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

• Main Authors: K. Tharpa, K. Basavaiah, U.R.A. Kumar, K.B. Vinay
• Format: Article
• Language: English
• Published: Association of the Chemical Engineers of Serbia 2009-09-01
• Series: Chemical Industry and Chemical Engineering Quarterly
• Subjects: raloxifene; quantification; LC-MS-MS; urine
• Online Access: http://www.ache.org.rs/CICEQ/2009/No3/CICEQ_Vol15_%20No3_pp119-%60123_Jul-Sep_2009.pdf

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.