Determination of raloxifene hydrochloride in human urine by LC-MS-MS

A sensitive and selective liquid chromatographic-tandem mass spectrometric (LC-MS-MS) method was developed to determine raloxifene hydrochloride (RLX) in human urine. After a solid-phase extraction with SPE cartridge, the urine sample was analyzed on a C18 column (Symmetry 3.5μm; 50 mm 4.6 mm i.d) interfaced with a triple quadruple tandem mass spectrometer. A positive electrospray ionization was employed as the ionization source. The mobile phase consisted of ammonium acetate (pH 4.0)–acetonitrile (60:40, v/v).The method was linear over a concentration range of 20–1000 ng mL-1. The lower limit of quantitation was 20 ng mL-1. The intra-day and inter-day relative standard deviation across three validation runs over the entire concentration range was <10.5%. The accuracy determined at three concentrations (50, 500 and 850 ng mL-1 RLX) was within ±0.84% in terms of relative errors.