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Quantitative determination of rifampicin in aquatic products by stable isotope-dilution high liquid chromatography–tandem mass spectrometry
Authors:Qin Li  Jingyuan Cao  Gang Han  Huan Liu  Jie Yan  Lidong Wu  Jincheng Li
Institution:1. College of Fisheries and Life Science, Shanghai Ocean University, Shangha, P. R. China

Chinese Academy of Fishery Sciences, Beijing, P. R. China

Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture and Rural Affairs, Beijing, P. R. China;2. Beijing University of Agriculture, Beijing, China;3. College of Fisheries and Life Science, Shanghai Ocean University, Shangha, P. R. China

Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture and Rural Affairs, Beijing, P. R. China;4. College of Fisheries and Life Science, Shanghai Ocean University, Shangha, P. R. China

Abstract:Rifampicin is a semi-synthetic broad-spectrum antibiotic obtained from rifamycin B. It is one of the most effective first-line antituberculosis drugs and is widely used in clinical practice. In the present study, we describe a rapid and sensitive method for the determination of rifampin in aquatic products by stable isotope-dilution high liquid chromatography–tandem mass spectrometry (HPLC–MS/MS). Samples were extracted with the acetonitrile, degreased by hexane, and then concentrated by nitrogen blowing. After separation using a C18 column with a mixture of acetonitrile and water as mobile phase, it was determined by HPLC–MS/MS using the stable isotope-dilution calibration method. The performance of our method was validated. The limit of detection was 0.25 μg kg−1 and the limit of quantification was 0.5 μg kg−1. At the three spiked levels of 0.5, 1.0 and 5.0 μg kg−1, the average recoveries of rifampicin in different aquatic products were between 75.28 and 107.6%, and the relative standard deviation ranged from 0.81 to 13.23%. This method was successfully applied for the determination of rifampin in different kinds of aquatic products and rifampicin residue was found in aquatic products obtained from markets in Beijing, China.
Keywords:aquatic products  determination  high liquid chromatography–tandem mass spectrometry  rifampin
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