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Graphene Oxide/Polyethylene Glycol-Stick for Thin Film Microextraction of beta-Blockers from Human Oral Fluid by Liquid Chromatography-Tandem Mass Spectrometry
KTH, School of Engineering Sciences (SCI), Applied Physics. Univ Mazandaran, Dept Chem, Babol Sar 4741695447, Iran.
Univ Mazandaran, Dept Chem, Babol Sar 4741695447, Iran..
KTH, School of Engineering Sciences (SCI), Applied Physics.ORCID iD: 0000-0001-9424-6965
Karolinska Univ Hosp, Dept Radiopharm, S-17176 Stockholm, Sweden..
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2019 (English)In: Molecules, ISSN 1420-3049, E-ISSN 1420-3049, Vol. 24, no 20Article in journal (Refereed) Published
Abstract [en]

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 beta -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 (R-2) 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.

Place, publisher, year, edition, pages
MDPI , 2019. Vol. 24, no 20
Keywords [en]
graphene oxide, polyethylene glycol, wooden stick, beta-blocker, oral fluid, LC-MS, MS
National Category
Analytical Chemistry
Identifiers
URN: urn:nbn:se:kth:diva-264869DOI: 10.3390/molecules24203664ISI: 000496249500033PubMedID: 31614604Scopus ID: 2-s2.0-85073427233OAI: oai:DiVA.org:kth-264869DiVA, id: diva2:1379814
Note

QC 20191217

Available from: 2019-12-17 Created: 2019-12-17 Last updated: 2019-12-17Bibliographically approved

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Laxman, KarthikDutta, JoydeepAbdel-Rehim, Mohamed

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