Simultaneous determination of raloxifene and tamoxifen using dispersive micro solid-phase extraction and HPLC method in real water, human hair and serum samples

A sensitive determination procedure was presented for two anticancer drugs (tamoxifen and raloxifene) in real water and biological samples based on magnetic dispersive micro solid-phase extraction-high-performance liquid chromatography with an ultraviolet detector. Fe3O4 NPs@SiO2@TiO2 nanocomposite was synthesised as a magnetic sorbent by the sol-gel technique. The effective parameters in the procedure were optimised with an experimental design, including screening and optimisation steps. Under the optimum determination conditions, the procedure displayed wide linear ranges of 5.3-735.0 and 7.0-806.0 ng mL(-1) with R-squared of 0.9916 and 0.9908, limit of detections of 1.6 and 2.1 ng mL(-1) for the raloxifene and tamoxifen determination, respectively. The intra-day relative standard deviations were 3.76 and 3.59% for three times the raloxifene and tamoxifen measurements, respectively. The preconcentration factors for the raloxifene and tamoxifen determination with a concentration of 20 ng mL(-1) were 506.1 and 546.7, respectively. The method was applied to analyse well water, tap water, and hair samples and determine raloxifene and tamoxifen simultaneously with recoveries between 88.5-96.4 and relative standard deviations lower than 8.4%. The method's advantages for raloxifene and tamoxifen measurement included easy operation, low sorbent and desorption solvent consumption, simple sorbent preparation and separation, and suitable analysis time.