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Combination of magnetic dispersive micro solid-phase extraction and supramolecular solvent-based microextraction followed by high-performance liquid chromatography for determination of trace amounts of cholesterol-lowering drugs in complicated matrices

Abstract

A novel, efficient, rapid, simple, sensitive, selective, and environmentally friendly method termed magnetic dispersive micro solid-phase extraction combined with supramolecular solvent-based microextraction (Mdμ-SPE–SSME) followed by high-performance liquid chromatography (HPLC) with UV detection is introduced for the simultaneous microextraction of cholesterol-lowering drugs in complicated matrices. In the first microextraction procedure, using layered double hydroxide (LDH)-coated Fe3O4 magnetic nanoparticles, an efficient sample cleanup is simply and rapidly provided without the need for time-consuming centrifugation and elution steps. In the first step, desorption of the target analytes is easily performed through dissolution of the LDH-coated magnetic nanoparticles containing the target analytes in an acidic solution. In the next step, an emulsification microextraction method based on a supramolecular solvent is used for excellent preconcentration, ultimately resulting in an appropriate determination of the target analytes in real samples. Under the optimal experimental conditions, the Mdμ-SPE–SSME–HPLC–UV detection procedure provides good linearity in the ranges of 1.0–1500 ng mL-1, 1.5–2000 ng mL-1, and 2.0–2000 ng mL-1 with coefficients of determination of 0.995 or less, low limits of detection (0.3, 0.5, and 0.5 ng mL-1), and good extraction repeatabilities (relative standard deviations below 7.8%, n = 5) in deionized water for rosuvastatin, atorvastatin, and gemfibrozil, respectively. Finally, the proposed method is successfully applied for the determination of the target analytes in complicated matrices.

Mdμ-SPE–SSME procedure

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Acknowledgements

The authors gratefully acknowledge the financial support of Semnan University.

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Correspondence to Maryam Rajabi.

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All drug-free human urine and plasma samples used in this study were obtained from individual participants with their informed consent in accordance with institutional principles and standards. These studies were approved by Semnan University Research Council and were performed in accordance with ethical standards.

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Arghavani-Beydokhti, S., Rajabi, M. & Asghari, A. Combination of magnetic dispersive micro solid-phase extraction and supramolecular solvent-based microextraction followed by high-performance liquid chromatography for determination of trace amounts of cholesterol-lowering drugs in complicated matrices. Anal Bioanal Chem 409, 4395–4407 (2017). https://doi.org/10.1007/s00216-017-0383-x

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Keywords

  • Magnetic dispersive micro solid-phase extraction
  • Supramolecular solvent-based microextraction
  • Layered double hydroxide-coated magnetic nanoparticles
  • Complicated matrices