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Single column comprehensive analysis of pharmaceutical preparations using dual-injection mixed-mode (ion-exchange and reversed-phase) and hydrophilic interaction liquid chromatography

Citation

Kazarian, AA and Taylor, MR and Haddad, PR and Nesterenko, PN and Paull, B, Single column comprehensive analysis of pharmaceutical preparations using dual-injection mixed-mode (ion-exchange and reversed-phase) and hydrophilic interaction liquid chromatography, Journal of Pharmaceutical and Biomedical Analysis, 86 pp. 174-181. ISSN 0731-7085 (2013) [Refereed Article]

Copyright Statement

Copyright 2013 Published by Elsevier B.V.

DOI: doi:10.1016/j.jpba.2013.08.003

Abstract

The comprehensive separation and detection of hydrophobic and hydrophilic active pharmaceutical ingredients (APIs), their counter-ions (organic, inorganic) and excipients, using a single mixed-mode chromatographic column, and a dual injection approach is presented. Using a mixed-mode Thermo Fisher Acclaim Trinity P1 column, APIs, their counter-ions and possible degradants were first separated using a combination of anion-exchange, cation-exchange and hydrophobic interactions, using a mobile phase consisting of a dual organic modifier/salt concentration gradient. A complementary method was also developed using the same column for the separation of hydrophilic bulk excipients, using hydrophilic interaction liquid chromatography (HILIC) under high organic solvent mobile phase conditions. These two methods were then combined within a single gradient run using dual sample injection, with the first injection at the start of the applied gradient (mixed-mode retention of solutes), followed by a second sample injection at the end of the gradient (HILIC retention of solutes). Detection using both ultraviolet absorbance and refractive index enabled the sensitive detection of APIs and UV-absorbing counter-ions, together with quantitative determination of bulk excipients. The developed approach was applied successfully to the analysis of a dry powder inhalers (FlixotideŽ, SpirivaŽ), enabling comprehensive quantification of all APIs and excipients in the sample.

Item Details

Item Type:Refereed Article
Keywords:mixed-mode chromatography, ion-exchange, HILIC, active pharmaceutical ingredients, excipients
Research Division:Chemical Sciences
Research Group:Analytical Chemistry
Research Field:Separation Science
Objective Division:Manufacturing
Objective Group:Human Pharmaceutical Products
Objective Field:Human Pharmaceutical Products not elsewhere classified
Author:Kazarian, AA (Dr Tom Kazarian)
Author:Haddad, PR (Professor Paul Haddad)
Author:Nesterenko, PN (Professor Pavel Nesterenko)
Author:Paull, B (Professor Brett Paull)
ID Code:86143
Year Published:2013
Web of Science® Times Cited:8
Deposited By:Austn Centre for Research in Separation Science
Deposited On:2013-08-27
Last Modified:2014-05-08
Downloads:0

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