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Simultaneous Determination of Six Fluoroquinolones in Chicken Manures by High Performance Liquid Chromatography with Fluorescence Detection
  
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KeyWord:fluoroquinolones(FQs); solid-phase extraction-high performance liquid chromatography with fluorescence detection; livestock and poultry excrement; analytical method
Author NameAffiliation
LIU Bo College of Resources and Environment, Hunan Agricultural University, Changsha 410128, China
State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China 
XUE Nan-dong State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China 
YANG Bing State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China 
GONG Dao-xin College of Resources and Environment, Hunan Agricultural University, Changsha 410128, China 
LI Fa-sheng State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China 
ZHANG Shi-lei State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China 
ZHOU Ling-li State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China 
MENG Lei State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China 
CHEN Xuan-yu College of Resources and Environment, Hunan Agricultural University, Changsha 410128, China
State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China 
YAN Yun-zhong State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China 
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Abstract:
      An analytical method for simultaneous determination of six fluoroquinolones(FQs) in chicken manures based on solid-phase extraction and high performance liquid chromatography with a fluorescence detection(HPLC/FLD) was developed in the current study. Samples were ultrasonically extracted in Mcllvaine-Na2EDTA buffer/acetonitrile(1∶1)(pH=2) for 15 min. The extract was cleaned by a HLB solid-phase extraction column, and then eluted with methanol solvent. The fluoroquinolones in the extract were determined by HPLC/FLD with acetonitrile/0.7% phosphate as mobile phase. In a concentration range of 0.01~1.0 mg·kg-1, R2 of calibration was greater than 0.99. The average percent recoveries ranged from 76.7% to 106.7% for six compounds in chicken manure samples at three different spiked levels(0.1, 0.5 mg·kg-1 and 1.0 mg·kg-1). The detection limits(LOD) were from 0.002 mg·kg-1 to 0.022 mg·kg-1, and limit of quantification(LOQ) from 0.006 8 mg·kg-1 to 0.074 mg·kg-1. This method was used to analyze six FQs in chicken manures collected from 5 chicken farms in Beijing. All six FQs were detected in most samples, with concentrations ranging from LOD to 1.13 mg·kg-1.