Title Određivanje elementarnih onečišćenja u fosamprenavir kalciju ICP tehnikom Title (english) Determination of elemental impurities in fosamprenavir calcium by ICP technique Author Maja Halužan Mentor Tomislav Bolanča (mentor)Committee member Tomislav Bolanča (predsjednik povjerenstva)Committee member Šime Ukić (član povjerenstva)Committee member Dajana Kučić Grgić (član povjerenstva)Granter University of Zagreb Defense date and country 2019-07-10, Croatia Scientific / art field, NATURAL SCIENCES Abstract Diplomski rad opisuje razvoj analitičke metode za određivanje elementnih onečišćenja u djelatnoj farmaceutskoj supstanciji fosamprenavir kalciju. Onečišćenja u lijekovima mogu biti organskog ili anorganskog porijekla i potjecati od različitih izvora, te potencijalno mogu ugroziti djelotvornost lijekova ili utjecati na sigurnost primjene. U radu je dan detaljan pregled važnosti kontrole anorganskih onečišćenja, te su opisane prednosti primjene ICP-MS tehnike u usklađivanju sa sve strožim
... More farmakopejskim zahtjevima. ICP-MS je zbog jednostavnosti masenih spektara brza tehnika za automatsku kvalitativnu, polukvantitativnu ili kvantitativnu elementarnu analizu u različitim uzorcima. Spektrogrami su jednostavni jer pikovi nastaju od jednostruko nabijenih iona bez obzira na složenost matrice. U ICP-MS spojevi se atomiziraju i ioniziraju bez obzira na kemijsku strukturu u kojoj je inkorporiran element od interesa. Interferencije obično nastaju zbog formiranja višestruko nabijenih iona, oksida ili poliatomskih izobaričnih interferencija formiranih u plazmi, te je u radu dan osvrt na utjecaj poliatomnih interferencija kao i način njihovog uklanjanja (upotreba kolizijskog plina, odabir odgovarajućih izotopa analita). Validacija metode neophodna je da bi se potvrdilo da je ona prikladna za namijenjenu svrhu. U radu je dan opis i način ispitivanja izvedbenih značajki kojima se metoda validira. Tijekom elementarne analize dobiven je lažno pozitivan odziv osmija (problem nastajanja toksičnog osmijevog tetraoksida u oksidirajućem mediju pri povišenoj temperaturi). Opisan je način stabilizacije osmija nužan za razvoj dobre metode za njegovo određivanje. Razvijene su metode za određivanje Ag, As, Au, Ba, Cd, Co, Cr, Cu, Hg, Ir, Li, Mo, Ni, Pb, Pd, Pt, Rh, Ru, Sb, Se, Sn, Tl i V te za određivanje osmija u fosamprenavir kalciju. Ispitane su glavne izvedbene značajke za svaku metodu (linearnost, granica kvantifikacije, selektivnost, točnost i preciznost te otpornost) uz predložene kriterije prihvatljivosti. Pokazalo se da svaka od razvijenih metoda zadovoljava sve kriterije za sve ispitane izvedbene značajke, te su obje metode validirane. Less Abstract (english) The thesis describes the development of an analytical method for determination of elemental impurities in the active pharmaceutical ingredient fosamprenavir calcium. Elemental impurities in drug products may be of organic or inorganic origin and come from different sources, and may potentially endanger drug efficacy or affect the safety of use. This paper gives a detailed overview of the importance of controlling the presence of inorganic impurities and describes the benefits of using
... More ICP-MS techniques in aligning with increasingly stringent pharmacopoeia requirements. For ease of mass spectrum, ICP-MS is a fast technique for automatic qualitative, semiquantitative or quantitative elemental analysis in various samples. The mass specrta obtained are simple because the peaks are made of single-charged ions, regardless of the complexity of the matrix. In ICP-MS compounds are atomized and ionized regardless of the chemical structure in which an element of interest is incorporated. The interferences are usually due to the formation of multiple charged ions, oxides or polyatomic isobaric interferences formed in the plasma, and an overview of the effects of polyatomic interference as well as the method of their removal (collagen gas utilization, selection of appropriate isotopes of the analyte) is given. Validation of the method is necessary to confirm that it is suitable for the intended purpose. This paper presents a description of the performance tests that are necessary to validate the method. During the multielement analysis, a false positive osmium response was obtained (the problem of formation of toxic osmium tetroxide in the oxidising medium at elevated temperature). The method for stabilization of osmium necessary for the development of a good method for its determination is described. The method for the determination of Ag, As, Au, Ba, Cd, Co, Cr, Cu, Hg, Ir, Li, Mo, Ni, Pb, Pd, Pt, Rh, Ru, Sb, Se, Sn, Tl V in fosamprenavir calcium and the ethod for determination of osmium in fosamprenavir calcium were developed. The main performance features for each (linearity, quantification limit, selectivity, accuracy, precision and robustness) were tested with the proposed eligibility criteria. It has been shown that each of the developed methods meets all the criteria for all tested performance features and the methods were validated. Less Keywords
fosamprenavir
ICH
elementarna onečišćenja
induktivno spregnuta plazma
ICP-MS
validacija metode
Keywords (english)
fosamprenavir
ICH
elemental impurities
inductively coupled plasma
ICPMS
method validation
Language croatian URN:NBN urn:nbn:hr:149:977848 Study programme Title: Applied Chemistry - Graduate study; specializations in: Environmental chemistry and green technologies, Advanced materials and technologies, Applied organic chemistry Type of resource Text File origin Born digital Access conditions Open access Terms of use Created on 2022-02-21 13:16:34
