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Titel: Crystalline sponge affinity screening : A fast tool for soaking condition optimization without the need of X-ray diffraction analysis
VerfasserIn: Rosenberger, Lara
von Essen, Carolina
Khutia, Anupam
Kühn, Clemens
Georgi, Katrin
Hirsch, Anna K. H.
Hartmann, Rolf W.
Badolo, Lassina
Sprache: Englisch
Titel: European Journal of Pharmaceutical Sciences
Bandnummer: 164
Verlag/Plattform: Elsevier
Erscheinungsjahr: 2021
Freie Schlagwörter: Crystalline sponge method
Metal organic framework
Host-guest chemistry
Single-crystal X-ray diffraction
Affinity screening
LC-MS2
DDC-Sachgruppe: 500 Naturwissenschaften
Dokumenttyp: Journalartikel / Zeitschriftenartikel
Abstract: Structural elucidation of small molecules only available in low quantity (nanogram) is one of the big advantages of the crystalline sponge method. The optimization of various soaking parameters is crucial for effective analyte absorption and repetitive positioning in the pores of the crystal. Time-consuming X-ray diffraction measurements are necessary for data collection and confirmation of successful guest inclusion. In this work, we report a screening method to select optimal soaking conditions without the need of single-crystal X-ray diffraction analysis for individual compounds and mixtures. 14 substances were chosen as test compounds. Parallel guest soaking of individual compounds and mixtures was conducted using various soaking conditions. After evaporation of solvent, excessive material was removed, and guest molecules released through dissolution of the framework. Liquid chromatography-tandem mass spectrometry allowed the estimation of analyte trapped in the pores and the selection of optimal soaking condition dependent on the highest amount of analyte to crystal size (affinity factor). The tool allowed subsequent crystallographic analysis of ten compounds with minimal experiment time. Additionally, a study to examine the lower limit of detection of the crystalline sponge method was conducted. Determination of two target analytes was possible using only 5 ng of sample. Our study shows the potential of an affinity screening to prioritize soaking parameters by estimation of the guest concentration in a single crystal for one or multiple target compounds within a short period of time.
DOI der Erstveröffentlichung: 10.1016/j.ejps.2021.105884
URL der Erstveröffentlichung: https://www.sciencedirect.com/science/article/abs/pii/S0928098721001858
Link zu diesem Datensatz: urn:nbn:de:bsz:291--ds-390759
hdl:20.500.11880/35235
http://dx.doi.org/10.22028/D291-39075
ISSN: 0928-0987
Datum des Eintrags: 16-Feb-2023
Fakultät: NT - Naturwissenschaftlich- Technische Fakultät
Fachrichtung: NT - Pharmazie
Professur: NT - Prof. Dr. Rolf W. Hartmann
NT - Prof. Dr. Anna Hirsch
Sammlung:SciDok - Der Wissenschaftsserver der Universität des Saarlandes

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