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http://hdl.handle.net/1942/39285
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DC Field | Value | Language |
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dc.contributor.author | PROSTKO, Piotr | - |
dc.contributor.author | Pikkemaat, Jeroen | - |
dc.contributor.author | Selter, Philipp | - |
dc.contributor.author | Lukaschek, Michail | - |
dc.contributor.author | Wechselberger, Rainer | - |
dc.contributor.author | KHAMIAKOVA, Tatsiana | - |
dc.contributor.author | VALKENBORG, Dirk | - |
dc.date.accessioned | 2023-01-23T12:18:04Z | - |
dc.date.available | 2023-01-23T12:18:04Z | - |
dc.date.issued | 2022 | - |
dc.date.submitted | 2023-01-12T15:02:59Z | - |
dc.identifier.citation | Metabolites, 12 (12) (Art N° 1248) | - |
dc.identifier.uri | http://hdl.handle.net/1942/39285 | - |
dc.description.abstract | Bioavailability and chemical stability are important characteristics of drug products that are strongly affected by the solid-state structure of the active pharmaceutical ingredient (API). In pharmaceutical development and quality control activities, solid-state NMR (ssNMR) has proved to be an excellent tool for the detection and accurate quantification of undesired solid-state forms. To obtain correct quantitative outcomes, the resulting spectrum of an analytical sample should be deconvoluted into the individual spectra of the pure components. However, the ssNMR deconvolution is particularly challenging due to the following: the relatively large line widths that may lead to severe peak overlap, multiple spinning sidebands as a result of applying Magic Angle Spinning (MAS), and highly irregular peak shapes commonly observed in mixture spectra. To address these challenges, we created a tailored and automated deconvolution approach of ssNMR mixture spectra that involves a linear combination modelling (LCM) of previously acquired reference spectra of pure solid-state components. For optimal model performance, the template and mixture spectra should be acquired under the same conditions and experimental settings. In addition to the parameters controlling the contributions of the components in the mixture, the proposed model includes terms for spectral processing such as phase correction and horizontal shifting that are all jointly estimated via a non-linear, constrained optimisation algorithm. Finally, our novel procedure has been implemented in a fully functional and user-friendly R Shiny webtool (hence no local R installation required) that offers interactive data visualisations, manual adjustments to the automated deconvolution results, and the traceability and reproducibility of analyses. | - |
dc.description.sponsorship | This study was supported by the Special Research Fund (BOF19DOC33) and own means of Hasselt University. P.P. has a research grant from Janssen Pharmaceutical Companies of Johnson and Johnson. The authors wish to thank Nicolas Sauwen for finding a solution for minimising the frowning effect occurring after signal apodization, valuable comments on methodological aspects of our deconvolution method, and overall support with the Shiny app development. | - |
dc.language.iso | en | - |
dc.publisher | MDPI | - |
dc.rights | © 2022 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). | - |
dc.subject.other | solid-state NMR | - |
dc.subject.other | deconvolution | - |
dc.subject.other | quantification | - |
dc.subject.other | pharmaceutical development | - |
dc.subject.other | quality control | - |
dc.subject.other | software | - |
dc.subject.other | R Shiny | - |
dc.subject.other | non-linear optimisation | - |
dc.title | R Shiny App for the Automated Deconvolution of NMR Spectra to Quantify the Solid-State Forms of Pharmaceutical Mixtures | - |
dc.type | Journal Contribution | - |
dc.identifier.issue | 12 | - |
dc.identifier.volume | 12 | - |
local.bibliographicCitation.jcat | A1 | - |
dc.description.notes | Valkenborg, D (corresponding author), UHasselt Hasselt Univ, Data Sci Inst, Agoralaan 1, B-E3590 Diepenbeek, Belgium.; Valkenborg, D (corresponding author), Interuniv Inst Biostat & Stat Bioinformat I BioSta, Agoralaan 1, B-E3590 Diepenbeek, Belgium. | - |
dc.description.notes | dirk.valkenborg@uhasselt.be | - |
local.publisher.place | ST ALBAN-ANLAGE 66, CH-4052 BASEL, SWITZERLAND | - |
local.type.refereed | Refereed | - |
local.type.specified | Article | - |
local.bibliographicCitation.artnr | 1248 | - |
dc.identifier.doi | 10.3390/metabo12121248 | - |
dc.identifier.pmid | 36557287 | - |
dc.identifier.isi | 000902841000001 | - |
local.provider.type | wosris | - |
local.description.affiliation | [Prostko, Piotr; Valkenborg, Dirk] UHasselt Hasselt Univ, Data Sci Inst, Agoralaan 1, B-E3590 Diepenbeek, Belgium. | - |
local.description.affiliation | [Prostko, Piotr; Valkenborg, Dirk] Interuniv Inst Biostat & Stat Bioinformat I BioSta, Agoralaan 1, B-E3590 Diepenbeek, Belgium. | - |
local.description.affiliation | [Pikkemaat, Jeroen; Selter, Philipp; Lukaschek, Michail; Wechselberger, Rainer] Dept Analyt Dev, Janssen Pharmaceut, Turnhoutseweg 30, B-E2340 Beerse, Belgium. | - |
local.description.affiliation | [Khamiakova, Tatsiana] Janssen Pharmaceut, Mfg & Appl Stat, Turnhoutseweg 30, B-E2340 Beerse, Belgium. | - |
local.uhasselt.international | no | - |
item.contributor | PROSTKO, Piotr | - |
item.contributor | Pikkemaat, Jeroen | - |
item.contributor | Selter, Philipp | - |
item.contributor | Lukaschek, Michail | - |
item.contributor | Wechselberger, Rainer | - |
item.contributor | KHAMIAKOVA, Tatsiana | - |
item.contributor | VALKENBORG, Dirk | - |
item.accessRights | Open Access | - |
item.fullcitation | PROSTKO, Piotr; Pikkemaat, Jeroen; Selter, Philipp; Lukaschek, Michail; Wechselberger, Rainer; KHAMIAKOVA, Tatsiana & VALKENBORG, Dirk (2022) R Shiny App for the Automated Deconvolution of NMR Spectra to Quantify the Solid-State Forms of Pharmaceutical Mixtures. In: Metabolites, 12 (12) (Art N° 1248). | - |
item.fulltext | With Fulltext | - |
crisitem.journal.issn | 2218-1989 | - |
crisitem.journal.eissn | 2218-1989 | - |
Appears in Collections: | Research publications |
Files in This Item:
File | Description | Size | Format | |
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R Shiny App for the Automated Deconvolution of NMR Spectra to Quantify the Solid-State Forms of Pharmaceutical Mixtures.pdf | Published version | 2.21 MB | Adobe PDF | View/Open |
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