃取柱的洗脱溶剂及水样体积进行了优化。优化后的方法如下:水样富集体积为200～500 mL,用稀硫酸酸化至pH值=3.0,用HLB小柱进行富集净化,95%甲醇洗脱,在0～200μg/L范围内5种磺胺的标准曲线线性关系良好(r≥0.999),该方法检测限<50 ng/L、精确度高(RSD<5%)、加标回收率为86.8%～97.3%。经过对实际河水水样的测试,证明适用于自然水体及给水系统中磺胺类抗生素的快速检测。
Determination of Five Sulfonamide Antibiotics in Natural Water by Solid Phase Extraction / High Performance Liquid Chromatography / Tandem Mass Spectrometry. During the experiment, the enrichment effects of two extraction columns (HLB and C18) were compared, and the pH value of the water sample, the elution solvent of the extraction column and the water sample volume were optimized. The optimized method was as follows: The volume of water sample was 200 ~ 500 mL, acidified with dilute sulfuric acid until pH = 3.0, concentrated and purified with HLB cartridge, eluting with 95% methanol, and in the range of 0 ~ 200μg / L The standard curve of the five sulfonamides was linear (r≥0.999). The limit of detection (RSD <5%) of this method was less than 50 ng / L and the recoveries were 86.8% -97.3%. After the actual river water test, proved to be suitable for natural water and water supply system in the rapid detection of sulfonamides.