Preparation and characterization of microporous fibers for sample preparation and LC-MS determination of drugs.
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 microm 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%.
Buszewski
Boguslaw
B
Faculty of Chemistry, Nicolaus Copernicus University, Torun, Poland. bbusz@chem.uni.torun.pl
Nowaczyk
Jacek
J
Ligor
Tomasz
T
Olszowy
Pawel
P
Ligor
Magdalena
M
Wasiniak
Bartlomiej
B
Miekisch
Wolfram
W
Schubert
Jochen K
JK
Amann
Anton
A
D002317:Cardiovascular Agents / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D013058:Mass Spectrometry; D008567:Membranes, Artificial; D008970:Molecular Weight; D010316:Particle Size; D011108:Polymers / Q000138:chemical synthesis* / Q000737:chemistry*; D016062:Porosity; D011758:Pyrroles / Q000138:chemical synthesis* / Q000737:chemistry*; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction; D013499:Surface Properties
D002317:Cardiovascular Agents; D008567:Membranes, Artificial; D011108:Polymers; D011758:Pyrroles; C067635:polypyrrole