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HPLC column-switching technique for sample preparation and fluorescence determination of propranolol in urine using fused-core columns in both dimensions

Analytical and Bioanalytical Chemistry volume 405, pages 6583–6587 (2013)Cite this article

Abstract

A new and fast high-performance liquid chromatography (HPLC) column-switching method using fused-core columns in both dimensions for sample preconcentration and determination of propranolol in human urine has been developed. On-line sample pretreatment and propranolol preconcentration were performed on an Ascentis Express RP-C-18 guard column (5 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water (5:95, v/v) at a flow rate of 2.0 mL min−1 and at a temperature of 50 °C. Valve switch from pretreatment column to analytical column was set at 4.0 min in a back-flush mode. Separation of propranolol from other endogenous urine compounds was achieved on the fused-core column Ascentis Express RP-Amide (100 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water solution of 0.5 % triethylamine, pH adjusted to 4.5 by means of glacial acetic acid (25:75, v/v), at a flow rate of 1.0 mL min−1 and at a temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 229/338 nm. A volume of 1,500 μL of filtered urine sample solution was injected directly into the column-switching HPLC system. The total analysis time including on-line sample pretreatment was less than 8 min. The experimentally determined limit of detection of the method was found to be 0.015 ng mL−1.

Chromatogram 1, which was recorded by direct injection of 1,500 μL of two different urine samples without SPE sample pretreatment. Chromatogram 2, which was recorded by injection of 1,500 μL of urine sample with propranolol directly to the column-switching system

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Acknowledgments

The authors acknowledge the financial support of the Charles University in Prague—project UNCE 204026.

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Affiliations

  1. Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovského 1203, Hradec Králové, 500 05, Czech Republic

    Dalibor Šatínský, Lucie Havlíková & Petr Solich

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  1. Dalibor Šatínský
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  2. Lucie Havlíková
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  3. Petr Solich
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Correspondence to Dalibor Šatínský.

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Published in the topical collection Analytical and Bioanalytical Luminescence with guest editor Montserrat Pujol.

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Šatínský, D., Havlíková, L. & Solich, P. HPLC column-switching technique for sample preparation and fluorescence determination of propranolol in urine using fused-core columns in both dimensions. Anal Bioanal Chem 405, 6583–6587 (2013). https://doi.org/10.1007/s00216-013-7098-4

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  • DOI: https://doi.org/10.1007/s00216-013-7098-4

Keywords

  • Fused-core column
  • HPLC
  • Column switching
  • Large-volume sample
  • Propranolol
  • Urine