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doctoral thesis
Kvantitativno praćenje reakcije sinteze i kristalizacije omeprazola Ramanovom spektroskopijom in-line
Zagreb: University of Zagreb, Faculty of Science, 2017. urn:nbn:hr:217:702684
Šahnić, Damir
University of Zagreb
Faculty of Science
Department of Chemistry

Institutional repository: Repository of the Faculty of Science

Cite this document

Šahnić, D. (2017). Kvantitativno praćenje reakcije sinteze i kristalizacije omeprazola Ramanovom spektroskopijom in-line (Doctoral thesis). Zagreb: University of Zagreb, Faculty of Science. Retrieved from https://urn.nsk.hr/urn:nbn:hr:217:702684

Šahnić, Damir. "Kvantitativno praćenje reakcije sinteze i kristalizacije omeprazola Ramanovom spektroskopijom in-line." Doctoral thesis, University of Zagreb, Faculty of Science, 2017. https://urn.nsk.hr/urn:nbn:hr:217:702684

Šahnić, Damir. "Kvantitativno praćenje reakcije sinteze i kristalizacije omeprazola Ramanovom spektroskopijom in-line." Doctoral thesis, University of Zagreb, Faculty of Science, 2017. https://urn.nsk.hr/urn:nbn:hr:217:702684

Šahnić, D. (2017). 'Kvantitativno praćenje reakcije sinteze i kristalizacije omeprazola Ramanovom spektroskopijom in-line', Doctoral thesis, University of Zagreb, Faculty of Science, accessed 25 November 2024, https://urn.nsk.hr/urn:nbn:hr:217:702684

Šahnić D. Kvantitativno praćenje reakcije sinteze i kristalizacije omeprazola Ramanovom spektroskopijom in-line [Doctoral thesis]. Zagreb: University of Zagreb, Faculty of Science; 2017 [cited 2024 November 25] Available at: https://urn.nsk.hr/urn:nbn:hr:217:702684

D. Šahnić, "Kvantitativno praćenje reakcije sinteze i kristalizacije omeprazola Ramanovom spektroskopijom in-line", Doctoral thesis, University of Zagreb, Faculty of Science, Zagreb, 2017. Available at: https://urn.nsk.hr/urn:nbn:hr:217:702684

Metadata
TitleKvantitativno praćenje reakcije sinteze i kristalizacije omeprazola Ramanovom spektroskopijom in-line
Title (english)Quantitative monitoring of omeprazole synthesis reaction and crystallization by in-line Raman spectroscopy
AuthorDamir Šahnić
MentorPredrag Novak (mentor)
Committee memberSnežana Miljanić (predsjednik povjerenstva)
Committee memberPredrag Novak (član povjerenstva)
Committee memberErnest Meštrović (član povjerenstva)
GranterUniversity of Zagreb
Faculty of Science
(Department of Chemistry)
Zagreb
Defense date and country2017-09-18, Croatia
Scientific / art field,
discipline and subdiscipline		NATURAL SCIENCES
Chemistry
Universal decimal classification
(UDC)		54 - Chemistry. Crystallography. Mineralogy
Abstract
Opisan je razvoj kvantitativne metode praćenja reakcije sinteze i kristalizacije aktivne farmaceutske supstance, omeprazola in situ, Ramanovom spektroskopijom in-line. Praćenje in-line provedeno je uporabom disperzivnog Ramanovog instrumenta. Prije praćenja reakcije, reakcijske komponente su sintetizirane i okarakterizirane off-line, pomoću Ramanove spektroskopije i spektroskopije NMR. Spektroskopska mjerenja i komplementarne kromatografske analize, korištene za razvoj kalibracijskog modela, prikupljene su iz seta eksperimenata provedenih u mjerilu od jedne litre. Temeljem podataka prikupljenih tijekom kalibracijskih eksperimenata, razvijen je kemometrijski model metodom parcijalnih projekcija najmanjih kvadrata za sve tri reakcijske komponente, koji izračunava postotni udio svake komponente u reakcijskoj smjesi. Metoda je uspješno primijenjena u praćenju tijeka reakcije eksperimenta u kilo-laboratorijskom mjerilu. Kristalizacija omeprazola praćena je semikvantitativno metodom analize glavnih komponenata i multivarijatnom rezolucijom krivulja.
Abstract (english)
The development of a quantitative in-line Raman spectroscopic method for in situ monitoring of the active pharmaceutical ingredient, omeprazole synthesis reaction and crystallization is described. In-line monitoring was performed using a dispersive Raman instrument. Prior to reaction monitoring, the reaction components were characterized off-line by means of Raman and NMR spectroscopy. The spectroscopic measurements and the complementary chromatographic analyses, used in the calibration model development, were gathered from a set of experiments, performed at a one liter scale. Based on the data set obtained from the calibration experiments, a partial least square regression model was developed for all three reaction components, enabling the determination of the percentage of each component present in the reaction mixture. The model was successfully applied to monitor the reaction progress in a kilo-lab scale experiment. Omeprazole crystallization was monitored semi-quantitatively by means of principal component analysis and multivariate curve resolution methods.
Keywords
Keywords (english)
Languagecroatian
URN:NBNurn:nbn:hr:217:702684
Study programmeTitle: Doctoral study in chemistry
Study programme type: university
Study level: postgraduate
Academic / professional title: doktor/doktorica znanosti, područje prirodnih znanosti, polje kemija (doktor/doktorica znanosti, područje prirodnih znanosti, polje kemija)
Type of resourceText
Extent151 str. ; 30 cm
File originBorn digital
Access conditionsOpen access
Embargo expiration date: 2019-09-18
Terms of useLicence In copyright icon
Created on2017-10-30 17:25:54