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Preparation and characterization of microporous fibers for sample preparation and LC‐MS determination of drugs
Authors:Boguslaw Buszewski  Jacek Nowaczyk  Tomasz Ligor  Pawel Olszowy  Magdalena Ligor  Bartlomiej Wasiniak  Wolfram Miekisch  Jochen K. Schubert  Anton Amann
Affiliation:1. Chair of Physical Chemistry and Physicochemistry of Polymers, Faculty of Chemistry, Nicolaus Copernicus University, Torun, Poland;2. Chair of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus Copernicus University, Torun, Poland. Fax: +48‐56‐611‐4837;3. Department of Anesthesiology and Intensive Care, Faculty of Medicine, University of Rostock, Rostock, Germany;4. Department of Anesthesiology and Critical Medicine Care, Innsbruck Medical University, Innsbruck, Austria
Abstract:
The aim of this study was the preparation of polypyrrole (PPy) fibers for solid phase microextraction (SPME). PPy coatings were obtained during the electrochemical polymerization process. The utility of various metal wires (Fe, Cu, Ag, Cu/Ag, kanthal and medical stainless steel) as a support for polymers was compared. Various experimental conditions of the synthesis process such as scan rate, voltage limits and number of scans and deposition time were applied. The average polymer thickness was in the range of 7–125 μm and its weight was in the scope of 0.65–5.6 mg. Different techniques, mainly elemental analysis, Fourier transform infrared spectroscopy, microscopy, and chromatography were performed for the characterization of obtained fibers with microporous structure. The extraction efficiency of cardiovascular drugs (metoprolol, propranolol, oxprenolol, propafenone and mexiletine) by means of fibers was tested. The concentration of mentioned compounds in standard solution was in the span of 10–150 ng/mL. LC‐MS was employed for determination of drugs in desorption solution. LODs varied from 0.013 to 1.51 ng/mL for metoprolol and mexiletine respectively. The repeatability of extraction was obtained with the RSD values lower than 10%.
Keywords:Cardiovascular drugs  Electropolymerization  HPLC‐MS  Polypyrrole  Solid phase microextraction
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