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| Simultaneous Determination of 5 Cephalosporins in Fish by High Performance Liquid Chromatography-Tandem Mass Spectrometry |
| BEI Yijiang, WANG Yang*, ZHU Ningyu, KE Qingqing, CHEN Xiaofang, LI Shiyan, ZHOU Fan |
| Zhejiang Fishery Technical Extension Center, Hangzhou 310023, China |
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Abstract A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the determination of five cephalosporins in fish (cephalexin, cefalonium, cephapirin, cefquinome and cefazolin). Samples were extracted with acetonitrile and then the extract was cleaned up with a Prime HLB solid-phase extraction (SPE) cartridge prior to being analyzed using an AB-4500 Qtrap LC-MS/MS system. The chromatographic separation was performed on an Accucore C18 RP-MS column (2.1 mm × 100 mm, 2.7 μm) by gradient elution using a mobile phase made up of acetonitrile and 0.1% acetic acid in water at a 0.4 mL/min flow rate. The column temperature was set at 30 ℃. The analytes were detected using multiple-reaction monitoring (MRM) in the positive electrospray ionization mode and quantified by the external standard method. Complete separation was achieved within 8 min. The calibration curves for all five analytes were linear over the concentration range from 0 to 75 μg/kg. The limit of detection for all analytes was 0.5 μg/kg, and the limit of quantification was 2.0 μg/kg. At spiked levels of 10, 25 and 40 μg/kg, the intra-assay recoveries of all five cephalosporins were 81.0%–111.0% with relative standard deviation (RSD) of 0.41%–10.50%, and the inter-assay recoveries were 84.7%– 106.0% with RSD of 0.88%–8.71%.
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2018, Vol. 32 
