超高效液相色谱-串联质谱法同时测定环境水样中的15种抗生素

Simultaneous determination of 15 antibiotics in environmental water samples by ultra performance liquid chromatography- tandem mass spectrometry

采用固相萃取/超高效液相色谱-串联质谱法,建立了水样中磺胺类、四环素类、氟喹诺酮类、大环内酯类和氯霉素类15种抗生素的同时测定方法.水样经HLB固相萃取柱富集,ACQUITY UPLC BEH C18色谱柱分离,以乙腈和5 mmol·L-1乙酸铵溶液(含0.1%甲酸)为流动相梯度洗脱,电喷雾离子源-串联质谱多反应监测模式检测.结果表明,同时测定15种抗生素的线性范围为5—100μg·L-1(相关系数均大于0.997),检出限为2.1—22.0 ng·L-1,定量限为6.9—71.8 ng·L-1;空白水样在加标水平为5、10、20μg·L-1时,抗生素的回收率为50.1%—109.0%,相对标准偏差为0.4%—8.5%(n=7).用本文建立的方法检测某农业小流域环境水样,发现5类抗生素可被不同程度检出,浓度范围为0.1—106.2 ng·L-1.

A simultaneous determination method for 15 antibiotics including sulfonamides,tetracyclines,quinolones,macrolides and chloramphenicols in water samples was developed by ultra performance liquid chromatography-tandem mass spectrometry with solid-phase extraction.The antibiotics in water samples were enriched by HLB solid-phase extraction column,and separated by ACQUITY UPLC BEH C18 column and eluted by acetonitrile and 5 mmol·L-1 ammonium acetate solution containing 0.1%formic acid as the mobile phases with gradient elution,and then determined by electrospray ion source-tandem mass spectrometry with multi-reaction monitoring mode.The results showed that the linear ranges were 5—100μg·L-1(R≥0.997)with the detection limits of 2.1—22.0 ng·L-1 and the limits of quantification of 6.9—71.8 ng·L-1 for the simultaneous determination of 15 antibiotics.The recoveries of blank water sample spiked with 5,10 and 20μg·L-1 antibiotic standards were in the range of 50.1%—109.0%(0.4%≤RSDs≤8.5%,n=7).The five kinds of antibiotics in environmental water samples of an agricultural watershed could be detected with the range of 0.1—106.2 ng·L-1 by using the developed method in this study.