Pub Date : 2014-03-01DOI: 10.2478/s11532-013-0379-0
V. Mánuel, J. Pinto, Carolina Mendiguchía, C. Moreno
AbstractIn this work, Cd(II) extraction in natural waters by organophosphorus extractants as organic phase, as well as its back-extraction in an acidic media, has been studied. Cadmium extraction behavior at natural waters’ pH conditions (values in the range 7–8) was studied with two different extractants and co-ions, obtaining the highest extraction efficiency when using 0.1M Cyanex 272 in kerosene as organic phase and 0.1 M NO3− as co-ion. Once they were selected, the effect on the extraction efficiency of sample pH, buffer concentration, extraction time, Cyanex 272 concentration as well as back-extractant concentration, was studied. The presence of the main inorganic and organic ligands in the sample was also studied, observing that extraction efficiency was affected most significantly when chlorides were present, with a decrease of about 14%, proving negligible for the others. Under the selected conditions, spiked real samples were successfully analyzed.
{"title":"Solvent extraction with organophosphorus extractants in environmental samples: determination of cadmium(II) in natural water","authors":"V. Mánuel, J. Pinto, Carolina Mendiguchía, C. Moreno","doi":"10.2478/s11532-013-0379-0","DOIUrl":"https://doi.org/10.2478/s11532-013-0379-0","url":null,"abstract":"AbstractIn this work, Cd(II) extraction in natural waters by organophosphorus extractants as organic phase, as well as its back-extraction in an acidic media, has been studied. Cadmium extraction behavior at natural waters’ pH conditions (values in the range 7–8) was studied with two different extractants and co-ions, obtaining the highest extraction efficiency when using 0.1M Cyanex 272 in kerosene as organic phase and 0.1 M NO3− as co-ion. Once they were selected, the effect on the extraction efficiency of sample pH, buffer concentration, extraction time, Cyanex 272 concentration as well as back-extractant concentration, was studied. The presence of the main inorganic and organic ligands in the sample was also studied, observing that extraction efficiency was affected most significantly when chlorides were present, with a decrease of about 14%, proving negligible for the others. Under the selected conditions, spiked real samples were successfully analyzed.\u0000","PeriodicalId":9888,"journal":{"name":"Central European Journal of Chemistry","volume":"260 1","pages":"348-353"},"PeriodicalIF":0.0,"publicationDate":"2014-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74707473","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2014-03-01DOI: 10.2478/s11532-013-0384-3
J. Geng, B. Johnson, A. Wheatley, Jack Luo
AbstractUsing a very popular and commonly used surfactant sodium dodecylbenzene sulfonate (SDBS, C18H29SO3Na) for a case study, we report a new method of monitoring different forms of surfactant molecules in aqueous solution and measuring their critical micelle concentration (CMC) by ultraviolet-visible (UV-Vis) spectroscopy. The forms of SDBS micelles are also investigated by synthesizing and characterizing NiB nanoparticles using the micelles as molecular templates. In addition, the observed shifts of UV-Vis bands are analysed from the viewpoint of the electrons locations and distributions within the molecules and the possible overlap of their electronic orbitals between neighbouring molecules in each micelle.
{"title":"Spectroscopic route to monitoring individual surfactant ions and micelles in aqueous solution: A case study","authors":"J. Geng, B. Johnson, A. Wheatley, Jack Luo","doi":"10.2478/s11532-013-0384-3","DOIUrl":"https://doi.org/10.2478/s11532-013-0384-3","url":null,"abstract":"AbstractUsing a very popular and commonly used surfactant sodium dodecylbenzene sulfonate (SDBS, C18H29SO3Na) for a case study, we report a new method of monitoring different forms of surfactant molecules in aqueous solution and measuring their critical micelle concentration (CMC) by ultraviolet-visible (UV-Vis) spectroscopy. The forms of SDBS micelles are also investigated by synthesizing and characterizing NiB nanoparticles using the micelles as molecular templates. In addition, the observed shifts of UV-Vis bands are analysed from the viewpoint of the electrons locations and distributions within the molecules and the possible overlap of their electronic orbitals between neighbouring molecules in each micelle.","PeriodicalId":9888,"journal":{"name":"Central European Journal of Chemistry","volume":"5 1","pages":"307-311"},"PeriodicalIF":0.0,"publicationDate":"2014-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82467334","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2014-03-01DOI: 10.2478/s11532-013-0383-4
Qing-hai Zeng, Lu-Sheng Chen, Xian-Shuang Song, G. Hu, Lin-Yun Hu
AbstractThis paper reports a new method for determination of VB6 (pyridoxine hydrochloride) by its perturbation effects on a novel Belousov-Zhabotinskii (BZ) oscillating system. This novel BZ system, in which malic acid serves as the substrate, contains an enzyme-like complex, macrocyclic complex {[CuL](ClO4)2}, as catalyst. The ligand L in the complex is 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene. Results show that the addition of pyridoxine hydrochloride can perturb the oscillation amplitude and period, and the change of the oscillation amplitude is linearly proportional to the concentration of pyridoxine hydrochloride in the range of 5×10−7−2.5×10−4 M. The obtained RSD with seven samples is 3.073%. An assay of pharmaceutical tablets of vitamin B6 was evaluated. Some foreign ions were studied with respect to their possible influence on the determination of pyridoxine hydrochloride. The factors which influence this reaction include the concentration of reactant, the temperature of the reaction, property of catalyst, etc. Furthermore, the possible reaction mechanism has been proposed using the Field-Körös-Noyes (FKN) model.
{"title":"Determination of vitamin B6 (pyridoxine hydrochloride) based on a novel BZ oscillating reaction system catalyzed by a macrocyclic complex","authors":"Qing-hai Zeng, Lu-Sheng Chen, Xian-Shuang Song, G. Hu, Lin-Yun Hu","doi":"10.2478/s11532-013-0383-4","DOIUrl":"https://doi.org/10.2478/s11532-013-0383-4","url":null,"abstract":"AbstractThis paper reports a new method for determination of VB6 (pyridoxine hydrochloride) by its perturbation effects on a novel Belousov-Zhabotinskii (BZ) oscillating system. This novel BZ system, in which malic acid serves as the substrate, contains an enzyme-like complex, macrocyclic complex {[CuL](ClO4)2}, as catalyst. The ligand L in the complex is 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene. Results show that the addition of pyridoxine hydrochloride can perturb the oscillation amplitude and period, and the change of the oscillation amplitude is linearly proportional to the concentration of pyridoxine hydrochloride in the range of 5×10−7−2.5×10−4 M. The obtained RSD with seven samples is 3.073%. An assay of pharmaceutical tablets of vitamin B6 was evaluated. Some foreign ions were studied with respect to their possible influence on the determination of pyridoxine hydrochloride. The factors which influence this reaction include the concentration of reactant, the temperature of the reaction, property of catalyst, etc. Furthermore, the possible reaction mechanism has been proposed using the Field-Körös-Noyes (FKN) model.","PeriodicalId":9888,"journal":{"name":"Central European Journal of Chemistry","volume":"26 1","pages":"325-331"},"PeriodicalIF":0.0,"publicationDate":"2014-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85055013","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2014-03-01DOI: 10.2478/s11532-013-0387-0
V. Giurcan, D. Razus, M. Mitu, D. Oancea
AbstractThe structure of premixed free one-dimensional laminar ethane-air flames was investigated by means of numerical simulations performed with a detailed mechanism (GRI-Mech version 3.0) by means of COSILAB package. The work provides data on ethane-air mixtures with a wide range of concentrations ([C2H6] = 3.0–9.5 vol.%) at initial temperatures between 300 and 550 K and initial pressures between 1 and 10 bar. The simulations deliver the laminar burning velocities and the profiles of temperature, chemical species concentrations and heat release rate across the flame front. The predicted burning velocities match well the burning velocities measured in various conditions, reported in literature. The influence of initial concentration, pressure and temperature of ethane-air mixtures on maximum flame temperature, heat release rate, flame thickness and peak concentrations of main reaction intermediates is examined and discussed.
{"title":"Numerical study of the laminar flame propagation in ethane-air mixtures","authors":"V. Giurcan, D. Razus, M. Mitu, D. Oancea","doi":"10.2478/s11532-013-0387-0","DOIUrl":"https://doi.org/10.2478/s11532-013-0387-0","url":null,"abstract":"AbstractThe structure of premixed free one-dimensional laminar ethane-air flames was investigated by means of numerical simulations performed with a detailed mechanism (GRI-Mech version 3.0) by means of COSILAB package. The work provides data on ethane-air mixtures with a wide range of concentrations ([C2H6] = 3.0–9.5 vol.%) at initial temperatures between 300 and 550 K and initial pressures between 1 and 10 bar. The simulations deliver the laminar burning velocities and the profiles of temperature, chemical species concentrations and heat release rate across the flame front. The predicted burning velocities match well the burning velocities measured in various conditions, reported in literature. The influence of initial concentration, pressure and temperature of ethane-air mixtures on maximum flame temperature, heat release rate, flame thickness and peak concentrations of main reaction intermediates is examined and discussed.\u0000","PeriodicalId":9888,"journal":{"name":"Central European Journal of Chemistry","volume":"51 1","pages":"391-402"},"PeriodicalIF":0.0,"publicationDate":"2014-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85613885","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2014-03-01DOI: 10.2478/s11532-013-0374-5
M. Shoukry, Safaa S. Hassan
AbstractComplex formation equilibria of 1-aminocyclopropane carboxylic acid (ACC) and 3,3-bis(1-methylimidazol-2-yl) propionic acid (BIMP) with metal ions Cu2+, Ni2+, Co2+, Zn2+, Mn2+ and Fe2+ were investigated. ACC forms 1:1 and 1:2 complexes in addition to the hydrolysed form of the 1:1 complex, except in the case of Mn2+ and Fe2+, where the hydrolysed complex is not formed. BIMP forms 1:1 and 1:2 complexes in addition to the hydrolsed form of the 1:1 complex in the case of Mn2+ and Cu2+, however the hydrolysed complex is not detected for Ni2+, Co2+, Zn2+ and Fe2+. The concentration distribution diagrams of the complexes were determined. The Fe2+-complex with BIMP is exothermic and the thermodynamic parameters were calculated. The effect of organic solvent on the acid dissociation constants of 1-aminocyclopropane carboxylic acid (ACC) and 3,3-bis(1-methylimidazol-2-yl) propionic acid (BIMP) and the formation constants of Fe2+ complexes were investigated. Fe2+ forms a mixed-ligand complex with ACC and BIMP with stoichiometric coefficients 1:1:1. The formation constant was determined. The ternary complex is enhanced by back donation from the negatively charged 1-aminocyclopropane carboxylate to the π-system of BIMP. From the concentration distribution diagram, the ternary complex prevails in the physiological pH range.
{"title":"Thermodynamic investigation of the binary and ternary complexes involving 1-aminocyclopropane carboxylic acid with reference to plant hormone","authors":"M. Shoukry, Safaa S. Hassan","doi":"10.2478/s11532-013-0374-5","DOIUrl":"https://doi.org/10.2478/s11532-013-0374-5","url":null,"abstract":"AbstractComplex formation equilibria of 1-aminocyclopropane carboxylic acid (ACC) and 3,3-bis(1-methylimidazol-2-yl) propionic acid (BIMP) with metal ions Cu2+, Ni2+, Co2+, Zn2+, Mn2+ and Fe2+ were investigated. ACC forms 1:1 and 1:2 complexes in addition to the hydrolysed form of the 1:1 complex, except in the case of Mn2+ and Fe2+, where the hydrolysed complex is not formed. BIMP forms 1:1 and 1:2 complexes in addition to the hydrolsed form of the 1:1 complex in the case of Mn2+ and Cu2+, however the hydrolysed complex is not detected for Ni2+, Co2+, Zn2+ and Fe2+. The concentration distribution diagrams of the complexes were determined. The Fe2+-complex with BIMP is exothermic and the thermodynamic parameters were calculated. The effect of organic solvent on the acid dissociation constants of 1-aminocyclopropane carboxylic acid (ACC) and 3,3-bis(1-methylimidazol-2-yl) propionic acid (BIMP) and the formation constants of Fe2+ complexes were investigated. Fe2+ forms a mixed-ligand complex with ACC and BIMP with stoichiometric coefficients 1:1:1. The formation constant was determined. The ternary complex is enhanced by back donation from the negatively charged 1-aminocyclopropane carboxylate to the π-system of BIMP. From the concentration distribution diagram, the ternary complex prevails in the physiological pH range.\u0000","PeriodicalId":9888,"journal":{"name":"Central European Journal of Chemistry","volume":"1 1","pages":"318-324"},"PeriodicalIF":0.0,"publicationDate":"2014-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82325917","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2014-03-01DOI: 10.2478/s11532-013-0380-7
Sheraz A. K. Tanoli, Nazish U. Tanoli, Saman Usmani, Zaheer-ul-Haq, A. Ferreira
AbstractLarger size or novel structure molecules are always appreciated by all fields of experimental and computational science. Conversely, molecules with smaller size and simple structures are usually ignored with no explanation as to why. However, the vast majority of more diminutive molecules behave as a cornerstone in the synthesis of a bigger structural framework. Subsequently, we planned to uncover the interactions of small molecules towards macromolecules, and successfully presented the binding results of 2-aminopyridine and Isovanillin towards BSA through NMR techniques. STD epitope mapping and also the DOSY results provided evidence that Isovanillin remained closer to the binding cavity of protein. Titration experiments afforded 584 µM (0.584mM) and 487 µM (0.487 mM) dissociation constants for isovanillin and 2-aminopyridine respectively. Furthermore, changes in diffusion coefficient (with and without protein addition in DOSY spectra) were found to be 0.081 log (m2 s−1) and 0.096 log (m2 s−1) points for isovanillin and 2-aminopyridine respectively. Docking studies exhibit that these molecules can tie to site 1 (sub-area IIA) through the pi-pi interaction and hydrogen bonding with Trp213. Our results demonstrated that both compounds could be utilized as part of a transporter in the circulatory system and their extension-inspired compounds may be utilized in new drug design.
{"title":"The exploration of interaction studies of smaller size, mostly ignored yet intrinsically inestimable molecules towards BSA; An example of STD and DOSY NMR","authors":"Sheraz A. K. Tanoli, Nazish U. Tanoli, Saman Usmani, Zaheer-ul-Haq, A. Ferreira","doi":"10.2478/s11532-013-0380-7","DOIUrl":"https://doi.org/10.2478/s11532-013-0380-7","url":null,"abstract":"AbstractLarger size or novel structure molecules are always appreciated by all fields of experimental and computational science. Conversely, molecules with smaller size and simple structures are usually ignored with no explanation as to why. However, the vast majority of more diminutive molecules behave as a cornerstone in the synthesis of a bigger structural framework. Subsequently, we planned to uncover the interactions of small molecules towards macromolecules, and successfully presented the binding results of 2-aminopyridine and Isovanillin towards BSA through NMR techniques. STD epitope mapping and also the DOSY results provided evidence that Isovanillin remained closer to the binding cavity of protein. Titration experiments afforded 584 µM (0.584mM) and 487 µM (0.487 mM) dissociation constants for isovanillin and 2-aminopyridine respectively. Furthermore, changes in diffusion coefficient (with and without protein addition in DOSY spectra) were found to be 0.081 log (m2 s−1) and 0.096 log (m2 s−1) points for isovanillin and 2-aminopyridine respectively. Docking studies exhibit that these molecules can tie to site 1 (sub-area IIA) through the pi-pi interaction and hydrogen bonding with Trp213. Our results demonstrated that both compounds could be utilized as part of a transporter in the circulatory system and their extension-inspired compounds may be utilized in new drug design.\u0000","PeriodicalId":9888,"journal":{"name":"Central European Journal of Chemistry","volume":"38 1","pages":"332-340"},"PeriodicalIF":0.0,"publicationDate":"2014-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78047827","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2014-03-01DOI: 10.2478/s11532-013-0388-z
M. Idowu, Yasin Arslanoğlu, T. Nyokong
AbstractPeripherally and non-peripherally tetrasubstituted-[(N-methyl-2-pyridylthio)]phthalocyaninato magnesium (II) (5 and 6) and chloro aluminium (III) (7 and 8) tetraiodide have been synthesized and characterized. The photophysical properties of the complexes in dimethyl sulfoxide (DMSO) and aqueous medium in the presence and absence of cremophore EL have been studied. These complexes show high solubility in aqueous medium though they were aggregated. The triplet state quantum yields (FT) and the triplet lifetimes (tT) were found to be higher in DMSO with ΦT ranging from 0.32 to 0.51, while tT ranged from 282 to 622 ms in DMSO, compared to aqueous medium (pH 7.4 buffer) where ΦT ranged from 0.15 to 0.19 and tT from 26 to 35 ms. Addition of cremophore EL in aqueous solution resulted in partial disaggregation and increased photoactivity. The fluorescence lifetimes of the complexes showed strong dependence on their immediate environment. The ionic magnesium(II) and aluminium(III) phthalocyanines strongly bind to bovine serum albumin (BSA).
{"title":"Spectral properties and photophysical behaviour of water soluble cationic Mg(II) and Al(III) phthalocyanines","authors":"M. Idowu, Yasin Arslanoğlu, T. Nyokong","doi":"10.2478/s11532-013-0388-z","DOIUrl":"https://doi.org/10.2478/s11532-013-0388-z","url":null,"abstract":"AbstractPeripherally and non-peripherally tetrasubstituted-[(N-methyl-2-pyridylthio)]phthalocyaninato magnesium (II) (5 and 6) and chloro aluminium (III) (7 and 8) tetraiodide have been synthesized and characterized. The photophysical properties of the complexes in dimethyl sulfoxide (DMSO) and aqueous medium in the presence and absence of cremophore EL have been studied. These complexes show high solubility in aqueous medium though they were aggregated. The triplet state quantum yields (FT) and the triplet lifetimes (tT) were found to be higher in DMSO with ΦT ranging from 0.32 to 0.51, while tT ranged from 282 to 622 ms in DMSO, compared to aqueous medium (pH 7.4 buffer) where ΦT ranged from 0.15 to 0.19 and tT from 26 to 35 ms. Addition of cremophore EL in aqueous solution resulted in partial disaggregation and increased photoactivity. The fluorescence lifetimes of the complexes showed strong dependence on their immediate environment. The ionic magnesium(II) and aluminium(III) phthalocyanines strongly bind to bovine serum albumin (BSA).\u0000","PeriodicalId":9888,"journal":{"name":"Central European Journal of Chemistry","volume":"98 1","pages":"403-415"},"PeriodicalIF":0.0,"publicationDate":"2014-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85763494","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2014-02-21DOI: 10.2478/s11532-014-0525-3
B. Gierczyk, R. Pankiewicz
AbstractFormation of stable complexes between xenon and podand polyoxyethylene ligands was ascertained. The complexation process was studied by 129Xe NMR titration, NMR diffusiometry and heteronuclear NOE measurements. The ligands studied form a 1:1 complexes with Xe(0). Their stability constants depend on the ligand structure, i.e., polyoxyethylene chain length, number of complexating polyether units and the topology of the anchoring centre.
{"title":"Supramolecular complexes of podand ligands with xenon","authors":"B. Gierczyk, R. Pankiewicz","doi":"10.2478/s11532-014-0525-3","DOIUrl":"https://doi.org/10.2478/s11532-014-0525-3","url":null,"abstract":"AbstractFormation of stable complexes between xenon and podand polyoxyethylene ligands was ascertained. The complexation process was studied by 129Xe NMR titration, NMR diffusiometry and heteronuclear NOE measurements. The ligands studied form a 1:1 complexes with Xe(0). Their stability constants depend on the ligand structure, i.e., polyoxyethylene chain length, number of complexating polyether units and the topology of the anchoring centre.\u0000","PeriodicalId":9888,"journal":{"name":"Central European Journal of Chemistry","volume":"19 1","pages":"624-634"},"PeriodicalIF":0.0,"publicationDate":"2014-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78037627","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2014-02-21DOI: 10.2478/s11532-014-0511-9
M. K. Riekes, G. Kuminek, G. S. Rauber, S. Cuffini, H. K. Stulzer
AbstractThe polymorphs of nimodipine, Modification I (Mod I), the metastable racemate, and Modification II (Mod II), the stable conglomerate, were evaluated by means of the intrinsic dissolution procedure. For this purpose, a hydro alcoholic solution (ethanol:water, 50:50, v/v) was selected as the dissolution medium, maintained at 37±0.5°C. Different rotation speeds were tested (50, 75 and 100 rpm) and the lower one was chosen for the test validation. Although the sample initially characterized as polymorph Mod I presented higher intrinsic dissolution rates in all the conditions tested, no statistical differences were noticed between the two polymorphs. This result can be attributed to the partial solution-mediated phase transformation from Mod I to Mod II, detected through X-ray powder diffraction and differential scanning calorimetry. Also, reliable intrinsic dissolution rate data were acquired for the polymorph Mod II. The dissolution method was validated, being considered stable, specific, linear, sensible, accurate and precise.
{"title":"Development and validation of an intrinsic dissolution method for nimodipine polymorphs","authors":"M. K. Riekes, G. Kuminek, G. S. Rauber, S. Cuffini, H. K. Stulzer","doi":"10.2478/s11532-014-0511-9","DOIUrl":"https://doi.org/10.2478/s11532-014-0511-9","url":null,"abstract":"AbstractThe polymorphs of nimodipine, Modification I (Mod I), the metastable racemate, and Modification II (Mod II), the stable conglomerate, were evaluated by means of the intrinsic dissolution procedure. For this purpose, a hydro alcoholic solution (ethanol:water, 50:50, v/v) was selected as the dissolution medium, maintained at 37±0.5°C. Different rotation speeds were tested (50, 75 and 100 rpm) and the lower one was chosen for the test validation. Although the sample initially characterized as polymorph Mod I presented higher intrinsic dissolution rates in all the conditions tested, no statistical differences were noticed between the two polymorphs. This result can be attributed to the partial solution-mediated phase transformation from Mod I to Mod II, detected through X-ray powder diffraction and differential scanning calorimetry. Also, reliable intrinsic dissolution rate data were acquired for the polymorph Mod II. The dissolution method was validated, being considered stable, specific, linear, sensible, accurate and precise.\u0000","PeriodicalId":9888,"journal":{"name":"Central European Journal of Chemistry","volume":"77 1","pages":"549-556"},"PeriodicalIF":0.0,"publicationDate":"2014-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78327109","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2014-02-21DOI: 10.2478/s11532-014-0513-7
M. Pisarčik, F. Devínsky
AbstractBinding of cationic gemini surfactants alkanediyl-a-ω-bis(dimethyldodecylammonium bromides) with variable polymethylene spacer length ranging from 2 to 12 methylene groups to DNA in NaBr solution is investigated utilizing the tensiometry method. A simple method is presented for calculating the number of surfactant molecules bound to DNA. The results are evaluated in terms of the gemini surfactant spacer length, showing that gemini molecules with either short spacers (2 methylene groups) or long spacers are most efficiently adsorbed to DNA. A weak adsorption to DNA was found for gemini molecules with a medium spacer length (6 methylene groups in the spacer). The binding properties of cationic gemini surfactants as a function of spacer length are consistent with the results obtained by other experimental methods (dynamic light scattering measurements, fluorescence spectroscopy), indicating identical adsorption behaviour of gemini molecules as a function of the spacer length.
{"title":"Surface tension study of cationic gemini surfactants binding to DNA","authors":"M. Pisarčik, F. Devínsky","doi":"10.2478/s11532-014-0513-7","DOIUrl":"https://doi.org/10.2478/s11532-014-0513-7","url":null,"abstract":"AbstractBinding of cationic gemini surfactants alkanediyl-a-ω-bis(dimethyldodecylammonium bromides) with variable polymethylene spacer length ranging from 2 to 12 methylene groups to DNA in NaBr solution is investigated utilizing the tensiometry method. A simple method is presented for calculating the number of surfactant molecules bound to DNA. The results are evaluated in terms of the gemini surfactant spacer length, showing that gemini molecules with either short spacers (2 methylene groups) or long spacers are most efficiently adsorbed to DNA. A weak adsorption to DNA was found for gemini molecules with a medium spacer length (6 methylene groups in the spacer). The binding properties of cationic gemini surfactants as a function of spacer length are consistent with the results obtained by other experimental methods (dynamic light scattering measurements, fluorescence spectroscopy), indicating identical adsorption behaviour of gemini molecules as a function of the spacer length.\u0000","PeriodicalId":9888,"journal":{"name":"Central European Journal of Chemistry","volume":"690 1","pages":"577-585"},"PeriodicalIF":0.0,"publicationDate":"2014-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73502003","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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