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    Methods for indomethacin determination

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    Nesteroidni protuupalni lijekovi (NSAID) su prvi izbor u liječenju reumatskih poremećaja te drugih degenerativnih upalnih bolesti. Postoje brojne vrste ovih lijekova, a u ovom radu je istaknut jedan od njih, indometacin. Sa svojim analgetskim, antipiretskim i protuupalnim svojstvima jedan je od najmoćnijih lijekova koji se koristi u različitim kliničkim ispitivanjima i terapijama vezanim za mehanizam blokiranja sinteze prostaglandina čime se smanjuju i uklanjaju brojna upalna stanja pacijenata. Da bi se osigurala učinkovitost i sigurnost ovoga lijeka u farmaceutskoj i kliničkoj primjeni, potrebna je određena kontrola kvalitete proizvoda. Kontrola se provodi rutinskim farmaceutskim analizama uz pomoć različitih kemijskih metoda kojima se indometacin identificira kao zasebna aktivna komponenta u višekomponentnom sustavu cjelovitog farmaceutskog oblika. Osim toga, određivanje indometacina važno je i u kliničkoj praksi, gdje se njegova koncentracija određuje iz različitih bioloških uzoraka čime se postiže kvalitetnije praćenje određene terapije. Najčešće metode za određivanje indometacina su: potenciometrija, voltametrija, tekućinska kromatografija visoke djelotvornosti (HPLC), plinska kromatografija (GC), UV spektroskopija, kolorimetrija, fluorimetrija, kemiluminiscencija i imunokemijske metode (ELISA i radioimuno test). Svaka od metoda mora osigurati precizne validacijske parametre. Pri određivanju indometacina najčešće se kombiniraju dvije metode čime se postižu precizniji rezultati i sigurnija primjena u praksi.Nonsteroidal anti-inflammatory drugs (NSAIDs) are the first choice in the treatment of rheumatic disorders and other degenerative inflammatory diseases. There are numerous types of these drugs, and one of them, indomethacin, is highlighted in this paper. With its analgetic, antipyretic and anti-inflammatory properties, it is one of the most powerful drugs used in various clinical trials and therapies related to the mechanism of blocking prostaglandin synthesis, thus reducing and eliminating many inflammatory conditions of patients. To ensure the efficacy and safety of this drug in pharmaceutical and clinical use, particular product quality control is required. Such control is performed with routine pharmaceutical analysis using various chemical methods by which indomethacin is identified as a separate active ingredient in a multicomponent system of a complete pharmaceutical form. In addition, the determination of indomethacin is important in clinical practice, where its concentration is determined in different biological samples, ensuring better monitoring of a particular therapy. The most commonly used methods for the determination of indomethacin are: potentiometry, voltammetry, high performance liquid chromatography (HPLC), gas chromatography (GC), UV spectroscopy, colorimetry, fluorimetry, chemiluminescence and immunochemical methods (ELISA and radioimmunoassay). Each of these methods must provide precise validation parameters. For indomethacin determination, two methods are usually combined, this way more precise results and safer application in practice are achieved

    Chromatography as an analytical method for the determination of biological samples

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    Kromatografija je jedna od fizikalno-kemijskih metoda koja se temelji na razdvajanju smjesa, pri čemu se sastojci smjesa razdjeljuju između dviju faza. Svaka od kromatografskih metoda sastoji se od dvije faze, a to su nepokretna (stacionarna) i pokretna (mobilna) faza. Rezultat kromatografske analize je kromatogram koji nam služi za identifikaciju sastojaka. Kromatografiju dijelimo na dvije velike skupine: plošna kromatografija i kromatografija na stupcu. Kromatografija koja je danas najzastupljenija u znanstvenim i medicinskim istraživanjima je tekućinska kromatogrfija visoke djelotvornosti ili HPLC (engl. High Performance Liquid Cromatography). Zbog visoke osjetljivosti i analize širokog spektra uzoraka, koristi se i za analizu nekih bioloških uzoraka. Krv i kosa, kao biološki uzorci, najčešće se korsite za detekciju droga. Krv kao najpouzdaniji uzorak, zatim kosa kao uzorak koji najduže zadržava drogu, ekstrakcijskim se metodama pripremaju za imunokemijsku analizu, nakon čega se rezultati potvrđuju kromatografskim metodama. Kromatografske metode koje se koriste u svrhu analize droga su: tankoslojna kromatografija (TLC), plinska kromatografija (GC), tekućinska kromatografija s visokom djelotvornosti (HPLC) i plinska kromatografija sa spektrometrijom masa (GC/MS).Chromatography is one of physico-chemical methods based on the separation of the mixture, where ingredients of the mixture are separated through two phases. Each chromatographic method undergoes two phases called stationary and mobile phase. Result of chromatographic analisys is chromatogram which is used to identify ingredients. Chromatography is divided in two major groups: planar chromatography and column chromatography. Technique which is most commonly used in scientific and medical researches is HPLC (High Performance Liquid Chromatography). This technique is also used for analyzing some biological samples due to its high sensitivity and broad-spectrum sample analysis. Blood and hair, as biological samples, are most often used for drug detection. Blood, as the most reliable sample, and hair, as the one which retains drugs the longest, are prepared for immunochemical analysis using extraction methods. Chromatographic methods used for analyzing drugs are: thin-layer chromatography (TLC), gas chromatography (GC), high-performance liquid chromatography (HPLC) and gas chromatography-mass spectrometry (GC/MS)

    Determination of inorganic cations using electrophoresis on microchip with C4D C^{4}D detector

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    Kationi su atomi ili molekule koji su pozitivno nabijeni, a u električnom polju putuju prema negativno nabijenoj elektrodi, katodi. Velika rasprostranjenost anorganskih kationa u vodi, tjelesnim tekućinama, eksplozivima i mnogim lijekovima, privukla je pažnju znanstvenika za kreiranje precizne, efikasne te lako dostupne metode za njihovu detekciju. Cilj ovog rada je prikazati mogućnosti primjene elektroforeze na mikročipu i prikazati rezultate određivanja anorganskih kationa pomoću ove metode. Prilikom izvođenja minijaturizirane kapilarne elektroforeze, analiza se odvija u separacijskom kanalu mikročipa, a signal se dobiva uslijed promjene električne vodljivosti. Promjenom vodljivosti nastaje informacija koja se prikazuje u obliku izraženih pikova koji daju podatak o koncentracijama nabijenih specija.Cations are atoms or molecules that are positively charged and travel in an electric field to a negatively charged electrode, the cathode. The high prevalence of inorganic cations in water, body fluids, explosions, and many drugs has attracted the attention of scientists to create precise, efficient, and readily available methods for their detection. The goal of this paper is to present the possibilities of applied electrophoresis on a microchip and to present the results of determination of inorganic cations using these methods. During miniaturized capillary electrophoresis, the analysis takes place in the separation channel of the microchip, and the signal is obtained when the electrical conductivity changes. The change in conductivity produces information that is displayed in the form of pronounced peaks that give information about the concentration of charged species

    Determination of lutein in eggs enriched with functional ingredients

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    Sadržaj luteina određivan je u ukupno šest skupina jaja. Četiri skupine nesilica hranjene su krmnim smjesama različitog sastava od kojih je u krmnu smjesu kojom su hranjene nesilice za jednu skupinu kao funkcionalni sastojak dodan samo lutein, dok je u krmnu smjesu za drugu skupinu nesilica, uz druge funkcionalne sastojke dodan i lutein. Dvije skupine jaja proizvedena su na dva obiteljska poljoprivredna gospodarstva. Lutein je određivan u žumanjku jaja korištenjem tekućinske kromatografije visoke razlučivosti s UV detekcijom. Najmanja koncentracija luteina određena je u kontrolnoj skupini i iznosila je 0,644 mg/100 g žumanjka dok je najveća koncentracija luteina 3,661 odnosno 3,789 mg/100 g žumanjka, određena u skupinama jaja koja su dobivena od nesilica koje su hranjene krmnim smjesama u koje je dodan lutein. Usporedbom s literaturnim podacima, u ove dvije skupine koncentracija luteina je povećana za oko šest puta. U jajima koja su proizvedena na dva obiteljska poljoprivredna gospodarstva, koncentracija luteina je povećana za šest odnosno četiri puta.Lutein content was determined in a total of six groups of eggs. Four groups of laying hens were fed with feed mixtures of different composition, lutein was the only added functional ingredient to the feed mixture for one group of laying hens, while lutein with other functional ingredients was added to the feed mixture for another group of laying hens. Two groups of eggs were produced on two family farms. Lutein was determined in egg yolks using high-performance liquid chromatography with UV detection. The lowest concentration of lutein was determined in the control group and was 0.644 mg / 100 g of yolk, while the highest concentration of lutein was 3.661 and 3.799 mg / 100 g of yolk, determined in groups of eggs obtained from laying hens fed with feed mixtures enriched with lutein. Compared with the literature data in these two groups, the lutein concentration was increased by about six times. In eggs produced on two family farms, the lutein concentration was increased by six and four times, respectively

    Assessment of selected rare earth elements in hari (ICP-MS)

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    Globalna upotreba elemenata rijetkih zemalja je u porastu kroz industriju, poljoprivredne aktivnosti (gnojiva) i medicinu. Koncentracija elemenata rijetkih zemalja u okolišu nije velika, međutim njihovom upotrebom dolazi do njihove sve veće akumulacije u ljudskom organizmu. Cilj istraživanja bio je ispitati koncentraciju odabranih elemenata rijetkih zemalja: La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Tm, Yb. U uzorcima kose stanovnika Osječko- baranjske županije. Uzorci kose 391 ispitanika prikupljeni su na području dva veća mjesta (Osijek i Našice) i 3 naselja u okolini grada Osijeka (Vladislavci, Čepin , Dalj) i analizirani metodom ICP-MS.U usporedbi s uzorcima kose stanovnika koji žive na području sela Dalj, uzorci kose prikupljeni na području Osijeka, Našica Čepina, i Vladislavaca imali su manje koncentracije elemenata rijetkih zemalja. Vrijednosti medijana koncentracija svih analiziranih elemenata bile su u rasponu: 0,00-0,04 μg/g, a kretale su se u granicama referentnih vrijednosti pronađenih u literaturi.The global use of rare earth elements is growing in industry, agriculture (fertilizers) and medicine. The concentration of rare earth elements in the environment is not high, but their use leads to greater accumulation in the human body. The aim of the study was to examine the concentration of rare earth elements: La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Tm, Yb. In the hair samples of the inhabitants of Osijek-Baranja County. Hair samples of 391 respondents were collected in two larger places (Osijek and Našice) and 3 settlements around the city of Osijek (Vladislavci, Čepin, Dalj) and analyzed by ICP-MS method. Compared to hair samples of residents living in the village of Dalj, hair samples were collected in the area of Osijek, Našice, Čepin and Vladislavci had lower concentrations of rare earth elements. The values of the median concentration of all analyzed elements were in the range: 0,00-0,04 μg/g, and ranged within the reference values from the literature

    Inorganic nanomaterials

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    Anorganski nanomaterijali počeli su se istraživati intenzivnije zadnjih nekoliko desetljeća. Naime, nanomaterijali posjeduju poboljšana, ali opet sasvim drugačija svojstva u odnosu na makromaterijale od kojih su sintetizirani te se stoga koriste u mnoge svrhe u kojima makromaterijali ne bi imali nikakvog utjecaja. Nanomaterijali se, s obzirom na veličinu i svoj oblik, kategoriziraju kao nultodimenzionalni, jednodimenzionalni, dvodimenzionalni i trodimenzionalni nanomaterijali od kojih svaka vrsta posjeduje jedinstvena svojstva zbog kojih se oni i koriste. Sinteze nanomaterijala mogu biti različite, ali najviše se koriste metode mehanokemijske sinteze, metode manipulacije atoma i/ili molekula ("Top-down" i "Bottom-up") te katalitičke metode od kojih je najistaknutija fotokataliza. Kod spomenutih sinteza ključna svojstva su: jednostavnost, ušteda energije te što bolja svojstva nanomaterijala. Svojstva nanomaterijala ovise primarno o veličini čestica i pora. Poželjno je da su čestice što manje kako bi i svojstva bila bolja. Sukladno tome, nanomaterijali se mogu koristiti u raznim područjima biomedicine, farmacije, čak i prehrambene, tekstilne i kozmetičke industrije. Primarno se koriste u robotici i inženjerstvu gdje se posebnim tehnikama manipulacije mogu dobiti nanouređaji jedinstvenih i posebnih svojstava koji se zatim koriste u razne svrhe (kao npr. nanoalati). U biomedicinske svrhe, nanomaterijali se najviše koriste za detekciju različitih tumorskih biomarkera u najranijim fazama. Zahvaljujući posebnim magnetskim svojstvima nanomaterijala (superparamagnetičnost i magnetičnost), moguć je neometani transport lijeka do ciljanih konkretnih stanica i/ili tkiva.Inorganic nanomaterials have been researched more intensively for the last few decades. They have better, yet again, completely different properties compared to bulky materials from which they are syntesized, and therefore used for many purposes in which bulky materials would not have any impact. Nanomaterials, given their size and shape, are categorized as non-dimensional, one-dimensional, two-dimensional and three-dimensional nanomaterials, that each of has unique properties for which they are used. The synthesis of nanomaterials can be different, but the most commonly used methods are mechanochemical synthesis, methods of manipulation of atoms and/or molecules ("Top-down" and "Bottom-up") and catalytic methods, the most prominent of which is photocatalysis. In the mentioned syntheses, the key properties are: simplicity, energy savings and the best possible properties of nanomaterials. The properties of nanomaterials depend primarily on particle and pore size. It is desirable that the particles are as small as possible in order for the properties to be better. Accordingly, nanomaterials can be used in various fields of biomedicine, pharmacy, and even the food, textile, and cosmetic industries. They are primarily used in robotics and engineering where special manipulation techniques can be used to obtain nanodevices with unique and special properties which are then used for various purposes (such as nanotools). For biomedical purposes, nanomaterials are mostly used to detect various tumor biomarkers in the earliest stages. Thanks to the special magnetic properties of the nanomaterials (superparamagneticity and magnetism), the drugs can be easily transported to the targeted cells

    Bioosythesis and biochemistry of niacin

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    Niacin (vitamin B3) jedan je od 8 B-kompleks vitamina. Dolazi u obliku nikotinske kiseline, nikotinamida i nikotinamid ribozida. Nikotinska kiselina i nikotinamid su slične topljivosti u vodi. Otkriću niacina je prethodila epidemija pelagre, bolesti uzrokovane deficitom niacina u tijelu, koja se javila krajem 19.-og stoljeća. Moguća je biosinteza niacina iz triptofana, a on svoju glavnu ulogu ima kao nukleotid NAD+ NAD^{+} i NADP+ NADP^{+} te sudjeluje u preko 400 redoks reakcija kao koenzim. Osim enzimatski potpomognutih reakcija, NAD+ NAD^{+} sudjeluje i kao supstrat u mnogim reakcijama, od kojih su najbitnije one zaslužne za popravak DNA. U posljednje je vrijeme dana velika pažnja niacinu kao lijeku. U visokim koncentracijama se koristi kao lijek za snižavanje povišene koncentracije kolesterola u krvi, ali i u dermatološke svrhe kao lijek protiv crvenila i nepravilnosti kože.Niacin (vitamin B3) is one of 8 B-complex vitamins. It comes in forms of nicotinic acid, nicotinamide and nicotinamide riboside. Nicotinic acid and nicotinamide have similar solubility in water. Pellagra outbreak in the 19th century preceded the discovery of niacin, a disease caused by a deficit of niacin in the body. A biosynthesis of niacin from tryptophan is possible, but his main role is in the form of NAD+ NAD^{+} and NADP+ NADP^{+} where it participates in over 400 redox reactions as a coenzyme. Apart from enzymatic reactions, NAD+ NAD^{+} participates also as a substrate in many reactions, of which the most important ones being those responsible for DNA repair. Recently, light has been shed on niacin as a drug. In high concentrations it is used as a medicine for lowering high cholesterol in blood, as well as in dermatology as a cure for redness and imperfections of the skin

    Application of separation methods in analytical chemistry

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    Na kraju same reakcije vrlo rijetko se dobije čisti kemijski spoj, već smjesa tvari u kojoj su uz traženi produkt prisutni i nusprodukti, ostaci neizreagiranih reaktanata i katalizatori. Mnoge tvari izolirane iz prirode, kao i produkti sinteza nisu čisti. Stoga je jedna od bitnih uloga kemičara separiranje čistih spojeva od nečistoća iz homogenih ili heterogenih smjesa. Za tu svrhu, uz konvencionalne tehnike filtriraciju, sublimaciju, prekristalizaciju, brojne vrste destilacija i ekstrakciju upotrebljava se i velik broj kromatografskih metoda. U ovome radu objašnjene su instrumentalne separacijske metode ekstrakcije i kromatografije koje se zasnivaju na novijim istraživanjima svojstava tvari i koriste naprednu tehnologiju poput ultrazvuka i mikrovalova. Navedene su njihove prednosti nad konvencionalnim, aparatura potrebna za izvođenje, te primjena u različitim područjima.After the chemical reaction, remains a mixture containing not just the chemical combination (the product), but also byproducts, unreacted reactants, catalysts and other impurities that need to be removed. Many substances isolated from the nature as well as the products of synthesis are not pure. Therefore, one of the important tasks of a chemist is to separate a pure compounds from heterogeneous or homogeneous mixtures. Along with classical procedures, such as recrystallization, filtration, various types of distillation and extraction, a whole series of chromatographic methods is used. In this paper, extraction and chromatography as instrumental separation methods are explained. Those methods are based on properties of the substances and the use of advanced technologies like ultrasound and microwaves. The advantages of those methods over conventional ones, as well as performance equipment and application in different areas are stated

    Synthetic polymers

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    Cilj je i svrha ovoga rada upoznati se sa osnovnim kemijskim i fizikalnim svojstvima sintetskih polimera, reakcijama nastajanja, upotrebom te utjecajem na okoliš. Sintetski su polimeri umjetno sintetizirane makromolekule koje nastaju reakcijama polimerizacije. Zbog vrlo korisnih i specifičnih svojstava te iznimne kemijske postojanosti, glavna su komponenta za izradu plastičnih materijala, odnosno plastike, koja je danas jedna od glavnih korištenih materijala. Upotrebljavaju se u svim djelatnostima i područjima. Unatoč iznimnim svojstvima, proces razgradnje je kompleksan, dugotrajan te se nerijetko oslobađaju vrlo toksične supstance, što je glavni problem današnjice jer dolazi do zagađenja ekosustava i atmosfere. Recikliranjem, omogućavanjem biorazgradnje sintetskih polimera te pronalaskom alternativa koje su manje štetne, moguće je riješiti se zagađenja i poboljšati kvalitetu života.The aim and purpose of this work is to become familiar with the basic chemical and physical properties of synthetic polymers, formation reactions, use and environmental impact. Synthetic polymers are artificially synthesized macromolecules that are formed by polymerization reactions. Due to the very useful and specific properties of this exceptional chemical stability, they are the main component for the production of plastic materials, i.e. plastic, which is today one of the main materials used. They are used in all industries and areas. Despite its exceptional properties, the decommissioning process is complex, time-consuming and often releases highly toxic substances, which is the main problem of today because ecosystem and atmosphere contamination occurs. By recycling, enabling the biodegradation of synthetic polymers and finding alternatives that are less harmful, it is possible to get rid of pollution and improve quality of life

    Synthesis and characterization of N2O2-donor macrocyclic Schiff base silver complexes

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    Predmet ovog završnog rada je sinteza i karakterizacija kompleksnih spojeva srebra sa N2O2 N_{2}O_{2}-donornim makrocikličkim Schiffovim bazama. U svim sintezama koristili su se Schiffove baze kao ligandi. Korištene Schiffove baze nastale su reakcijom dialdehida sa m-fenilendiaminom uz etanol te trietilamin kao katalizator. Kompleksi su dobiveni reakcijom određenih Schiffovih baza sa AgPF6 AgPF_{6} i uparavanjem pomoću etera. Od ukupno 5 provedenih sinteza dobivena su 3 kompleksna spoja koja su analizirana IR spektroskopijom i čiji su spektri uz pretpostavljene strukture prikazane u ovom radu.The subject of this paperwork is the synthesis and characterization of complex silver compounds with N2O2 N_{2}O_{2} donor macrocyclic Schiff bases. In all synthesis of complex compounds as ligands Schiff bases were used. They were syntesized by the reaction of dialdehydes and m-phenylenediamine in ethanol and trietilamine as a catalyst. Complexes were made by the reaction of Schiff bases and AgPF6 AgPF_{6} in eter. Only 3 compounds from performed 5 synthesis were used for IR spectroscopy analysis and their assumed structures are presented int his paper work

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