Screening and Detection of Antibiotics in Fish Pond Water by Ultra Performance Liquid Chromatography-Mass Spectrometry with Solid Phase Extraction

KeyWord:ultra performance liquid chromatography-mass spectrometry  solid-phase extraction  antibiotics  fish pond water  fast screening

Abstract:

      A method was established for the rapid detection of 15 kinds of antibiotics(quinolones,chloramphenicol,tetracycline and sulfonamides) in river water near fish farms by ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry(UPLC-MS/MS) with solid-phase extraction.After filtration,a 500 mL of water sample was adjusted to pH 4.0 with hydrochloric acid,then added 0.5 g ethylenediaminetetraacetic acid disodium(Na2EDTA) to removal the interference of variousmetal ions,and finally enriched with an HLB solid-phase extraction column.The sample was detected by ultra performance liquid chromatography couple with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF MS),and screened for the antibiotics with antibiotic library.The corfirmation and quantitation of antibiotics in the sample were performed by UPLC-MS/MS in multi-period multi-reaction monitoring ion mode(MRM) with external standard method.The spiked recoveries for 15 antibiotics in blank matrix were in the range of 61.0%-98.4% with the relative standard deviations(n=3) of 4.6%-14.0%.The calibration curves of 15 antibiotics showed good linearity with the correlation coefficients not less than 0.990.The method detection limits(MDLs) ranged from 0.01 ng/L to 0.3 ng/L.With high sensitivity and good repeatability,this method could be applied in the detection of antibiotics in fish pond water in Beijing.