Razvoj metode tekućinske kromatografije ultravisoke djelotvornosti za određivanje onečišćenja u ceritinibu

master's thesis

• Title (english): Development of ultra performance liquid chromatographic method for determination of impurities in the ceritinib
• Author: Borna Mašić
• Mentor: Nives Galić (mentor)
• Committee member: Nives Galić (predsjednik povjerenstva)
• Committee member: Željka Soldin (član povjerenstva)
• Committee member: Morana Dulić (član povjerenstva)
• Committee member: Snežana Miljanić (član povjerenstva)
• Granter: University of Zagreb; Faculty of Science; (Department of Chemistry); Zagreb
• Defense date and country: 2018-09-28, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

U okviru diplomskog rada razvijena je metoda za kvantitativno određivanje onečišćenja ceritiniba primjenom kromatografije ultravisoke djelotvornosti uz korištenje programa Drylab za optimizaciju parametara. Konačna metoda prilagođena je vezanom sustavu kromatografije visoke djelotovornosti spregnutom sa spektrometrijom masa kako bi se potvrdila masa onečišćenja. Pri razvoju metode proveden je niz eksperimenata na dvije različite kolone, C18 i BEH Phenyl, pri temperaturama od 30 °C i 60 °C, tri pH-vrijednosti 2,0; 4,0; 6,0 te dva različita gradijenta u trajanju 13 i 25 minute. Apsorpcija je praćena pri valnim duljinama od 220 nm, 240 nm i 270 nm. Uz navedene parametre također su korištene različite kombinacije vodenih i organskih faza. Rezultati eksperimenata su analizirani uz pomoć DryLab programa i prilagođeni uvjetima realnog sustava kako bi se dobili konačni uvjeti metode. Odabrana kolona je BEH Phenyl, temperatura 55 °C, gradijent u trajanju 17 minuta, valna duljina 210 nm, pufer KH2PO4 pH vrijednosti 4,3. Kao organska faza odabran je acetonitril.

Abstract (english)

In this diploma thesis, a quantitative method for determination of ceritinib impurities by ultra performance liquid chromatography using Drylab program for parameter optimization was developed. The method was adapted for use in high-performance chromatography systems coupled with mass spectrometry to confirm the mass of the aforementioned impurities. The process of parameter optimization was performed via series of experiments in which two types of columns were used, C18 and BEH Phenyl, at temperatures of 30 °C and 60 °C, three pH values 2.0; 4.0; 6.0; at two different gradients in duration of 13 and 25 minutes. Chromatograms were recorded at wavelengths of 220 nm, 240 nm and 270 nm. Different combinations of organic and water phases were also used. The results of the experiments were analyzed with DryLab software and the final conditions of the method were established: BEH Phenyl column, system temperature of 55 °C, 17 minute gradient, a wavelength of 210 nm, buffer KH2PO4 pH value 4.3. Acetonitrile was used as the organic phase.

• Keywords: ceritinib; DryLab; onečišćenja; razvoj metode; UHPLC-MS
• Keywords (english): ceritinib; DryLab; impurities; method development; UHPLC-MS
• Language: croatian
• URN:NBN: urn:nbn:hr:217:853147
• Study programme: Title: 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 resource: Text
• File origin: Born digital
• Access conditions: Open access; Embargo expiration date: 2020-09-28
• Created on: 2018-11-26 10:48:55