基于分散固相萃取-超高效液相色谱串联质谱法测定沉积物中大环内酯类抗生素  

Determination of macrolide antibiotics in the sediment based on dispersed solid-phase extraction coupled with ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry

作　　者：李涛 王策 徐兆安 徐枫 LI Tao;WANG Ce;XU Zhaoan;XU Feng(Taihu Basin Hydrology&Water Resources Monitoring Center(Taihu Basin Environment Monitoring Center),Wuxi,214131,China;School of Energy and Environment,Southeast University,Nanjing,210096,China;Key Laboratory of Environmental Medicine Engineering,Southeast University,Nanjing,210096,China)

机构地区：[1]太湖流域水文水资源监测中心(太湖流域水环境监测中心),无锡214131 [2]东南大学能源与环境学院,南京210096 [3]东南大学环境医学工程教育部重点实验室,南京210096

出　　处：《环境化学》2022年第1期231-240,共10页Environmental Chemistry

基　　金：国家自然科学基金青年科学基金(41601509)资助.

摘　　要：采用分散固相萃取与超高效液相色谱串联质谱技术,建立了快速测定沉积物中9种大环内酯类抗生素(螺旋霉素、阿奇霉素、替米考星、竹桃霉素、红霉素、泰乐菌素、吉他霉素、罗红霉素和交沙霉素)的检测方法。沉积物经磷酸盐缓冲液和乙腈混合液浸提,再经过石墨化炭黑和C18硅胶分散固相萃取材料净化。采用超高效液相色谱串联质谱仪(UPLC-MS/MS)测定,以0.1%甲酸和乙腈为流动相,梯度洗脱,采用多反应监测(MRM)离子模式进行测定。结果表明,沉积物中9种大环内酯类回收率范围为67.6%—96.2%,相对标准偏差3.8%—13.6%(n=6),方法检出限介于0.005—0.01μg·kg^(-1)(R^(2)>0.995)。以太湖湖区典型沉积物样品作为验证,该方法满足实际样品的检测需求。A rapid determination method was established for 9 macrolide antibiotics(including Spiramycin,Azithromycin,Tilmicosin,Troleandomycin,Erythromycin,Tylosin,Kitasamycin,Roxithromycin and Josamycinin)in sediments using a dispersed solid-phase extraction method coupled with ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry(UPLC-MS/MS).The sediment samples were extracted by the mixture of phosphate buffer and acetonitrile,and then the resulting supernatant solution was purified by the dispersed solid extraction materials of GCB and C18.Finally,all the antibiotics concentrations were determined by UPLC-MS/MS under a multi-1monitoring mode(MRM),separated by a gradient elution with the mobile phase consisting of 0.1%formic acid and acetonitrile solutions.The results showed that the average recovery of the 9 macrolides in the sediments ranged from 67.6%to 96.2%,with the relative standard deviation was 3.8%—13.6%(n=6).The method detection limit(MDL)of the target compounds was in the range of 0.005—0.01μg·kg^(-1) in sediment(R^(2)>0.995).This established method has been validated by experimental analysis on sediment samples derived from typical sub-region of Taihu Lake.It demonstrated the feasibility of the method to detect the macrolide antibiotics in Taihu Lake.

关 键 词：大环内酯类抗生素 沉积物 分散式固相萃取 液相色谱串联质谱 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]