固相萃取-超高压液相色谱-串联质谱同时分析环境水样中四环素类和喹诺酮类抗生素

Simultaneous determination of tetracycline and quinolone antibiotics in environmental water samples using solid phase extraction-ultra pressure liquid chromatography coupled with tandem mass spectrometry

应用固相萃取及超高压液相色谱-质谱联用技术，建立了环境水样中4种四环素类和6种喹诺酮类抗生素的同时分析方法。样品经HLB固相萃取柱富集、净化后用甲醇洗脱，以超高压液相色谱-串联质谱仪多反应监测（MRM）离子模式定性、定量分析。以河水和海水为基质，卡巴氧为替代物进行回收率评价，4种四环素类抗生素在加标质量浓度分别为20．0ng／L和100．0ng／L时的回收率为94．0％～117．0％，相对标准偏差为2．0％～9．7％（n=4），方法的检出限均为20．0ng／L；6种喹诺酮类抗生素在加标质量浓度分别为5．0ng／L和20．0ng／L时的回收率为53．6％～93．9％，相对标准偏差为1．6％～8．1％（n=4），方法的检出限为0．4ng／L。结果表明，所建立的方法可成功地应用于近岸海域表层环境水样中目标抗生素残留的分析。

Using HLB cartridge for extraction and cleanup, a method for simultaneous determination of 4 tetracycline and 6 quinolone antibiotics in environmental water samples was developed by ultra pressure liquid chromatography coupled with tandem mass spectrometry. Using river water and sea water as matrices and carbadox as surrogate, the recoveries and relative standard deviations （RSD, n =4） were 94.0% - 117.0% and 2.0% -9.7% for 4 tetracyclines at 20.0 ng/L and 100.0 ng/L spiking levels and 63.5% -93.9% and 1.6% -8. 1% for 6 quinolones at 5.0 ng/L and 20.0 ng/L spiking levels, respectively. The detection limits were 20.0 ng/L for 4 tetracyclines and 0.4 ng/L for 6 quinolones. The method has been successfully applied to the survey of 10 target antibiotic residues in Jiulong River estuary, Fujian.