Li Qin, Cao Jingyuan, Han Gang, Liu Huan, Yan Jie, Wu Lidong, Li Jincheng
College of Fisheries and Life Science, Shanghai Ocean University, Shangha, P. R. China.
Chinese Academy of Fishery Sciences, Beijing, P. R. China.
Biomed Chromatogr. 2020 May;34(5):e4810. doi: 10.1002/bmc.4810. Epub 2020 Feb 25.
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 C 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 and the limit of quantification was 0.5 μg kg . At the three spiked levels of 0.5, 1.0 and 5.0 μg kg , 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.
利福平是一种从利福霉素B获得的半合成广谱抗生素。它是最有效的一线抗结核药物之一，在临床实践中广泛使用。在本研究中，我们描述了一种通过稳定同位素稀释高效液相色谱 - 串联质谱法（HPLC-MS/MS）测定水产品中利福平的快速灵敏方法。样品用乙腈萃取，用己烷脱脂，然后通过氮气吹干浓缩。使用以乙腈和水的混合物为流动相的C柱进行分离后，采用稳定同位素稀释校准法通过HPLC-MS/MS进行测定。我们方法的性能得到了验证。检测限为0.25μg/kg，定量限为0.5μg/kg。在0.5、1.0和5.0μg/kg三个加标水平下，不同水产品中利福平的平均回收率在75.28%至107.6%之间，相对标准偏差范围为0.81%至13.23%。该方法成功应用于不同种类水产品中利福平的测定，在中国北京市场获得的水产品中发现了利福平残留。
