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Different Analytical Techniques (different + analytical_techniques)
Selected AbstractsProcess induced disorder in crystalline materials: Differentiating defective crystals from the amorphous form of griseofulvinJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 8 2008Tao Feng Abstract This research investigates milling induced disorder in crystalline griseofulvin. Griseofulvin was subjected to cryogenic milling for various lengths of time. For comparison, the amorphous form of griseofulvin was also prepared by the quench melt method. Different analytical techniques were used to study the differences between the cryomilled, amorphous and crystalline forms of the drug. Cryogenic milling of griseofulvin progressively reduces the crystallinity of the drug by inducing crystal defects, rather than amorphous materials. Raman analysis provides evidence of structural differences between the two. The differences between the defective crystals produced by milling and the amorphous form are significant enough as to be measurable in their bulk thermal properties. Defective crystals show significant decrease in the heat of fusion as a function of milling time but do not exhibit a glass transition nor recrystallization from the amorphous form. Crystal defects undergo recrystallization upon heating at temperatures well below the glass transition temperature (Tg) in a process that is separate and completely independent from the crystallization of the amorphous griseofulvin, observed above Tg. Physical mixtures of defective crystals and amorphous drug demonstrate that the thermal events associated with each form persist in the mixtures, unaffected by the presence of the other form. © 2007 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 97: 3207,3221, 2008 [source] Kharasch-Type Cyclizations of 2-Substituted Indole Derivatives Surprisingly Lead to SpiroindolesEUROPEAN JOURNAL OF ORGANIC CHEMISTRY, Issue 28 2010Sarah Van der Jeught Abstract Starting from 1H -indole-2-carboxylic acid, a series of spiro[2-oxoindole-pyrrolidines] could be synthesized in a straightforward manner. The key reaction is a Kharasch radical cyclization reaction of trichloroacetylated precursors. The identity of the tricyclic final products that were formed could be determined as spiro[2-oxoindole-pyrrolidines] by using a combination of different analytical techniques (1H NMR, 13C NMR, gHMBC, HRMS) and additional reactions. The produced skeletons are interesting from a medicinal point of view. [source] Elimination and exchange of trifluoroacetate counter-ion from cationic peptides: a critical evaluation of different approachesJOURNAL OF PEPTIDE SCIENCE, Issue 3 2008Stéphane Roux Abstract Most synthesized peptides are nowadays produced using solid-phase procedures. Due to cleavage and purification conditions, they are mainly obtained in the presence of trifluoroacetic acid (TFA) and, for cationic peptides, as trifluoroacetate (TF-acetate) salts. However, TF-acetate interferes with physicochemical characterizations using infrared spectroscopy and might significantly affect the in vivo studies. Thus, TF-acetate exchange by another counter-ion is often required. Up to now, the classical procedure has consisted of freeze-drying the peptide several times in the presence of an excess of a stronger acid than TFA (pKa ,0): generally HCl (pKa = , 7). This approach means that working at pH < 1 can induce peptide degradation. We therefore tested three different approaches to exchange the tightly bound TF-acetate counter-ion from the dicationic octapeptide lanreotide: (i) reverse-phase HPLC, (ii) ion-exchange resin, and (iii) deprotonation/reprotonation cycle of the amino groups. The first two approaches allow the partial to almost complete exchange of the TF-acetate counter-ion by another ion from an acid weaker than TFA, such as acetic acid (pKa = 4.5), and the third requires a basic solution that permits the complete removal of TF-acetate counter-ion. The efficiency of these three procedures was tested and compared by using different analytical techniques such as 19F-NMR, 1H-NMR and attenuated total reflectance Fourier transformed infrared spectroscopy (ATR FT-IR). We also show that ATR-IR can be used to monitor the TFA removal. The counter-ion exchange procedures described in this study are easy to carry out, fast, harmless and reproducible. Moreover, two of them offer the very interesting possibility of exchanging the initial TF-acetate by any other counter-ion. Copyright © 2007 European Peptide Society and John Wiley & Sons, Ltd. [source] Characterization of New Amphiphilic Block Copolymers of N -Vinyl Pyrrolidone and Vinyl Acetate, 1 , Analysis of Copolymer Composition, End Groups, Molar Masses and Molar Mass Distributions,MACROMOLECULAR CHEMISTRY AND PHYSICS, Issue 8 2010Nick Fandrich Abstract New amphiphilic block copolymers consisting of N -vinyl pyrrolidone and vinyl acetate were synthesized via controlled radical polymerization using a reversible addition/fragmentation chain transfer (RAFT)/macromolecular design via the interchange of xanthates (MADIX) system. The synthesis was carried out in 1,4-dioxane as process solvent. In order to get conclusions on the mechanism of the polymerization the molecular structure of formed copolymers was analysed by means of different analytical techniques. 13C NMR spectroscopy was used for the determination of the monomer ratios. End groups were analysed by means of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. This technique was also used to determine possible fragmentations of the RAFT end groups. By means of a combination of size exclusion chromatography, 13C NMR and static light scattering molar mass distributions and absolute molar masses could be analysed. The results clearly show a non-ideal RAFT mechanism. [source] Has social mobility in Britain decreased?THE BRITISH JOURNAL OF SOCIOLOGY, Issue 2 2010Reconciling divergent findings on income, class mobility Abstract Social mobility has become a topic of central political concern. In political and also media circles it is widely believed that in Britain today mobility is in decline. However, this belief appears to be based on a single piece of research by economists that is in fact concerned with intergenerational income mobility: specifically, with the relation between family income and children's later earnings. Research by sociologists using the same data sources , the British birth cohort studies of 1958 and 1970 , but focusing on intergenerational class mobility does not reveal a decline either in total mobility rates or in underlying relative rates. The paper investigates these divergent findings. We show that they do not result from the use of different subsets of the data or of different analytical techniques. Instead, given the more stable and generally less fluid class mobility regime, it is the high level of income mobility of the 1958 cohort, rather than the lower level of the 1970 cohort, that is chiefly in need of explanation. Further analyses , including ones of the relative influence of parental class and of family income on children's educational attainment , suggest that the economists' finding of declining mobility between the two cohorts may stem, in part at least, from the fact that the family income variable for the 1958 cohort provides a less adequate measure of ,permanent income' than does that for the 1970 cohort. But, in any event, it would appear that the class mobility regime more fully captures the continuity in economic advantage and disadvantage that persists across generations. [source] ANALYSIS OF ROMAN WALL PAINTINGS FROM THE THERMAE OF ,IULIA CONCORDIA'ARCHAEOMETRY, Issue 4 2010G. A. MAZZOCCHIN Twenty-six wall painting fragments and some plaster, ,intonachino' and stucco samples, discovered at Iulia Concordia, have been studied by different analytical techniques to gain information about the pigment nature and the composition of the materials. The presence of calcite, dolomite and aragonite allow the distinction of four groups of wall samples varying in the nature of pigments and in the application technique. These differences can be attributed to different execution times or, more probably, to the arrangement of the rooms in the building structure. The nature of the pigments found in the Thermae of Iulia Concordia appears similar to that found in other Roman villas of Venetia et Histria, with the use of precious pigments such as Egyptian blue and cinnabar. [source] Biomarkers for detection of prenatal alcohol exposure: A critical review of fatty acid ethyl esters in meconium,,BIRTH DEFECTS RESEARCH, Issue 7 2008Larry Burd Abstract BACKGROUND: The objective of this study was a review of published studies utilizing measurement of fatty acid ethyl esters (FAEE) in meconium as biomarkers for prenatal alcohol exposure. METHODS: We completed a literature search of PubMed using the terms meconium, fatty acid ethyl esters, biomarkers, and prenatal alcohol exposure. We included only peer reviewed studies utilizing analysis of meconium for the presence of FAEE in humans through the year 2007. RESULTS: We found 10 articles reporting on original research examining the relationship of FAEE from meconium and prenatal alcohol exposure (PAE). The 10 articles used six different PAE assessment strategies and four different analytical techniques for determining FAEE endpoints. The articles included 2,221 subjects (range 4 to 725) with 455 (20.5%) subjects identified as exposed using the methods stated in the articles. FAEE levels above the studies' respective cutoffs were reported for 502 (22.6%) subjects. CONCLUSIONS: The accurate identification of alcohol-exposed pregnancies represents a significant challenge in the development of FAEE detection cutoffs to maximize the sensitivity and specificity of the test. We present several options for the improvement of exposure assessment in future studies of FAEE as biomarkers for PAE. Birth Defects Research (Part A), 2008. © 2008 Wiley-Liss, Inc. [source] | |||||||||||||