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dc.contributor.authorLi, Boyan
dc.contributor.authorCalvet, Amandine
dc.contributor.authorRyder, Alan G.
dc.contributor.authorCasamayou-Boucau, Yannick
dc.contributor.authorMorris, Cheryl
dc.date.accessioned2016-01-30T10:02:31Z
dc.date.issued2015-02-23
dc.identifier.citationLi, B.; Calvet, A.; Casamayou-Boucau, Y.; Morris, C.; Ryder, A.G. (2015) 'Low-content quantification in powders using Raman spectroscopy: a facile chemometric approach to sub 0.1% limits of detection'. Analytical Chemistry, 87 (6):3419-3428.en_IE
dc.identifier.issn1520-6882
dc.identifier.urihttp://hdl.handle.net/10379/5508
dc.description.abstractA robust and accurate analytical methodology for low-content (<0.1%) quantification in the solid-state using Raman spectroscopy, sub-sampling, and chemometrics was demonstrated using a piracetam–proline model. The method involved a 5-step process: collection of relatively large number of spectra (8410) from each sample by Raman mapping, meticulous data pretreatment to remove spectral artefacts, use of a 0–100% concentration range partial least squares (PLS) regression model to estimate concentration at each pixel, use of a more-accurate, reduced concentration range PLS model to accurately calculate analyte concentration at each pixel, and finally statistical analysis of all 8000+ concentration predictions to produce an accurate overall sample concentration. The relative prediction accuracy was ~2.4% for a 0.05~1.0% concentration range and the limit of detection was comparable to high performance liquid chromatography (0.03% versus 0.041%). For data pretreatment, we developed a unique cosmic ray removal method and used an automated baseline correction method, neither of which required subjective user intervention and thus were fully automatable. The method is applicable to systems, which cannot be easily analyzed chromatographically such as hydrate, polymorph, or solvate contamination.en_IE
dc.description.sponsorshipResearch undertaken as part of the Synthesis and Solid State Pharmaceutical Centre, funded by Science Foundation Ireland and industry partners, and Enterprise Ireland (Grant No: TC- 2012-5106).en_IE
dc.formatapplication/pdfen_IE
dc.language.isoenen_IE
dc.publisherAmerican Chemical Societyen_IE
dc.relation.ispartofAnalytical Chemistryen
dc.rightsAttribution-NonCommercial-NoDerivs 3.0 Ireland
dc.rights.urihttps://creativecommons.org/licenses/by-nc-nd/3.0/ie/
dc.subjectRaman spectroscopyen_IE
dc.subjectChemometricsen_IE
dc.subjectQuantificationen_IE
dc.subjectLow contenten_IE
dc.subjectAPIen_IE
dc.subjectChemistryen_IE
dc.titleLow-content quantification in powders using Raman spectroscopy: a facile chemometric approach to sub 0.1% limits of detection.en_IE
dc.typeArticleen_IE
dc.date.updated2015-12-22T16:40:34Z
dc.identifier.doi10.1021/ac504776m
dc.local.publishedsourcehttp://pubs.acs.org/doi/abs/10.1021/ac504776men_IE
dc.description.peer-reviewedpeer-reviewed
dc.contributor.funder|~|1267883|~|1267869|~|
dc.description.embargo2016-02-23
dc.internal.rssid8415505
dc.local.contactAlan Ryder, School Of Chemistry, Room 213, Arts/Science Building, Nui Galway. 2943 Email: alan.ryder@nuigalway.ie
dc.local.copyrightcheckedNo
dc.local.versionACCEPTED
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