水体中磺胺、四环素、喹诺酮类抗生素检测方法

摘要

建立了固相萃取-高效液相色谱-串联质谱法(SPE-HPLC-MS/MS)同时检测水体中3类15种抗生素的分析方法.水样用Oasis HLB固相萃取小柱净化富集.通过对比水样在不同pH条件下的回收率,优化了环境水样中抗生素固相萃取过程中的前处理条件.采用甲醇和0.1％甲酸溶液作为流动相,经过梯度洗脱进行分离,在HPLC-MS/MS多反应监测模式下进行定性定量分析.结果表明,环境水体中15种抗生素的检出限和定量下限分别为0.12～1.6 ng/L和0.2 ～3.0 ng/L,自来水加标回收率为34.9％ ～ 102.5％ (pH =4).用该方法对海河流域13个地表水水样进行了初步检测,结果表明,部分抗生素普遍存在于地表水体中.其中,磺胺甲基异噁唑检出频率最高,在13个地表水样品中均有检出.%A method for the determination of 15 antibiotics in surface water was developed by using solid-phase extraction and liquid chromatography-electrospray ionization tandem mass spectrometry (SPE-HPLC-MS/MS).Water samples were enriched and cleaned-up by HLB solid-phase extraction cartridges.All antibiotics were separated by gradient elution with the mobile phase of methanol and 0.1％ formic acid (V/V).The eluate was then analyzed by HPLC-MS/MS in positive electrospray ionization and multiple reaction monitoring (MRM) mode.The result showed that the limits of qualitification and quantification were 0.12-1.6 ng/L and 0.2-3.0 ng/L respectively.The recoveries of 15 sulfonamide antibiotics in tap water were 34.9％-102.5％.The developed method was applied to analyze 13 surface water samples in Haihe basin.The results showed that some antibiotics were detected in some surface water samples.