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master's thesis
Razvoj metode tekućinske kromatografije ultravisoke djelotvornosti za analizu razgradnih produkata lijeka dasatiniba
Zagreb: University of Zagreb, Faculty of Science, 2017. urn:nbn:hr:217:128694
Šestan, Davor
University of Zagreb
Faculty of Science
Department of Chemistry

Institutional repository: Repository of the Faculty of Science

Cite this document

Šestan, D. (2017). Razvoj metode tekućinske kromatografije ultravisoke djelotvornosti za analizu razgradnih produkata lijeka dasatiniba (Master's thesis). Zagreb: University of Zagreb, Faculty of Science. Retrieved from https://urn.nsk.hr/urn:nbn:hr:217:128694

Šestan, Davor. "Razvoj metode tekućinske kromatografije ultravisoke djelotvornosti za analizu razgradnih produkata lijeka dasatiniba." Master's thesis, University of Zagreb, Faculty of Science, 2017. https://urn.nsk.hr/urn:nbn:hr:217:128694

Šestan, Davor. "Razvoj metode tekućinske kromatografije ultravisoke djelotvornosti za analizu razgradnih produkata lijeka dasatiniba." Master's thesis, University of Zagreb, Faculty of Science, 2017. https://urn.nsk.hr/urn:nbn:hr:217:128694

Šestan, D. (2017). 'Razvoj metode tekućinske kromatografije ultravisoke djelotvornosti za analizu razgradnih produkata lijeka dasatiniba', Master's thesis, University of Zagreb, Faculty of Science, accessed 20 November 2024, https://urn.nsk.hr/urn:nbn:hr:217:128694

Šestan D. Razvoj metode tekućinske kromatografije ultravisoke djelotvornosti za analizu razgradnih produkata lijeka dasatiniba [Master's thesis]. Zagreb: University of Zagreb, Faculty of Science; 2017 [cited 2024 November 20] Available at: https://urn.nsk.hr/urn:nbn:hr:217:128694

D. Šestan, "Razvoj metode tekućinske kromatografije ultravisoke djelotvornosti za analizu razgradnih produkata lijeka dasatiniba", Master's thesis, University of Zagreb, Faculty of Science, Zagreb, 2017. Available at: https://urn.nsk.hr/urn:nbn:hr:217:128694

Metadata
TitleRazvoj metode tekućinske kromatografije ultravisoke djelotvornosti za analizu razgradnih produkata lijeka dasatiniba
Title (english)Development of ultra performance liquid chromatographic method for the analysis of dasatinib degradation products
AuthorDavor Šestan
MentorNives Galić (mentor)
Committee memberNives Galić (predsjednik povjerenstva)
Committee memberVesna Petrović Peroković (član povjerenstva)
Committee memberŽeljka Soldin (član povjerenstva)
Committee memberPredrag Novak (član povjerenstva)
GranterUniversity of Zagreb
Faculty of Science
(Department of Chemistry)
Zagreb
Defense date and country2017-11-27, Croatia
Scientific / art field,
discipline and subdiscipline		NATURAL SCIENCES
Chemistry
Abstract
U ovom diplomskom radu razvijena je učinkovita i osjetljiva metoda tekućinske kromatografije ultravisoke djelotvornosti (UHPLC) za analizu onečišćenja i razgradnih produkta lijeka dasatiniba. DryLab je korišten za određivanje optimalnih uvjeta temperature, vremena gradijentnog eluiranja i sastava pokretne faze kromatografskog odijeljivanja metodom UHPLC. Najprikladnija kolona bila je Acquity UPLC CSH Phenyl-Hexyl 1,7 μm; 2,1 mm  100 mm. Optimalni uvjeti su: temperatura kolone = 50 °C, pH pokretne faze = 2 (fosfatni pufer za UHPLC, mravlja kiselina za LC-MS/MS analizu) i ukupno vrijeme trajanja analize: 27,5 min. Forsirana ragradnja dasatiniba provedena je u kiselom i lužnatom mediju, uz prisutnost vodikovog peroksida te na povišenoj temperaturi. Za analizu razgradnih produkata korišten je vezani sustav LC-MS/MS. Na temelju MS i MS/MS spektara pretpostavljene su strukture razgradnih produkata i predložene odgovarajuće sheme fragmentiranja.
Abstract (english)
In this diploma thesis efficient ultra-high performance liquid chromatography (UHPLC) method for determination of impurities and degradation product of dasatinib was developed. DryLab software was used to determine the optimal conditions for UHPLC separation like temperature, time of gradient elution and composition of the mobile phase. The most efficient chromatographic column was Acquity UPLC CSH Phenyl-Hexyl 1,7 μm; 2,1 mm  100 mm. The optimal condition were: column temperature = 50 °C, pH of mobile phase = 2 (phosphate buffer for UHPLC and formic acid for LC-MS/MS analysis), and total time of analysis = 27.5 min. Forced degradation of dasatinib was performed in acid and basic conditions, upon addition of hydrogen peroxide, and on the elevated temperature. The LC-MS/MS system was used for the analysis of the degradation products. Based on the MS and MS/MS spectra, the stuctures of degradation products, as well as fragmentation shemes were proposed.
Keywords
Keywords (english)
Languagecroatian
URN:NBNurn:nbn:hr:217:128694
Study programmeTitle: Graduate university studies in chemistry; specializations in: Research programme
Course: Research programme
Study programme type: university
Study level: graduate
Academic / professional title: magistar/magistra kemije (magistar/magistra kemije)
Type of resourceText
File originBorn digital
Access conditionsOpen access
Embargo expiration date: 2019-12-01
Terms of useLicence In copyright icon
Created on2017-12-07 13:55:08