超声提取-超高效液相串联质谱分析沉积物中15种抗生素

在现有方法基础上对沉积物中磺胺类、喹诺酮类、大环内脂类和四环素类抗生素的提取、富集、净化以及仪器分析方法进行了优化。以EDTA-Mcllvaine缓冲溶液与乙腈(V:V,1:1)混合液作为提取液,利用超声波细胞破碎仪进行超声提取,串联强阴离子交换柱(SAX)和HLB固相萃取柱进行固相萃取(SPE),通过超高效液相/串联质谱(UPLC-MS/MS)测定沉积物中抗生素的含量。抗生素基质加标回收率在56.4%~110%,相对标准偏差为1.1%~24.3%,方法检出限0.0055~0.716 ng/g。本方法有效地提高了沉积物中抗生素的提取效率,并应用于实际样品的测定中。

Ultrasonic extraction-ultra performance liquid chromatography-tandem mass spectrometry for analysis of 15 antibiotics in sediment

The extraction,enrichment,purification and instrumental analysis of the sulfonamides,quinolones,macrolides and tetracyclines in sediments were optimized based on the previous study.The mixture of EDTAMcllvaine buffer solution and acetonitrile(ACN)(1:1)was used as the extraction solution for the ultrasonic extraction of target compounds by ultrasonic cell crusher.Subsequently,the strong anion exchange(SAX)cartridge and Waters Oasis HLB cartridge were tandem connected to purify the target antibiotics,the product was then detected by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Optimized results showed the recoveries of target antibiotics were 56.4%-110%,the relative standard deviations(RSDs)were 1.1%-24.3%,with the limits of detection(LODs)in the range of 0.0055-0.716 ng/g.The method can effectively improve the extraction efficiency of antibiotics in the sediment,and can be applied to real samples.