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| Determination of Seven Quinolones Antibiotics in Fishery Water Using Salting-out Assisted Liquid－Liquid Extraction and High Performance Liquid Chromatography－Tandem Mass Spectrometry |
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| DOI： |
| KeyWord:salting-out assisted liquid－liquid extraction high performance liquid chromatography－tandem mass spectrometry quinolones antibiotics fishery water |
| Author | Institution |
| YANG Xiao，LIU Ling-li，LI Xiao-ling，XIAO Wei，CHEN Xiang-yi，XIE Zhong-gui |
1. Hunan Fisheries Science Institute，Changsha ，China; 2. Fishery Products Quality Supervision and Testing Center，Ministry of Agriculture and Rural Affairs，Changsha ，China |
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| Abstract: |
| A method for determination of seven quinolones antibiotics in fishery water was established based on salting-out assisted liquid－liquid extraction（SALLE） coupled with high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）．Water samples were extracted with acetonitrile and layered with salting-out agent of magnesium sulfate．The acetonitrile solution was concentrated under a stream of nitrogen gas．All antibiotics were separated by gradient elution on a Waters Atlantis C18 column（150 mm × 2.1 mm，3.0 μm） with the mobile phases of 0.1%（by volume） formic acid aqueous solution and methanol，and then analyzed with an electrospray ionization source in the positive ion mode．The external standard method was used for quantitative analysis of the antibiotics．Various parameters affecting the extraction process such as pH value of the water sample，type and volume of extraction solvent，type and weight of salting-out agent and vortex agitation time were investigated．Under the optimal conditions，the correlation coefficients（r2） of linear calibration curves were over 0.995 in the corresponding concentration ranges．The limits of detection（LOD） and the limits of quantitation（LOQ） of the method were in the range of 3－10 ng/L and 10－25 ng/L，respectively．Recoveries for the seven quinolones at three spiked levels ranged from 77.8% to 104%，with relative standard deviations（RSD） of 3.1%－10%．The method is simple，sensitive and effective，and could be used for the determination of seven quinolones antibiotics in fishery water. |
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