高效液相色谱-三重四极杆质谱联用法测定水体及土壤中6种抗生素

High performance liquid chromatography-triple quadrupole mass spectrometry for determination of 6 antibiotics in water and soil

本文研究建立了固相萃取-高效液相色谱-三重四极杆质谱联用法(HPLC-MS/MS)测定水体及土壤中喹诺酮类、大环内酯类、磺胺类和四环素类共6种抗生素的分析方法.水质及土壤样品经净化富集后,在HPLC-MS/MS多反应监测模式下进行定性及定量分析.研究表明,6种抗生素的加标回收率在55.1%-120.0%之间,相对标准偏差为0.928%-12.5%(n=6).水体的方法检出限为0.1-1.2 ng·L^(−1);土壤的方法检出限为0.17-2.4μg·kg^(−1).该方法灵敏度高,准确性强,适用于水体和土壤样品中痕量抗生素的定性定量分析.该方法应用于农田土壤和地下水的定量分析,部分抗生素有所检出,浓度范围为ND-12.6μg·kg^(−1)、ND-15.8 ng·L^(−1).

In this study,a determination method for six kinds of antibiotics,including quinolones,tetracyclines,macrolides and sulfonamides in water and soil was established using solid phase extraction(SPE)and high performance liquid chromatography-triple quadrupole mass spectrometry(HPLC-MS/MS).The water and soil samples were extracted and cleaned by HLB columns,and the qualitative and quantitative analysis were determined with multiple reaction monitoring(MRM).It was shown that the recoveries of the six antibiotics ranged from 55.1%to 120.0%with the relative standard deviations of 0.928%to 12.5%(n=6).The limit of detections in water and soil were 0.1—1.2 ng·L^(−1)and 0.17—2.4μg·kg^(−1),respectively.This method has high efficiency and high sensitivity,which can be used for the qualitative and quantitative analysis of trace antibiotics in soil and water samples.Antibiotics were detected in this method,and the concentrations ranged from not detected to 12.6μg·kg^(−1),not detected to 15.8 ng·L^(−1),respectively.