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

Mikhail, IE, Tehranirokh, M ORCID: 0000-0002-0057-4720, Gooley, AA, Guijt, RM ORCID: 0000-0003-0011-5708 and Breadmore, MC ORCID: 0000-0001-5591-4326 2020 , 'In-syringe electrokinetic protein removal from biological samples prior to electrospray ionization mass spectrometry' , Angewandte Chemie - International Edition, vol. 59, no. 51 , pp. 23162-23168 , doi: 10.1002/anie.202006481.

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Abstract

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 Type: Article
Authors/Creators:Mikhail, IE and Tehranirokh, M and Gooley, AA and Guijt, RM and Breadmore, MC
Keywords: analytical chemistry
Journal or Publication Title: Angewandte Chemie - International Edition
Publisher: Wiley-V C H Verlag Gmbh
ISSN: 1433-7851
DOI / ID Number: 10.1002/anie.202006481
Copyright Information:

Copyright 2020 Wiley-VCH GmbH

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