Artículos de revistas
Rapid determination of hydrochlorothiazide in human plasma by high performance liquid chromatography-tandem mass spectrometry
Autor
Sousa, Carlos E.M.
Bedor, Danilo C. G.
Gonçalves, Talita M.
Ramos, Virna L.S.
Carvalho, Andre L.M.
Albuquerque, Miracy M.
Santana, Davi P.
Institución
Resumen
This paper describes a rapid (2.0 min) and sensitive (LLOQ 5 ng/mL) analytical method for the quantitation of hydrochlorothiazide (HCTZ) in human plasma. The method is based on High-performance Liquid chromatography-tandem mass spectrometry (LC-MS/MS) using clortalidone as internal standard (I.S.). Sample preparation involved liquid-liquid extraction with methyl tert-butyl ether. The chromatographic separation was achieved on a monolitic C18 (50 x 4,6 mm) reversed-phase column and a mobile phase containing acetonitrile/water (80:20 v/v, add 5% isopropyl alcohol), in isocratic conditions. The target analytes were transferred into a triple quadrupole mass spectrometer equipped with an electrospray ionization source for mass detection. The ion transitions selected for MRM detection were: m/z 296.10 > 204.85 and 337.13 > 189.77 for HCTZ and I.S., respectively. The assay was linear in the concentration range of 5-400 ng/mL. The mean recovery for HCTZ was 80.46%. Intra- and inter-day precision (Relative Standard Desviation) were < 10.3 % and <11.7%, respectively and the accuracy (Relative Error) was in the range ± 4.54%, the accuracy was evaluated by the ratio between concentration found/nominal concentration. The method was successfully applied to a single oral dose pharmacokinetics study in 26 healthy human volunteers