Xây dựng và thẩm định phương pháp định lượng bilastin trong huyết tương người bằng phương pháp LC-MS/MS

Abstract

A simple, specifc and sensitive LC-MS/MS method has been developed for determination of bilastine in human plasma. The analyte and the internal standard (carbamazepine) were extracted from human plasma by the protein precipitation method with acetonitrile. Chromatographic analysis was developed on a C18 column (dimention 50 x 2.1 mm, particle 1.7 µm) with isocratic elution at a fow rate of 0.2 ml/min using a mobile phase of water (10 mM ammonium formate + 0.1 % formic acid) and acetonitrile (10 mM ammonium formate + 0.1 % formic acid) with suitable ratio. The Waters Xevo TQ-XS UPLC-MS/MS was operated under the multi reaction-monitoring mode using the positive ion mode, with transitions at (m/z) 463.80 →271.72 for (BIL), 236.70 → 164.70 for (IS). The method was validated over concentration range from 3 ng/ml to 600 ng/ml. The intra and inter-day precision and accuracy were within between 91.5 % and 105.7 %. This method can be used for BA-BE studies of bilastine preparations.