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In-syringe electrokinetic protein removal from biological samples prior to electrospray ionization mass spectrometry


Mikhail, IE and Tehranirokh, M and Gooley, AA and Guijt, RM and Breadmore, MC, In-syringe electrokinetic protein removal from biological samples prior to electrospray ionization mass spectrometry, Angewandte Chemie - International Edition, 59, (51) pp. 23162-23168. ISSN 1433-7851 (2020) [Refereed Article]

Copyright Statement

Copyright 2020 Wiley-VCH GmbH

DOI: doi:10.1002/anie.202006481


Here, an electrokinetic extraction (EkE) syringe is presented allowing for on‐line electrokinetic removal of serum proteins before ESI-MS. The proposed concept is demonstrated by the determination of pharmaceuticals from human serum within minutes, with sample preparation limited to a 5 dilution of the sample in the background electrolyte (BGE) and application of voltage, both of which can be performed in‐syringe. Signal enhancements of 3.6-32 fold relative to direct infusion of diluted serum and up to 10.8 fold enhancement, were obtained for basic and acidic pharmaceuticals, respectively. Linear correlations for the basic drugs by EkE‐ESI‐MS/MS were achieved, covering the necessary clinical range with LOQs of 5.3, 7.8, 6.1, and 17.8 ng mL-1 for clomipramine, chlorphenamine, pindolol, and atenolol, respectively. For the acidic drugs, the EkE‐ESI‐MS LOQs were 3.1 μg mL-1 and 2.9 μg mL-1 for naproxen and paracetamol, respectively. The EkE‐ESI‐MS and EkE‐ESI‐MS/MS methods showed good accuracy (%found of 81 % to 120 %), precision (≤20 %), and linearity (r>0.997) for all the studied drugs in spiked serum samples.

Item Details

Item Type:Refereed Article
Keywords:analytical chemistry
Research Division:Chemical Sciences
Research Group:Analytical chemistry
Research Field:Separation science
Objective Division:Expanding Knowledge
Objective Group:Expanding knowledge
Objective Field:Expanding knowledge in the chemical sciences
UTAS Author:Mikhail, IE (Dr Ibraam Mikhail)
UTAS Author:Tehranirokh, M (Dr Masoomeh Tehrani Rokh)
UTAS Author:Guijt, RM (Dr Rosanne Guijt)
UTAS Author:Breadmore, MC (Professor Michael Breadmore)
ID Code:143975
Year Published:2020
Funding Support:Australian Research Council (IC140100022)
Web of Science® Times Cited:2
Deposited By:Chemistry
Deposited On:2021-04-13
Last Modified:2022-08-25

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