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

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(R²>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。

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

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(R²>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.