We found a match
Your institution may have rights to this item. Sign in to continue.
- Title
Chemometrically Assisted Optimization of Pregabalin Fluorescent Derivatization Reaction with a Novel Xanthone Analogue and Validation of the Method for the Determination of Pregabalin in Bulk via a Plate Reader.
- Authors
Kritikos, Nikolaos; Iliou, Aikaterini; Kalampaliki, Amalia D.; Gikas, Evangelos; Kostakis, Ioannis K.; Michel, Benoît Y.; Dotsikas, Yannis
- Abstract
Quantitation of chromophore-free analytes is always a challenge. To this purpose, derivatization of the analyte constitutes a common strategy, leading to a product with a strong signal. In the current study, a novel xanthone analogue was utilized for the first time for the derivatization of pregabalin, a model analyte with a primary amine moiety that lacks a chromophore. The fact that only the xanthene-based derivative, formed after the derivatization reaction fluoresces, enables avoiding its chromatographic separation from the reagent and thus reducing the analysis time of a series of samples in 1–2 min via a plate reader. The reaction conditions were optimized via a central composite design (CCD), with fluorescence signal as the measure of the yield. The following factors that affect the derivatization reaction were chosen: (a) temperature, (b) reaction time, and (c) triethylamine solution volume used to drive the reaction to completion. After the identification of the optimal conditions, the method was validated according to ICH guidelines, using a fluorescence plate reader for signal measurement (λex = 540, λem = 615 nm). Finally, the newly developed high-throughput method was applied to the determination of drug content in pregabalin bulk.
- Subjects
XANTHONE; DERIVATIZATION; TIME series analysis; PREGABALIN
- Publication
Molecules, 2022, Vol 27, Issue 6, p1954
- ISSN
1420-3049
- Publication type
Article
- DOI
10.3390/molecules27061954