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U ovom diplomskom radu uspješno su razvijene metode za određivanje sadržaja i onečišćenja febantela/pirantela/prazikvantela te albendazola/levamisola po principu kvalitete ugrađene u dizajn (QbD). Forsirana razgradnja provedena je na temeljnoj standardnoj otopini pojedinog anthelmintika kako bi se vidjela potencijalna onečišćenja. Ispitana je osjetljivost anthelmintika na temperaturu, oksidans, kiselinu, lužinu i svjetlost (pirantel). Nakon što su definirani uvjeti kojima se postiže 10-30% razgradnih produkata forsirana razgradnja je provedena prema najblažim uvjetima na otopinama febantela/pirantela/prazikvantela i albendazola/levamisola kako bi se procjenila učinkovitost razvijenih metoda. Metode su razvijene na BEH C18 koloni (100 x 2,1 nm, 1,7 μm) na tekućinskom kromatografu ultra visoke djelotvornosti. Optimalni pH za odjeljivanje sastavnica uzorka dobiven je programskim paketom Marvin Benas, a metode su razvijene koristeći programski paket DryLab koji na temelju unesenih podataka stvara virtualne kromatograme i predviđa kromatografske parametre pojedine sastavnice uzorka. Trajanje metode za određivanje sadržaja febantela/pirantela/prazikvantela je 10 min, a za određivanje onečišćenja 19 min, dok je za određivanje sadržaja albendazola/levamisola potrebno 7 min, a za određivanje onečišćenja 9 min. The aim of this study was to develop UPLC method for assay and impurities determination of febantel/praziquantel/pyrantel and albendazole/levamisole using quality by design approach (QbD). Stock solutions were exposed to the influence of temperature, oxidizing agent, acid, base and light (pyrantel) in order to achieve 10-30% degradation products so the potential impurities could be detected. After defining the forced degradation conditions, febantel/pyrantel/praziquantel solution and albendazole/levamisole solution were exposed to the mildest conditions. Based on the collected results, efficacy of separating the components using developed methods was evaluated. Methods were successfully developed using BEH C18 column (100 x 2,1 nm, 1,7 μm) on ultra-performance liquid chromatograph. Optimal pH for separating the components was determined using Marvin Beans software, while methods were developed using DryLab software. Based on the input data, DryLab creates virtual chromatograms and predicts chromatographic parameters for each component. Duration of method for assay determination of febantel/pyrantel/praziquantel is 10 min, while method for impurities determination lasts 19 min. Method for assay determination of albendazole/levamisole lasts 7 min, while duration of method for impurities determination lasts 9 min. |
