Journal of Chromatography B, 958 (2014) 22–28
Contents lists available at ScienceDirect
Journal of Chromatography B journal homepage: www.elsevier.com/locate/chromb
Comparison of different sorbent materials for solid-phase extraction of selected drugs in human urine analyzed by UHPLC–UV Sylwia Magiera a,∗ , Judyta Hejniak a , Jacek Baranowski b a b
Department of Inorganic, Analytical Chemistry and Electrochemistry, Silesian University of Technology, 7 M. Strzody Str., 44-100 Gliwice, Poland Department of Clinical Physiology, University Hospital, SE-581 85 Linköping, Sweden
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Article history: Received 27 December 2013 Received in revised form 3 March 2014 Accepted 6 March 2014 Available online 15 March 2014 Keywords: Sorbent comparison Solid-phase extraction Drugs Liquid chromatography
a b s t r a c t A procedure based on solid-phase extraction (SPE) followed by ultra-high-performance liquid chromatography (UHPLC) with UV detection has been developed for the analysis of multiple drugs in human urine. The compounds evaluated were aliskiren, prasugrel, rivaroxaban, prednisolone, propranolol, ketoprofen, nifedipine, naproxen, terbinafine, ibuprofen, diclofenac, sildenafil and acenocoumarol. Seventeen different solid phase extraction (SPE) cartridges were tested to evaluate their applicability for the isolation of drugs from human urine. Comparison were recovery of different drugs and reproducibility. The samples were analyzed by UHPLC using a Poroshell 120 EC-C18 column and acetonitrile −0.05% TFA in water as the mobile phase under gradient elution conditions. SPE combined with UHPLC–UV allowed the determination of drugs over a linear range of 0.01–30.0 g/mL, with limits of detection at 0.003–0.217 g/mL and precision of 0.8–7.1%. Phenyl (C6 H5 ) sorbent was found to provide the most effective clean-up, removing the greatest amount of interfering substance and simultaneously ensuring analyte recoveries higher than 85.5% with relative standard deviations (RSD) 0.996, indicating satisfactory linearity of the standard curves in the selected calibration range (Table 4). Additionally, the intercept value for all analytes contributed
Contents lists available at ScienceDirect
Journal of Chromatography B journal homepage: www.elsevier.com/locate/chromb
Comparison of different sorbent materials for solid-phase extraction of selected drugs in human urine analyzed by UHPLC–UV Sylwia Magiera a,∗ , Judyta Hejniak a , Jacek Baranowski b a b
Department of Inorganic, Analytical Chemistry and Electrochemistry, Silesian University of Technology, 7 M. Strzody Str., 44-100 Gliwice, Poland Department of Clinical Physiology, University Hospital, SE-581 85 Linköping, Sweden
a r t i c l e
i n f o
Article history: Received 27 December 2013 Received in revised form 3 March 2014 Accepted 6 March 2014 Available online 15 March 2014 Keywords: Sorbent comparison Solid-phase extraction Drugs Liquid chromatography
a b s t r a c t A procedure based on solid-phase extraction (SPE) followed by ultra-high-performance liquid chromatography (UHPLC) with UV detection has been developed for the analysis of multiple drugs in human urine. The compounds evaluated were aliskiren, prasugrel, rivaroxaban, prednisolone, propranolol, ketoprofen, nifedipine, naproxen, terbinafine, ibuprofen, diclofenac, sildenafil and acenocoumarol. Seventeen different solid phase extraction (SPE) cartridges were tested to evaluate their applicability for the isolation of drugs from human urine. Comparison were recovery of different drugs and reproducibility. The samples were analyzed by UHPLC using a Poroshell 120 EC-C18 column and acetonitrile −0.05% TFA in water as the mobile phase under gradient elution conditions. SPE combined with UHPLC–UV allowed the determination of drugs over a linear range of 0.01–30.0 g/mL, with limits of detection at 0.003–0.217 g/mL and precision of 0.8–7.1%. Phenyl (C6 H5 ) sorbent was found to provide the most effective clean-up, removing the greatest amount of interfering substance and simultaneously ensuring analyte recoveries higher than 85.5% with relative standard deviations (RSD) 0.996, indicating satisfactory linearity of the standard curves in the selected calibration range (Table 4). Additionally, the intercept value for all analytes contributed
