Fast real-time monitoring of entacapone crystallization and characterization of polymorphs via Raman spectroscopy, statistics and SWAXS
Crystallization of the drug entacapone from binary solvent mixtures was monitored in situ using a Raman optical probe. The recorded Raman spectra and statistical analysis, which included the principal components method and indirect hard modeling made it possible to estimate the starting point of cry...
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| Format: | Article |
| Language: | English |
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Sciendo
2014-03-01
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| Series: | Acta Pharmaceutica |
| Subjects: | |
| Online Access: | http://www.degruyter.com/view/j/acph.2014.64.issue-1/acph-2014-0009/acph-2014-0009.xml?format=INT |
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| author | Jednačak Tomislav Hodzic Aden Scheibelhofer Otto Marijan Marijan Khinast Johannes G. Novak Predrag |
| author_facet | Jednačak Tomislav Hodzic Aden Scheibelhofer Otto Marijan Marijan Khinast Johannes G. Novak Predrag |
| author_sort | Jednačak Tomislav |
| collection | DOAJ |
| description | Crystallization of the drug entacapone from binary solvent mixtures was monitored in situ using a Raman optical probe. The recorded Raman spectra and statistical analysis, which included the principal components method and indirect hard modeling made it possible to estimate the starting point of crystallization, to assess crystallization temperatures and to provide information on the polymorphic content of the mixture. It was established that crystallization temperatures were proportional to the volume content of the solvent in mixtures. The samples were also evaluated off-line via Raman spectroscopy and SWAXS. The collected data showed the presence of forms b and g in all solvent mixtures. In a toluene/methanol 30:70 mixture, in addition to forms b and g, at least one of the forms A, D or a was also indicated by SWAXS. The results have shown that the presence of a particular polymorph is strongly dependent on the nature and portion of the solvent in the binary solvent mixture. |
| format | Article |
| id | doaj-art-8fa176e675d04303b754a90dbcfbdaf7 |
| institution | Kabale University |
| issn | 1330-0075 1846-9558 |
| language | English |
| publishDate | 2014-03-01 |
| publisher | Sciendo |
| record_format | Article |
| series | Acta Pharmaceutica |
| spelling | doaj-art-8fa176e675d04303b754a90dbcfbdaf72025-02-02T22:58:52ZengSciendoActa Pharmaceutica1330-00751846-95582014-03-0164111310.2478/acph-2014-0009acph-2014-0009Fast real-time monitoring of entacapone crystallization and characterization of polymorphs via Raman spectroscopy, statistics and SWAXSJednačak Tomislav0Hodzic Aden1Scheibelhofer Otto2Marijan Marijan3Khinast Johannes G.4Novak Predrag5University of Zagreb, Faculty of Science, Department of Chemistry HR-10000 Zagreb, CroatiaResearch Center Pharmaceutical Engineering GmbH, A-8010 Graz, AustriaResearch Center Pharmaceutical Engineering GmbH, A-8010 Graz, AustriaUniversity of Zagreb, Faculty of Science, Department of Chemistry HR-10000 Zagreb, CroatiaResearch Center Pharmaceutical Engineering GmbH, A-8010 Graz, Austria / Institute for Particle and Process Technology, A-8010 Graz, AustriaUniversity of Zagreb, Faculty of Science, Department of Chemistry HR-10000 Zagreb, CroatiaCrystallization of the drug entacapone from binary solvent mixtures was monitored in situ using a Raman optical probe. The recorded Raman spectra and statistical analysis, which included the principal components method and indirect hard modeling made it possible to estimate the starting point of crystallization, to assess crystallization temperatures and to provide information on the polymorphic content of the mixture. It was established that crystallization temperatures were proportional to the volume content of the solvent in mixtures. The samples were also evaluated off-line via Raman spectroscopy and SWAXS. The collected data showed the presence of forms b and g in all solvent mixtures. In a toluene/methanol 30:70 mixture, in addition to forms b and g, at least one of the forms A, D or a was also indicated by SWAXS. The results have shown that the presence of a particular polymorph is strongly dependent on the nature and portion of the solvent in the binary solvent mixture.http://www.degruyter.com/view/j/acph.2014.64.issue-1/acph-2014-0009/acph-2014-0009.xml?format=INTentacaponein-line crystallization monitoringmultivariate analysispolymorphismRaman spectroscopySWAXS |
| spellingShingle | Jednačak Tomislav Hodzic Aden Scheibelhofer Otto Marijan Marijan Khinast Johannes G. Novak Predrag Fast real-time monitoring of entacapone crystallization and characterization of polymorphs via Raman spectroscopy, statistics and SWAXS Acta Pharmaceutica entacapone in-line crystallization monitoring multivariate analysis polymorphism Raman spectroscopy SWAXS |
| title | Fast real-time monitoring of entacapone crystallization and characterization of polymorphs via Raman spectroscopy, statistics and SWAXS |
| title_full | Fast real-time monitoring of entacapone crystallization and characterization of polymorphs via Raman spectroscopy, statistics and SWAXS |
| title_fullStr | Fast real-time monitoring of entacapone crystallization and characterization of polymorphs via Raman spectroscopy, statistics and SWAXS |
| title_full_unstemmed | Fast real-time monitoring of entacapone crystallization and characterization of polymorphs via Raman spectroscopy, statistics and SWAXS |
| title_short | Fast real-time monitoring of entacapone crystallization and characterization of polymorphs via Raman spectroscopy, statistics and SWAXS |
| title_sort | fast real time monitoring of entacapone crystallization and characterization of polymorphs via raman spectroscopy statistics and swaxs |
| topic | entacapone in-line crystallization monitoring multivariate analysis polymorphism Raman spectroscopy SWAXS |
| url | http://www.degruyter.com/view/j/acph.2014.64.issue-1/acph-2014-0009/acph-2014-0009.xml?format=INT |
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