Development of a sensitive and selective LC-MS/MS method for the determination of α-fluoro-β-alanine, 5-fluorouracil and capecitabine in human plasma

摘要: Abstract A sensitive and selective quantitative method to determine α-fluoro-β-alanine (FBAL), 5-fluorouracil (5-FU), capecitabine (Cape) from a single human plasma aliquot (50 μL) has been developed validated. First, 5-FU Cape were extracted by liquid–liquid extraction (LLE) using mixture of acetonitrile ethyl acetate. This was followed derivatization with dansyl chloride. The dansyl-derivatives further purified LLE methyl tertiary-butyl ether (MTBE) analyzed reversed-phase analytical column “Primesep D” (2.1 mm × 50 mm; 5 μm) embedded basic ion-pairing groups. remaining aqueous phase containing FBAL treated chloride the dansyl-FBAL solid extraction. Ultra high pressure liquid chromatography (UPLC) technology on BEH C18 stationary 1.7 μm particle size used for analysis dansyl-FBAL. validated over concentration ranges 10–10,000, 5–5000, 1–1000 ng/mL FBAL, 5-FU, Cape, respectively. results assay validation show that is rugged, precise, accurate, well suited support pharmacokinetic studies where approximately 300 samples can be in 1 day.