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| Simultaneous determination of four fluoroquinolones in biogas slurry by high performance liquid chromatography with fluorescence detection |
| Received:April 01, 2016 |
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| KeyWord:fluoroquinolones;solid-phase extraction-high performance liquid chromatography with fluorescence detection;biogas slurry;analytical method |
| Author Name | Affiliation | E-mail | | HE Nan-nan | College of Resources and Environmental Sciences, Nanjing Agricultural University, Nanjing 210095, China | | | GUAN Yong-xiang | Jiangsu Station of Cultivate-land Qualitative and Agro-Environmental Protection, Nanjing 210036, China | | | LIANG Yong-hong | Jiangsu Station of Cultivate-land Qualitative and Agro-Environmental Protection, Nanjing 210036, China | | | WU Hao | Jiangsu Station of Agro-Environmental Monitoring and Protection, Nanjing 210036, China | | | LUO Zhao-hui | College of Resources and Environmental Sciences, Nanjing Agricultural University, Nanjing 210095, China | lzhui@niau.edu.cn | | ZHAO Hai-yan | College of Resources and Environmental Sciences, Nanjing Agricultural University, Nanjing 210095, China | haiyanzhao@njau.edu.cn | | GU Zu-li | College of Resources and Environmental Sciences, Nanjing Agricultural University, Nanjing 210095, China | |
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| Abstract: |
| An analytical method for simultaneous determination of four fluoroquinolones(FQs) in biogas slurry based on solid-phase extraction and high performance liquid chromatography with a fluorescence detection(HPLC/FLD) was developed in this study. The homogenized sample adjusted to pH=4 was extracted with Na2EDTA solution, purified by Oasis HLB solid phase extraction after vortexing, and eluted with 6 mL methanol solvent. The FQs in the extract were determined by HPLC/FLD with acetonitrile and 0.01 mol·L-1 tetrabutylammonium bromide as mobile phases. Quantitation was carried out using an external standard method. The standard curves for all the compounds were linear over the concentration ranges of 0.002 mg·L-1 to 5.0 mg·L-1 with all correlation coefficients above 0.990． The spiked recoveries at six levels of 0.1, 0.2, 0.5, 1.0, 2.0 mg·L-1 and 5.0 mg·L-1 were ranged from 80.4% to 105.7%, and the relatives standard deviations(RSD) were in the ranges of 1.0% to 5.1%. The limits of detection were from 0.004 mg·L-1 to 0.01 mg·L-1. This method was used to analyze four FQs in biogas slurry samples fermented with chicken dung, pig dung, and cow dung collected from 3 large and medium-sized biogas projects in Nanjing. Four FQs were detected in all samples, with concentrations ranging from 5 μg·L-1 to 204 μg·L-1, four kinds of FQs were detected. Therefore, antibiotic pollution problems in biogas slurry deserve attention. |
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