浙江省主要畜禽产区养殖废水中抗生素残留研究

结合固相萃取、高效液相色谱—串联质谱分析,建立了适合畜禽养殖废水中磺胺类、氟喹诺酮类、四环素类、氯霉素类等共29种抗生素残留的测定方法,废水样品经盐酸调节pH 6.0、离心后经HLB固相萃取柱净化,液相色谱—串联质谱正离子模式测定磺胺类、氟喹诺酮类、四环素类,负离子模式测定氯霉素类。空白地表水中磺胺类和氟喹诺酮类添加浓度为0.02～1.0μg.L-1,四环素类和氯霉素类添加浓度为0.04～1.0μg.L-1,回收率范围为68.6%～95.0%(n=5),相对标准偏差(RSDs)为2.8%～12.3%,方法的定量限(LOQ)为0.02～0.04μg.L-1。利用该方法对养殖废水、养殖场附近河域20个水样进行测定,检出5种磺胺类化合物和氟苯尼考。

Antibiotic residues in waste waters from main livestock farms in Zhejiang Province

Analytical methods for the determination of 29 antibiotic residues including sufonamides,tetracyclines,chloramphenicals and fluoroquinolones in waste waters were developed.Samples were adjusted into pH=6,centrifugated and cleaned-up through solid phase extraction column.HPLC-MS/MS with electrospray was used to determine sufonamides,tetracyclines,fluoroquinolones in positive ion scan mode and chloramphenicals in negative scan mode.The fortified recoveries of antibiotic residues in surface water were 68.6%-91.5% at fortification levels ranging from 0.02-1.0 μg·L-1 for sufonamides and fluoroquinolones and 0.04-1.0 μg·L-1 for tetracyclines and chloramphenicals.Relative standard deviations(RSDs) were 2.8%-12.3%(n=5).The limit of quantization(LOQ)were 0.02-0.04 μg·L-1.The method was applied to determine residues in 20 waste water samples from livestock and poultry farms or rivers near farms.As a result,five kinds of sufonamides and florfenicol were detected.