Title Određivanje farmaceutika u aktivnom mulju Title (english) Determination of pharmaceuticals in activated sludge Author Antonela Čović Mentor Danijela Ašperger (mentor)Committee member Danijela Ašperger (predsjednik povjerenstva)Committee member Mirta Čizmić (član povjerenstva)Committee member Marijana Hranjec (član povjerenstva)Granter University of Zagreb Defense date and country 2017-07-10, Croatia Scientific / art field, NATURAL SCIENCES Abstract Farmaceutici su kemijske tvari koje se koriste u liječenju i spriječavanju bolesti. Smatraju se novim onečišćivalima jer za njih nema propisana zakonska doza prilikom ispuštanja obrađenih otpadnih voda u okoliš. Zbog povećane potrošnje farmaceutika oni su sve više prisutni u okolišu, vodama, tlu i sedimentu. Razlog tomu je što se male molekule farmaceutika ne mogu ukloniti u potpunosti klasičnim metodama obrade otpadnih voda farmaceutskih industrija, a zadržavaju se koncentrirane i u aktivnom mulju sustava za obradu otpadnih voda. Stoga je potrebno uvesti zakonski propisane maksimalno dopuštene koncentracije farmaceutika u okolišu, ali i pratiti koncentracije farmaceutika prije i nakon obrade otpadnih voda farmaceutske industrije kao i u aktivnom mulju kojeg treba u konačnici na adekvatan način zbrinuti. U tu svrhu potrebno je prvo razviti analitičke metode ekstrakcije farmaceutika iz realnih uzoraka i kvantitativno i kvalitativno odrediti farmaceutike odgovarajućim tehnikama. Farmaceutici određivani u ovom radu su: antihelmintici (albendazol, febantel, prazikvantel), antibiotici (azitromicin, cefdinir, eritromicin, klaritromicin, nitrofurantoin), kemoterapeutici (hidroksiklorokin) i antiemetik (metoklopramid). Cilj rada je odrediti optimalne uvjete ekstrakcije farmaceutika metodom mućkanja iz aktivnog mulja. Parametri koji su optimirani su vrsta i volumen otapala, vrijeme ekstrakcije, omjer mase uzorka i otapala, te utjecaj pH-vrijednosti. Kvantitativna i kvalitativna analiza farmaceutika provedena je vezanim kromatografskim sustavima: tekućinskom kromatografijom visoke djelotvornosti s detektorom s nizom dioda (HPLC-DAD) i tekućinskom kromatografijom visoke djelotvornosti sa spektrometrom masa (HPLC-MS/MS). Najbolji rezultati su postignuti sa sustavima otapala metanol:acetonitril, metanol:aceton, metanol:voda i metanol:heksan s 0,5 g uzorka uz volumen otapala od 3 mL. Međutim, generalno, ova metoda nije dala zadovoljavajuća iskorištenja, sva su bila maksimalno do 30 % te se metoda kao takva nije niti validirala niti se preporuča za rutinsku primjenu unatoč jednostavnosti i niskoj cijeni metode ekstrakcije.
Abstract (english) Pharmaceuticals are chemical substances used in the treatment and prevention of diseases. They are considered as new pollutants because they do not have defined a regulatory legal dose for releasing treated wastewater into the environment. Due to increased pharmaceutical consumption they are present in the water, soil, sediment and in the environment. The reason is that small molecules of pharmaceuticals can not be completely removed by the classical wastewater treament methods of the pharmaceutical industry and they are retained in the active sludge of wastewater treatment. Therefore, it is necessary to introduce leagally prescribed maximum concentration of pharmaceuticals in the environment but it is also necessary to monitor the concentrations of the pharmaceuticals before and after wastewater treatment of the pharmaceutical industry. The concentration of pharmaceutcals in active sludge should be monitored and the sludge should be disposed in adequate procedure after the usage. For this purpose it is necessary to develop analytical methods for extraction of pharmaceuticals from real samples and quantitatively and qualitatively determine the pharmaceuticals by appropriate tehniques. The pharmaceuticals used in this paper are: antihelminitics (albendazole, febantel, praziquantel), antibiotics (azitromycine, eritromycine, cefdinir, chlaritromycine, nitrofurantoin), chemoterapeutic agent (hydroxychloroquine) and antiemetic (metoclopramide). The aim of this paper is to determine the optimum conditions for extraction of the pharmaceuticals by the method of agitation from the active sludge. Optimized parameters are type and volume of solvent, time of extraction, sample and solvent ratio and pH value. The quantitative and qualitative analysis of the pharmaceuticals was preformed by tandem chromatographic systems: high preformace liquid chromatography with diode array detectors (HPLC-DAD) and high preformance liquid chromatography with mass spectrometry (HPLC-MS/MS). The best results were achived with solvent systems: methanol:acetonitrile, methanol:acetone, methanol:water and methanol:hexane with 0,5 g of sample with a solvent volume of 3 mL. However, with this method the achieved efficiencies were up to 30 % which is not satisfactory. The method as such was neither validated nor recommended for routine use despite the simplicity and low cost of the extraction method.
Keywords
aktivni mulj
farmaceutici
metoda mućkanja
tekućinska kromatografija visoke djelotvornosti
tekućinska kromatografija visoke djelotvornosti sa spektrometrom masa
Keywords (english)
activated sludge
pharmaceuticals
extraction by agitation
high performance liquid chromatography (HPLC-DAD)
high preformance liquid chromatography tandem mass spectrometry (HPLC-MS/MS)
Language croatian URN:NBN urn:nbn:hr:149:417435 Study programme Title: Chemical Engineering - Graduate study Type of resource Text File origin Born digital Access conditions Open access Terms of use Created on 2019-11-07 08:50:42
