Bitte benutzen Sie diese Referenz, um auf diese Ressource zu verweisen:
Volltext verfügbar? / Dokumentlieferung
doi:10.22028/D291-39075
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 |
Dateien zu diesem Datensatz:
Es gibt keine Dateien zu dieser Ressource.
Alle Ressourcen in diesem Repository sind urheberrechtlich geschützt.