在线固相萃取-超高效液相色谱-三重四极杆质谱快速测定地表水中磺胺类抗生素

Rapid and Ultra-trace Levels Analysis of Sulfonamide Antibiotics in Surface Water by On-line Solid Phase Extraction with Ultra-performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry

建立了在线固相萃取-超高效液相色谱-三重四极杆质谱联用技术测定地表水中痕量磺胺类抗生素的方法。样品经滤膜过滤,HLB在线固相萃取小柱富集纯化,以Acquity BEH 130为分析柱,三重四极杆质谱进行检测,外标法定量。通过在线固相萃取,并对色谱和质谱等条件进行优化,该方法检出限为0.2~1.1 ng/L,回收率为80.6%~113%,相对标准偏差<10.6%,浓度范围内线性良好(r>0.9972),满足了磺胺类抗生素痕量分析测试的要求,且分析时间仅需17 min。该方法灵敏度高、分析速度快,对于保障水环境安全,及时提供污染信息,有效应对环境应急突发事件具有十分重要的意义。

A method for determining the ultra-trace level of sulfonamide antibiotics in surface water was developed based on on-line solid phase extraction-ultra performance liquid chromatography-triple quadrupole mass spectrometry(On line SPE-UPLC-MS/MS).The water sample was directly injected into on-line SPE after filtered by filter membrane.The HLB column was used for enriching and purifying.The analytes were separated by Acquity BEH 130 column,detected using tandem mass spectrometry,and quantified by external standard method.By optimizing SPE,chromatography and mass spectrometry condition,the method detection limits come out to be in the range of 0.2~1.1 ng/L,the recoveries ranged from 80.6%to 113%,and the relative standard deviations were less than 10.6%,and good linearities were obtained within investigated mass concentration ranges(r>0.9972),which were deemed satisfactory.The process takes just 17 min for determination.The method is sensitivity,fast and high efficiency,which is suitable for the determination of sulfonamide antibiotics in surface water.It is important to ensure the safety of water environment,to provide timely pollution information,and to effectively respond to environmental emergencies.