Epitope Mapping of Macrolide Antibiotics to Bovine Serum Albumin by Saturation Transfer Difference NMR Spectroscopy

Saturation transfer difference NMR spectroscopy was employed to characterize epitopes of macrolide antibiotics, azithromycin, oleandomycin and telithromycin binding to bovine serum albumin. The structural parts of azithromycin and oleandomycin in intimate contact with bovine serum albumin were found to be similar while those of telithromycin showed similarities but also some differences. The latter were mostly due to different structural elements of antibiotics that interact with the protein, especially the alkyl-heteroaryl side chain in telithromycin and cladinose and desosamine sugars in azithromycin and oleandomycin. The epitope maps as determined in this study can contribute to better understanding of the overall bioactivity of macrolides

Intra- and intermolecular hydrogen bonding in acetylacetone and benzoylacetone derivatives

Enaminoni (enamini β-dikarbonilnih spojeva) pripadaju skupini organskih molekula koje posjeduju zanimljiva biološka i farmakološka svojstva, a mogu postojati u tri tautomerne forme, s mogućnošću stvaranja intra- i intermolekulskih vodikovih veza. Detaljna strukturna karakterizacija ove skupine organskih molekula nužna je kako bi se što bolje objasnila i povezala svojstva s molekulskom strukturom i vodikovim vezama prisutnim u otopini i čvrstom stanju. U ovom radu određena je struktura derivata pentan-2,4-diona i 1-fenil-but-2-en-1-ona u otopini, pomoću različitih spektroskopskih i računskih metoda. Korištenjem jednodimenzijskih i dvodimenzijskih tehnika spektroskopije NMR, te spektroskopije UV, spektroskopije IR i Ramanove spektroskopije proučavan je utjecaj supstituenata (2-amino-3- nitrofenola i derivata 2-amino-2-metilfenola), prirode otapala (različita polarnost, različita proton-donorska odnosno proton-akceptorska svojstava) i temperature na vodikove veze (intra- i intermolekulske) i molekulsku strukturu derivata pentan-2,4-diona i 1-fenil-but-2-en1-ona. Eksperimentalni rezulatati upotpunjeni su podacima konformacijske analize pri čemu su korištene računske metode na semiempirijskoj razini (PM6) i metode funkcionala gustoće (DFT). Vodikove veze su okarakterizirane u vakuumu, kloroformu i dimetilsulfoksidu (DMSO-u). Ova istraživanja su pokazala da su svi derivati pentan-2,4-diona i 1-fenil-but-2-en-1- ona u otopini prisutni u keto-aminskoj formi, neovisno o otapalu i temperaturi. Dokazano je postojanje jakih intramolekulskih vodikovih veza tipa N–H ...O, te slabih intermolekulskih interakcija između dvije molekule spoja i/ili između molekule spoja i otapala.Enaminones (enamines of β-dicarbonyl compounds) belongs to a group of organic molecules with interesting biological and farmaceutical properties, and might exist in three tautomeric forms, with the possibility of forming intra- and intermolecular hydrogen bonds. Detailed structural characterization of this group of organic molecules is needed to establish structure acitivity ralationships with special emphasis on hydrogen bonding. In this doctoral thesis structures of pentane-2,4-dione and 1-phenyl-but-2-en-1-one derivatives has been determined in solution, by using different spectroscopic (one and two dimensional NMR spectroscopy, UV, IR and Raman spectroscopy) and computational methods. Special attention has been devoted to the influence of the substituents (2-amino-3- nitrophenol i derivatives of 2-amino-2-methylphenols), nature of the solvent (different polarity and different proton-donor and proton-acceptor abbilites) and temperature on hydrogen bonding (intra- and intermolecular) structure of pentane-2,4-dione and 1-phenylbut-2-en-1-one derivatives. The experimental results were complemented with those obtained by computational methods, performed at the semiempirical PM6 level and by using density functional theory (DFT). Hydrogen bonding were characterized in vacuum, chloroforme and dimethyl sulfoxide (DMSO). All investigated pentane-2,4-dione and 1-phenyl-but-2-en-1-one derivatives have been found to exist in the ketoamine form in solution, irrespective of the solvent and the temperature. Results showed presence of strong intramolecular hydrogen bonds of the N– H ...O type as well as weaker intermolecular interactions between two molecules or between the molecule and the solvent

Intra- and intermolecular hydrogen bonding in acetylacetone and benzoylacetone derivatives

Enaminoni (enamini β-dikarbonilnih spojeva) pripadaju skupini organskih molekula koje posjeduju zanimljiva biološka i farmakološka svojstva, a mogu postojati u tri tautomerne forme, s mogućnošću stvaranja intra- i intermolekulskih vodikovih veza. Detaljna strukturna karakterizacija ove skupine organskih molekula nužna je kako bi se što bolje objasnila i povezala svojstva s molekulskom strukturom i vodikovim vezama prisutnim u otopini i čvrstom stanju. U ovom radu određena je struktura derivata pentan-2,4-diona i 1-fenil-but-2-en-1-ona u otopini, pomoću različitih spektroskopskih i računskih metoda. Korištenjem jednodimenzijskih i dvodimenzijskih tehnika spektroskopije NMR, te spektroskopije UV, spektroskopije IR i Ramanove spektroskopije proučavan je utjecaj supstituenata (2-amino-3- nitrofenola i derivata 2-amino-2-metilfenola), prirode otapala (različita polarnost, različita proton-donorska odnosno proton-akceptorska svojstava) i temperature na vodikove veze (intra- i intermolekulske) i molekulsku strukturu derivata pentan-2,4-diona i 1-fenil-but-2-en1-ona. Eksperimentalni rezulatati upotpunjeni su podacima konformacijske analize pri čemu su korištene računske metode na semiempirijskoj razini (PM6) i metode funkcionala gustoće (DFT). Vodikove veze su okarakterizirane u vakuumu, kloroformu i dimetilsulfoksidu (DMSO-u). Ova istraživanja su pokazala da su svi derivati pentan-2,4-diona i 1-fenil-but-2-en-1- ona u otopini prisutni u keto-aminskoj formi, neovisno o otapalu i temperaturi. Dokazano je postojanje jakih intramolekulskih vodikovih veza tipa N–H ...O, te slabih intermolekulskih interakcija između dvije molekule spoja i/ili između molekule spoja i otapala.Enaminones (enamines of β-dicarbonyl compounds) belongs to a group of organic molecules with interesting biological and farmaceutical properties, and might exist in three tautomeric forms, with the possibility of forming intra- and intermolecular hydrogen bonds. Detailed structural characterization of this group of organic molecules is needed to establish structure acitivity ralationships with special emphasis on hydrogen bonding. In this doctoral thesis structures of pentane-2,4-dione and 1-phenyl-but-2-en-1-one derivatives has been determined in solution, by using different spectroscopic (one and two dimensional NMR spectroscopy, UV, IR and Raman spectroscopy) and computational methods. Special attention has been devoted to the influence of the substituents (2-amino-3- nitrophenol i derivatives of 2-amino-2-methylphenols), nature of the solvent (different polarity and different proton-donor and proton-acceptor abbilites) and temperature on hydrogen bonding (intra- and intermolecular) structure of pentane-2,4-dione and 1-phenylbut-2-en-1-one derivatives. The experimental results were complemented with those obtained by computational methods, performed at the semiempirical PM6 level and by using density functional theory (DFT). Hydrogen bonding were characterized in vacuum, chloroforme and dimethyl sulfoxide (DMSO). All investigated pentane-2,4-dione and 1-phenyl-but-2-en-1-one derivatives have been found to exist in the ketoamine form in solution, irrespective of the solvent and the temperature. Results showed presence of strong intramolecular hydrogen bonds of the N– H ...O type as well as weaker intermolecular interactions between two molecules or between the molecule and the solvent

Intra- and intermolecular hydrogen bonding in acetylacetone and benzoylacetone derivatives

Enaminoni (enamini β-dikarbonilnih spojeva) pripadaju skupini organskih molekula koje posjeduju zanimljiva biološka i farmakološka svojstva, a mogu postojati u tri tautomerne forme, s mogućnošću stvaranja intra- i intermolekulskih vodikovih veza. Detaljna strukturna karakterizacija ove skupine organskih molekula nužna je kako bi se što bolje objasnila i povezala svojstva s molekulskom strukturom i vodikovim vezama prisutnim u otopini i čvrstom stanju. U ovom radu određena je struktura derivata pentan-2,4-diona i 1-fenil-but-2-en-1-ona u otopini, pomoću različitih spektroskopskih i računskih metoda. Korištenjem jednodimenzijskih i dvodimenzijskih tehnika spektroskopije NMR, te spektroskopije UV, spektroskopije IR i Ramanove spektroskopije proučavan je utjecaj supstituenata (2-amino-3- nitrofenola i derivata 2-amino-2-metilfenola), prirode otapala (različita polarnost, različita proton-donorska odnosno proton-akceptorska svojstava) i temperature na vodikove veze (intra- i intermolekulske) i molekulsku strukturu derivata pentan-2,4-diona i 1-fenil-but-2-en1-ona. Eksperimentalni rezulatati upotpunjeni su podacima konformacijske analize pri čemu su korištene računske metode na semiempirijskoj razini (PM6) i metode funkcionala gustoće (DFT). Vodikove veze su okarakterizirane u vakuumu, kloroformu i dimetilsulfoksidu (DMSO-u). Ova istraživanja su pokazala da su svi derivati pentan-2,4-diona i 1-fenil-but-2-en-1- ona u otopini prisutni u keto-aminskoj formi, neovisno o otapalu i temperaturi. Dokazano je postojanje jakih intramolekulskih vodikovih veza tipa N–H ...O, te slabih intermolekulskih interakcija između dvije molekule spoja i/ili između molekule spoja i otapala.Enaminones (enamines of β-dicarbonyl compounds) belongs to a group of organic molecules with interesting biological and farmaceutical properties, and might exist in three tautomeric forms, with the possibility of forming intra- and intermolecular hydrogen bonds. Detailed structural characterization of this group of organic molecules is needed to establish structure acitivity ralationships with special emphasis on hydrogen bonding. In this doctoral thesis structures of pentane-2,4-dione and 1-phenyl-but-2-en-1-one derivatives has been determined in solution, by using different spectroscopic (one and two dimensional NMR spectroscopy, UV, IR and Raman spectroscopy) and computational methods. Special attention has been devoted to the influence of the substituents (2-amino-3- nitrophenol i derivatives of 2-amino-2-methylphenols), nature of the solvent (different polarity and different proton-donor and proton-acceptor abbilites) and temperature on hydrogen bonding (intra- and intermolecular) structure of pentane-2,4-dione and 1-phenylbut-2-en-1-one derivatives. The experimental results were complemented with those obtained by computational methods, performed at the semiempirical PM6 level and by using density functional theory (DFT). Hydrogen bonding were characterized in vacuum, chloroforme and dimethyl sulfoxide (DMSO). All investigated pentane-2,4-dione and 1-phenyl-but-2-en-1-one derivatives have been found to exist in the ketoamine form in solution, irrespective of the solvent and the temperature. Results showed presence of strong intramolecular hydrogen bonds of the N– H ...O type as well as weaker intermolecular interactions between two molecules or between the molecule and the solvent

Detemination of fungicide residues in grape by GC/MS.

The extensive use of pesticides in modern farming on fruit and vegetables has posed risks to public health and environment. Pesticide residues can be found even when they are applied in accordance with good agricultural practices. This paper deals with the analysis residues of three fungicides (benalaxyl, dimethomorph, tetraconazole) by chromatographic method in grape samples. The applicability of the proposed method to detect and quantify pesticide residues has been demonstrated by the analysis sample grapes varieties "Zilavka" and "Blatina" cultivated on a small farm in the vineyards in a broader the region of Mostar. Analytes were extracted using SPE technique and analysis is performed by gas chromatography, employing mass selective detection in the selected ion monitoring mode, The content fungicides (benalaxyl, dimethomorph, tetraconazole) in grape samples is regulated by relevant EU regulation (The Annexes of Commission Regulation (EC), No. 396/2005). In grape samples analyzed in this study residues of benalaxyl and tetraconazole were found. The fungicide concentrations were bellow the MRL value permitted by EU regulations for grape