Rapid Determination of 19 Fluoroquinolones Antibiotic Residues in Soil by QuEChERS/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
  
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KeyWord:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  soil  fluoroquinolone antibiotics(FQs)  isotope labelled internal standards  matrix dispersive solid phase extraction
  
AuthorInstitution
CHEN Lei,WU Yun-qi,ZHAO Zhi-yong,ZHAO Xiao-yan,ZHOU Chang-yan 1.Institute for Agro-food Standards and Testing Technology,Shanghai Academy of Agricultural Sciences;2.Laboratory of Quality and Safety Risk Assessment for Agro-foodShanghai,China Ministry of Agriculture and Affairs;3.Food Science and Technology College,Henan Agricultural University
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Abstract:
      A method of ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) combined with internal standard method was developed for the simultaneous determination of 19 kinds of fluoroquinolones antibiotic(FQs) residues in soil based on QuEChERS(Quick,Easy,Cheap,Effective,Rugged,Safe) pre-treatment.Firstly,5.0 g of soil was blended with 100 μL 10 mg/L internal standard compounds,then the analyte was extracted with 20 mL 0.1 mol/L EDTA-McIlvaine buffer and acetonitrile(1∶1,by volume),cleaned-up with a matrix dispersive solid phase extraction material(150 mg anhydrous MgSO4,15 mg PSA,15 mg C18),finally detected by UPLC-MS/MS with electrospray ionization in positive ion scanning under multiple reaction monitoring mode.Under the optimized conditions,the limits of detection and quantitation of the method were in the ranges of 0.2-1.0 μg/kg and 1.0-5.0 μg/kg,respectively,with correlation coefficients(r2) of 0.992-0998. Recoveries for 19 FQs at three spiked levels of 10,50 and 200 μg/kg ranged from 65.2% to 104% with relative standard deviations(n=5) not more than 14%.The method was simple,rapid and accurate,and was suitable for the determination of fluoroquinolones antibiotic residues in soil.
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