Determination of 4 Macrolide Antibiotics in Typical Waste Water and Activated Sludge Using HPLC-ESI-MS/MS
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KeyWord:HPLC-ESI-MS/MS  USE  SPE  macrolide antibiotics  waste water  activated sludge
雷晓宁,方小丹,鲁建江,陆紫皓,葛林科,张蓬,那广水 1.石河子大学化学化工学院,新疆兵团化工绿色过程重点实验室;2.国家海洋环境监测中心,国家海洋局近岸海域生态环境重点实验室
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      A reliable,sensitive and selective method was developed for the determination of 4 macrolide antibiotics(MLs) in typical waste water and activated sludge using high performance liquid chromatography-electrospray ionization tandem mass spectrometry(HPLC-ESI-MS/MS).The target antibiotics in water samples were enriched and cleaned up with HLB solid phase extraction cartridges,and then eluted with 6 mL methanol.The activated sludge sample was ultrasonically extracted with a mixture of acetonitrile-phosphate buffer.The eluate was collected and concentrated under a gentle stream of nitrogen gas.The target compounds were separated on a Waters Symmetry-C18 column with acetonitrile-10 mmol?L-1 ammonium acetate as mobile phase,and analyzed by HPLC-ESI-MS/MS under positive electrospray ionization and selected reaction monitoring mode.Good linearities of 4 MLs were achieved over the concentration range of 0.1-100 μg?L-1,with correlation coefficients above 0.99.The overall recoveries of 4 MLs in waste water and activated sludge matrices were in the ranges of 70.2% -90.6% and 75.6% -88.7%,respectively,with relative standard deviations(RSD,n=6) of 2.7%-7.8 %.The method detection limits of 4 MLs in water samples and activated sludge were in the ranges of 0.013-0.025 ng?L-1 and 0.09-0.22 ng?g-1,respectively.The developed method was applied in the analysis of the typical waste water and activated sludge in Shihezi,Xinjiang,and the results indicated that the target antibiotics were detected in all samples.