Title Određivanje ksenobiotika u aktivnom mulju Title (english) Determination of xenobiotics in active sludge Author Ivana Mađor-Božinović Mentor Danijela Ašperger (mentor)Committee member Danijela Ašperger (predsjednik povjerenstva)Committee member Davor Dolar (član povjerenstva)Committee member Dragana Vuk (član povjerenstva)Granter University of Zagreb Defense date and country 2019-09-26, Croatia Scientific / art field, NATURAL SCIENCES Abstract Ksenobiotike možemo definirati kao tvari strane živom organizmu, kao što su farmaceutici, pesticidi, neki prehrambeni aditivi, kozmetika i industrijski otpad. Njihovo korištenje u nepoznatim i nekontroliranim količinama predstavlja potencijalno štetan utjecaj na okoliš i živi svijet općenito. Stoga je vrlo važno razviti metode njihovog određivanja i praćenja. U ovom radu određivano je ukupno deset farmaceutika koji pripadaju različitim skupinama: antibiotici (azitromicin, cefdinir, eritromicin, klaritromicin, nitrofurantoin), antiemetici (metoklopramid), antihelmintici ili antiparazitici (albendazol, febantel, prazikvantel) i kemoterapeutik (hidroksiklorokin). Cilj ovog rada je odrediti optimalne uvjete ultrazvučne ekstrakcije (USE) i ekstrakcije raspršenjem matice uzorka kroz čvrstu fazu (MSPD) smjese deset ksenobiotika iz aktivnog mulja. USE metodom provedeno je devet eksperimenta kojima je ispitan utjecaj koncentracije standardne otopine, mase uzorka, otapala ili smjese otapala za eluiranje, te otapala za rekonstrukciju, dok je kod MSPD provedeno pet eksperimenata i optimirano je otapalo/smjesa otapala za eluiranje. Ekstrakti su analizirani tekućinskom kromatografijom visoke djelotvornosti s detektorom s nizom dioda (HPLC-DAD). Metoda je validirana određivanjem ponovljivosti, obnovljivosti, granice detekcije i granice kvantifikacije. Najbolji rezultati za USE postignuti su standardnom otopinom od 10 mg/L i 0,5 grama uzorka. Najbolji sustav otapala je aceton:metanol = 1:1, a korištenjem pokretne faze kao otapala za rekonstrukciju postigla su se nešto viša iskorištenja za pojedine ksenobiotike. Za MSPD metodu najbolja čista otapala su metanol i etanol, a najbolji sustavi su 1-propanol:voda = 60:40 i metanol:voda = 80:20 kojima su ekstrahirani svi ksenobiotici. Obzirom da se USE i MSPD metodom ne postižu željena iskorištenja (preko 50 % za sve ksenobiotike) potrebno je provesti daljnje eksperimente za njihovu optimizaciju ili isprobati neku alternativnu metodu ekstrakcije.
Abstract (english) Xenobiotics are defined as substances foreign to a living organism, such as pharmaceuticals, pesticides, some food additives, cosmetics and industrial waste. Using xenobiotics in unknown and uncontrolled quantities is potentially harmful to the environment and the living world in general. It is therefore very important to develop methods of their monitoring and determination. In this paper, a mixture of ten pharmaceuticals classified to different groups have been quantified: antibiotics (azithromycin, cefdinir, erythromycin, clarithromycin, nitrofurantoin), antiemetics (metoclopramide), antihelmintics or antiparasitics (albendazole, febantel, praziquantel) and chemotherapeutic (hydroxychloroquine). The aim of this paper is to optimize the conditions for ultrasonic extraction and matrix solid phase dispersion (MSPD) of ten xenobiotics from activated sludge. Nine experiments were performed using ultrasonic extraction (USE). Parameters which were optimized were the concentration of standard solution, mass of the sample, solvent or mixture of solvents for elution and solvents for dissolving the dry residue, while with MSPD five experiments were performed and solvent/mixture of solvents for elution were optimized. The extracts were analysed by high-performance liquid chromatography with diode array detector (HPLC-DAD). The method was validated by determining repeatability, renewability, limit of detection and limit of quantification. The best results for the USE were achieved with a standard solution of 10 mg/L and 0,5 grams of sample. The best solvent system is acetone:methanol = 1:1. Also, by using the mobile phase as the solvent for dissolving the dry residue, higher yields for some of the xenobiotics were achieved. For the MSPD method, the best pure solvents are methanol and ethanol, and the best systems are 1-propanol:water = 60:40 and methanol:water = 80:20, which extracted all xenobiotics. Since the USE and the MSPD did not achieve the desired recoveries (over 50 % for all xenobiotics) it is necessary to carry out further experiments or try an alternative method of extraction.
Keywords
ksenobiotici
aktivni mulj
ultrazvučna ekstrakcija
ekstrakcija raspršenjem matice uzorka kroz čvrstu fazu (MSPD)
tekućinska kromatografija visoke djelotvornosti s detektorom s nizom dioda (HPLC–DAD)
Keywords (english)
xenobiotics
activated sludge
ultrasonic extraction
matrix solid phase dispersion (MSPD)
high-performance liquid chromatography with diode array detector (HPLC-DAD)
Language croatian URN:NBN urn:nbn:hr:149:487451 Project Number: IP-2014-09-2353 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 Closed access Terms of use Created on 2022-02-23 12:50:22
