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.
出处
《中国环境监测》
CAS
CSCD
北大核心
2013年第4期111-115,共5页
Environmental Monitoring in China
基金
国家国际科技合作专项(2013DFA71340)
水利部公益性行业科研专项(201101018)
