Razvoj i optimizacija metoda ekstrakcije za kromatografsku analizu farmaceutika u sedimentu

doctoral thesis

• Title (english): Extraction methods development and optimization for chromatographic analysis of pharmaceuticals in sediment
• Author: Dijana Cerić
• Mentor: Danijela Ašperger (mentor)
• Committee member: Dragana Mutavdžić Pavlović (predsjednik povjerenstva)
• Committee member: Tatjana Gazivoda Kraljević (član povjerenstva)
• Committee member: Miranda Sertić (član povjerenstva)
• Granter: University of Zagreb; Faculty of Chemical Engineering and Technology; Zagreb
• Defense date and country: 2018-03-19, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry; Analytic Chemistry
• Universal decimal classification (UDC): 54 - Chemistry. Crystallography. Mineralogy

Abstract

Farmaceutici su tvari koje se koriste u humanoj i veterinarskoj medicini te se ubrajaju u skupinu tzv. novih zagađivala. Pojavljivanje farmaceutika u okolišu još uvijek nije zakonski regulirano, dok određeni broj radova bilježi njihov štetan utjecaj na ljudsko zdravlje. Pregledom literaturnih podataka farmaceutici su određivani u različitim uzorcima iz okoliša poput vode, mulja, tla, gnojiva te nešto manje u sedimentu koji je isptivan u ovome radu. Sediment se ponaša kao potencijalni primatelj mnogih štetnih tvari, uključujući i farmaceutike koji mogu dospijeti do rezervoara pitkih voda ovisno o karakteristikama sedimenta. U ovome radu određivani su farmaceutici koji pripadaju različitim strukturnim grupama te je za njihovo izdvajanje iz kompleksnog uzorka sedimenta razvijeno i optimirano pet različitih metoda ekstrakcije: ekstrakcija mućkanjem, ultrazvučna ekstrakcija, mikrovalna ekstrakcija, ekstrakcija raspršenjem matice uzorka kroz čvrstu fazu te tlačna ekstrakcija otapalom. Izabrani farmaceutici su tilozin iz skupine makrolidnih antibiotika, albendazol, febantel i levamisol iz skupine antihelmintika, lidokain i prokain kao anestetici te hidrokortizon i deksametazon iz skupine glukokortikoida. Koncentracije farmaceutika ekstrahiranih iz uzorka sedimenta određene su tekućinskom kromatografijom uz detekciju detektorom s nizom dioda. Nakon provedene kromatografske analize sve metode su validirane te su određeni sljedeći optimalni parametri za pojedinu metodu ekstrakcije: masa sedimenta, otapalo, vrijeme kontakta sediment-otapalo, vrijeme trajanja ekstrakcije, broj okretaja te temperatura ekstrakcije (ekstrakcija mućkanjem); otapalo, vrijeme trajanja ekstrakcije, snaga i temperatura ultrazvučne kupelji (ultrazvučna ekstrakcija); otapalo, vrijeme trajanja ekstrakcije, temperatura, volumen otapala (mikrovalna ekstrakcija); sorbens, otapalo, volumen otapala, omjer mase sediment/sorbens (ekstrakcija raspršenjem matice uzorka kroz čvrstu fazu); otapalo (tlačna ekstrakcija otapalom).

Abstract (english)

Pharmaceuticals are substances that are used in human and veterinary practice and are socalled emerging contaminants. Their occurrence in the environment is still not law regulated, while certain number of published articles record their negative impact on human health. From the literature overview, pharmaceuticals were determined in different environment samples like water, sludge, soil, manure and little bit less in here examined sediment. Sediment acts like a potential receiver for many hazardous substances including pharmaceuticals who can be easily emitted to drinking water reservoirs depending on the sediment characteristics. In this work pharmaceuticals who belong to different structure groups were determined in sediment sample and following five extractions were developed and optimized: extraction by agitation, ultrasound solvent extraction, microwave assisted extraction, matrix solid phase dispersion and pressurized solvent extraction. Chosen pharmaceuticals were tylosine as macrolide antibiotic, albendazole, febantel and levamisole as antihelmintics, lidocaine and procaine as anesthetics and hydrocortisone and dexamethasone as glucocorticoids. Pharmaceutical concentrations extracted from sediment sample were determined by high performance liquid chromatography using diode array detector. After chromatographic analysis, all methods were validated and the following optimal parameters were determined for each extraction method: sediment mass, solvent, contact time between sediment and solvent, extraction duration, agitation frequency and extraction temperature (extraction by agitation); solvent, extraction duration, power and temperature of ultrasonic bath (ultrasonic extraction); solvent, extraction duration, temperature, solvent volume (microwave extraction); sorbent, solvent, solvent volume, sediment/sorbent mass ratio (matrix solid phase dispersion); solvent (pressurized solvent extraction).

• Keywords: ekstrakcija mućkanjem; ekstrakcija raspršenjem matice uzorka kroz čvrstu fazu; farmaceutici; mikrovalna ekstrakcija; sediment; tekućinska kromatografija visoke djelotvornosti; tlačna ekstrakcija otapalom; ultrazvučna ekstrakcija
• Keywords (english): extraction by agitation; matrix solid phase dispersion; pharmaceuticals; microwave assisted extraction; sediment; high performance liquid chromatography; pressurized solvent extraction; ultrasound solvent extraction
• Language: croatian
• URN:NBN: urn:nbn:hr:149:351447
• Promotion: 2018
• Study programme: Title: Engineering Chemistry - Doctoral Course; 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 resource: Text
• Extent: 273 str. ; 30 cm
• File origin: Born digital
• Access conditions: Closed access
• Created on: 2023-08-30 12:35:12