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Open AccessArticle

Graphene Oxide/Polyethylene Glycol-Stick for Thin Film Microextraction of β-Blockers from Human Oral Fluid by Liquid Chromatography-Tandem Mass Spectrometry

1
Functional Materials Group, Department of Applied Physics, School of Engineering Sciences, KTH Royal Institute of Technology, Isafjordsgatan 22, Kista, SE-164 40 Stockholm, Sweden
2
Department of Chemistry, University of Mazandaran, Babolsar 47416-95447, Iran
3
Department of Radiopharmacy, Karolinska University Hospital, S-171 76 Stockholm, Sweden
4
Department of Clinical Neuroscience, Centre for Psychiatry Research, Karolinska Institutet, SE-171 76 Stockholm, Sweden
*
Author to whom correspondence should be addressed.
Academic Editors: Marcello Locatelli, Angela Tartaglia, Abuzar Kabir, Roberta Risoluti and Stefano Materazzi
Molecules 2019, 24(20), 3664; https://doi.org/10.3390/molecules24203664
Received: 7 September 2019 / Revised: 26 September 2019 / Accepted: 4 October 2019 / Published: 11 October 2019
A wooden stick coated with a novel graphene-based nanocomposite (Graphene oxide/polyethylene glycol (GO/PEG)) is introduced and investigated for its efficacy in solid phase microextraction techniques. The GO/PEG-stick was prepared and subsequently applied for the extraction of β-blockers, acebutolol, and metoprolol in human oral fluid samples, which were subsequently detected by liquid chromatography tandem mass spectrometry (LC-MS/MS). Experimental parameters affecting the extraction protocol including sample pH, extraction time, desorption time, appropriate desorption solvent, and salt addition were optimized. Method validation for the detection from oral fluid samples was performed following FDA (Food and Drug Administration) guidelines on bioanalytical method validation. Calibration curves ranging from 5.0 to 2000 nmol L−1 for acebutolol and 25.0 to 2000 nmol L−1 for metoprolol were used. The values for the coefficient of determination (R2) were found to be 0.998 and 0.996 (n = 3) for acebutolol and metoprolol, respectively. The recovery of analytes during extraction was 80.0% for acebutolol and 62.0% for metoprolol, respectively. The limit of detections (LODs) were 1.25, 8.00 nmol L−1 for acebutolol and metoprolol and the lower limit of quantifications (LLOQ) were 5.00 nmol L−1 for acebutolol and 25.0 nmol L−1 for metoprolol. Validation experiments conducted with quality control (QC) samples demonstrated method accuracy between 80.0% to 97.0% for acebutolol and from 95.0% to 109.0% for metoprolol. The inter-day precision for QC samples ranged from 3.6% to 12.9% for acebutolol and 9.5% to 11.3% for metoprolol. Additionally, the GO/PEG-stick was demonstrated to be reusable, with the same stick observed to be viable for more than 10 extractions from oral fluid samples. View Full-Text
Keywords: graphene oxide/polyethylene glycol; wooden stick; β-blocker; oral fluid; LC-MS/MS graphene oxide/polyethylene glycol; wooden stick; β-blocker; oral fluid; LC-MS/MS
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MDPI and ACS Style

Karimiyan, H.; Hadjmohammadi, M.R.; Kunjali, K.L.; Moein, M.M.; Dutta, J.; Abdel-Rehim, M. Graphene Oxide/Polyethylene Glycol-Stick for Thin Film Microextraction of β-Blockers from Human Oral Fluid by Liquid Chromatography-Tandem Mass Spectrometry. Molecules 2019, 24, 3664.

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