HPLC with Post-Column Derivatization with Alizarin for Determination of OATD-02, an Anticancer Arginase Inhibitor in Clinical Development

The aim of this study was to develop an analytical method for selective determination of OATD-02 by high-performance liquid chromatography (HPLC) with post-column derivatization and fluorescence detection (FLD). OATD-02, a new boronic acid derivative, is a highly potent anticancer arginase inhibitor...

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Main Authors: Elzbieta Sobolewska, Magdalena Tyszkiewicz, Roman Blaszczyk, Magdalena Biesaga
Format: Article
Language:English
Published: MDPI AG 2023-08-01
Series:Applied Sciences
Subjects:
Online Access:https://www.mdpi.com/2076-3417/13/16/9201
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author Elzbieta Sobolewska
Magdalena Tyszkiewicz
Roman Blaszczyk
Magdalena Biesaga
author_facet Elzbieta Sobolewska
Magdalena Tyszkiewicz
Roman Blaszczyk
Magdalena Biesaga
author_sort Elzbieta Sobolewska
collection DOAJ
description The aim of this study was to develop an analytical method for selective determination of OATD-02 by high-performance liquid chromatography (HPLC) with post-column derivatization and fluorescence detection (FLD). OATD-02, a new boronic acid derivative, is a highly potent anticancer arginase inhibitor in clinical development. Chromatographic analysis of OATD-02 poses problems because this molecule has weak ultraviolet absorption. The derivatization reaction was based on the reaction between boronic acid from OATD-02 and alizarin solution. The optimized mobile phase consisted of a mixture of sodium bicarbonate in water and acetonitrile at a flow rate of 0.50 mL/min. Alizarin solution in methanol was delivered at a flow rate of 0.50 mL/min. The fluorescent complexes were detected by a fluorescence detector (excitation and emission wavelengths at 470 and 580 nm, respectively). The present method demonstrated proper values for selectivity, linearity, recovery (>99%), precision (RSD: 0.6%), sensitivity (LOD: 20 µg/mL and LOQ: 50 µg/mL), stability of solutions, and robustness.
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spelling doaj.art-8ef73bdfc5c7465fa5218c3957cda0052023-11-19T00:05:59ZengMDPI AGApplied Sciences2076-34172023-08-011316920110.3390/app13169201HPLC with Post-Column Derivatization with Alizarin for Determination of OATD-02, an Anticancer Arginase Inhibitor in Clinical DevelopmentElzbieta Sobolewska0Magdalena Tyszkiewicz1Roman Blaszczyk2Magdalena Biesaga3Faculty of Chemistry, University of Warsaw, Pasteur 1 Street, 02-093 Warsaw, PolandMolecure SA, Zwirki i Wigury 101 Street, 02-089 Warsaw, PolandMolecure SA, Zwirki i Wigury 101 Street, 02-089 Warsaw, PolandFaculty of Chemistry, University of Warsaw, Pasteur 1 Street, 02-093 Warsaw, PolandThe aim of this study was to develop an analytical method for selective determination of OATD-02 by high-performance liquid chromatography (HPLC) with post-column derivatization and fluorescence detection (FLD). OATD-02, a new boronic acid derivative, is a highly potent anticancer arginase inhibitor in clinical development. Chromatographic analysis of OATD-02 poses problems because this molecule has weak ultraviolet absorption. The derivatization reaction was based on the reaction between boronic acid from OATD-02 and alizarin solution. The optimized mobile phase consisted of a mixture of sodium bicarbonate in water and acetonitrile at a flow rate of 0.50 mL/min. Alizarin solution in methanol was delivered at a flow rate of 0.50 mL/min. The fluorescent complexes were detected by a fluorescence detector (excitation and emission wavelengths at 470 and 580 nm, respectively). The present method demonstrated proper values for selectivity, linearity, recovery (>99%), precision (RSD: 0.6%), sensitivity (LOD: 20 µg/mL and LOQ: 50 µg/mL), stability of solutions, and robustness.https://www.mdpi.com/2076-3417/13/16/9201post-column derivatizationactive pharmaceutical ingredientarginase inhibitorHPLC
spellingShingle Elzbieta Sobolewska
Magdalena Tyszkiewicz
Roman Blaszczyk
Magdalena Biesaga
HPLC with Post-Column Derivatization with Alizarin for Determination of OATD-02, an Anticancer Arginase Inhibitor in Clinical Development
Applied Sciences
post-column derivatization
active pharmaceutical ingredient
arginase inhibitor
HPLC
title HPLC with Post-Column Derivatization with Alizarin for Determination of OATD-02, an Anticancer Arginase Inhibitor in Clinical Development
title_full HPLC with Post-Column Derivatization with Alizarin for Determination of OATD-02, an Anticancer Arginase Inhibitor in Clinical Development
title_fullStr HPLC with Post-Column Derivatization with Alizarin for Determination of OATD-02, an Anticancer Arginase Inhibitor in Clinical Development
title_full_unstemmed HPLC with Post-Column Derivatization with Alizarin for Determination of OATD-02, an Anticancer Arginase Inhibitor in Clinical Development
title_short HPLC with Post-Column Derivatization with Alizarin for Determination of OATD-02, an Anticancer Arginase Inhibitor in Clinical Development
title_sort hplc with post column derivatization with alizarin for determination of oatd 02 an anticancer arginase inhibitor in clinical development
topic post-column derivatization
active pharmaceutical ingredient
arginase inhibitor
HPLC
url https://www.mdpi.com/2076-3417/13/16/9201
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