Measuring and using scanning-gradient data for use in method optimization for liquid chromatography.

Autor: den Uijl MJ; University of Amsterdam, van 't Hoff Institute for Molecular Sciences, Analytical-Chemistry Group, Science Park 904, 1098 XH Amsterdam, the Netherlands; Centre for Analytical Sciences Amsterdam (CASA), The Netherlands. Electronic address: M.J.denUijl@uva.nl., Schoenmakers PJ; University of Amsterdam, van 't Hoff Institute for Molecular Sciences, Analytical-Chemistry Group, Science Park 904, 1098 XH Amsterdam, the Netherlands; Centre for Analytical Sciences Amsterdam (CASA), The Netherlands., Schulte GK; Department of Chemistry, Gustavus Adolphus College, Saint Peter, Minnesota 56082, USA., Stoll DR; Department of Chemistry, Gustavus Adolphus College, Saint Peter, Minnesota 56082, USA., van Bommel MR; University of Amsterdam, van 't Hoff Institute for Molecular Sciences, Analytical-Chemistry Group, Science Park 904, 1098 XH Amsterdam, the Netherlands; Centre for Analytical Sciences Amsterdam (CASA), The Netherlands; University of Amsterdam, Amsterdam School for Heritage, Memory and Material Culture, Conservation and Restoration of Cultural Heritage, Johannes Vermeerplein 1, 1071 DV Amsterdam, the Netherlands., Pirok BWJ; University of Amsterdam, van 't Hoff Institute for Molecular Sciences, Analytical-Chemistry Group, Science Park 904, 1098 XH Amsterdam, the Netherlands; Centre for Analytical Sciences Amsterdam (CASA), The Netherlands; Department of Chemistry, Gustavus Adolphus College, Saint Peter, Minnesota 56082, USA.
Jazyk: angličtina
Zdroj: Journal of chromatography. A [J Chromatogr A] 2021 Jan 11; Vol. 1636, pp. 461780. Date of Electronic Publication: 2020 Dec 02.
DOI: 10.1016/j.chroma.2020.461780
Abstrakt: The use of scanning gradients can significantly reduce method-development time in reversed-phase liquid chromatography. However, there is no consensus on how they can best be used. In the present work we set out to systematically investigate various factors and to formulate guidelines. Scanning gradients are used to establish retention models for individual analytes. Different retention models were compared by computing the Akaike information criterion and the prediction accuracy. The measurement uncertainty was found to influence the optimum choice of model. The use of a third parameter to account for non-linear relationships was consistently found not to be statistically significant. The duration (slope) of the scanning gradients was not found to influence the accuracy of prediction. The prediction error may be reduced by repeating scanning experiments or - preferably - by reducing the measurement uncertainty. It is commonly assumed that the gradient-slope factor, i.e. the ratio between slopes of the fastest and the slowest scanning gradients, should be at least three. However, in the present work we found this factor less important than the proximity of the slope of the predicted gradient to that of the scanning gradients. Also, interpolation to a slope between that of the fastest and the slowest scanning gradient is preferable to extrapolation. For comprehensive two-dimensional liquid chromatography (LC × LC) our results suggest that data obtained from fast second-dimension gradients cannot be used to predict retention in much slower first-dimension gradients.
Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
(Copyright © 2020 The Authors. Published by Elsevier B.V. All rights reserved.)
Databáze: MEDLINE
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