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101.
Carmela Maria Montone Michela Antonelli Anna Laura Capriotti Chiara Cavaliere Giorgia La Barbera Susy Piovesana Aldo Lagan 《Journal of separation science》2019,42(10):1938-1947
An analytical method for determining seleno‐methionine, methyl‐seleno‐cysteine, and seleno‐cystine in wheat bran was developed and validated. Four different extraction procedures were evaluated to simultaneously extract endogenous free and conjugated seleno‐amino acids in wheat bran in order to select the best extraction protocol in terms of seleno amino acid quantitation. The extracted samples were subjected to a clean‐up by a reversed phase/strong cation exchange solid‐phase extraction and analyzed by chiral hydrophilic interaction liquid chromatography‐tandem mass spectrometry. The optimized extraction protocol was employed to validate the methodology. Process efficiency ranged from 58 to 112% and trueness from 73 to 98%. Limit of detection and limit of quantification were lower than 1 ng/g. Four wheat bran samples were analyzed for both total Se and single seleno‐amino acids determination. The results showed that Se‐ seleno‐methyl‐l selenocysteine was the major seleno‐amino acid in wheat bran while seleno‐methionine and seleno‐cysteine were both minor species. 相似文献
102.
103.
Host–Guest Chemistry of a Bis‐Calix[4]pyrrole Derivative Containing a trans/cis‐Switchable Azobenzene Unit with Several Aliphatic Bis‐Carboxylates
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Grazia Cafeo Franz H. Kohnke Giovanni Mezzatesta Aldo Profumo Camillo Rosano Antonino Villari Andrew J. P. White 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(14):5323-5327
The azobenzene unit used as a photochemically and thermally switchable linker in the assembly of a bis‐calix[4]pyrrole receptor provides a means to modulate the binding of bis‐carboxylates of significant biological importance in cancer research. Conversely, the complexation of different bis‐anionic guests has significant kinetic effects on both the photochemical and thermal trans/cis isomerization of the azobenzene unit. 相似文献
104.
Silvia Rita Amato Aviva Burnstock Maureen Cross Koen Janssens Francesca Rosi Laura Cartechini Raffaella Fontana Alice Dal Fovo Marco Paolantoni Chiara Grazia Aldo Romani Anne Michelin Christine Andraud Aurélie Tournié Joris Dik 《X射线光谱测定》2019,48(4):282-292
The paintings by Édouard Manet in The Courtauld Gallery Déjeuner sur l'herbe (1863–68), Marguerite de Conflans en Toilette de Bal (1870–1880), Banks of the Seine at Argenteuil (1874), and A Bar at the Folies–Bergère (1882) were investigated for the first time using a range of non-invasive in situ analyses. The aims of the study were to investigate the painting techniques and materials used for this group of works and to critically evaluate the technical evidence derived from the integrated use of imaging techniques and portable spectroscopic methods in this context. The paintings were investigated by means of macro X-ray fluorescence (MA-XRF), reflection spectral imaging, portable UV–Vis–NIR spectroscopy, portable Raman spectroscopy, and reflection FTIR. MA-XRF and reflection spectral imaging allowed visualising elements in the compositions that were not visible using traditional methods of technical study. For example, MA-XRF analysis of Déjeuner sur l'herbe revealed elements of the development of the composition that provided new evidence to consider its relationship to other versions of the composition. The study also highlighted questions about the interpretation of elemental distribution maps and spectral images that did not correspond to the reworking visible in X-radiographs. For example, in A Bar at the Folies–Bergère Manet made numerous changes during painting, which were not clearly visualised with any of the techniques used. The research has wider implications for the study of Impressionist paintings, as the results will support technical studies of works by other artists of the period who used similar materials and painting methods. 相似文献
105.
106.
Several experimental techniques are used to study the short range order, the dynamics and the glass transition in AgIAg2B2O3 compounds. Addition of Ag2O to B2O3, up to [Ag2O]/[B2O3] ?0.5 modifies the borate network by creating a BO4 unit for each silver added. Addition of AgI decreases the glass transition temperature (Tg) but has only minor effects on the short range structure of the borate network. Silver iodide is partially accomodated in the interstices of the glass network. The relationship among a tentative structural picture, the ion transport phenomena and the low temperature dynamics are discussed.An investigation of the dynamics in the AgI·Ag2O·2B2O3 glass near and above Tg is presented. With NMR techniques, we monitor the onset of tumbling of the borate units and the dynamical effects of crystallization and/or aging of the glass. Hysteresis effects in the ionic conductivity (σ) temperature dependence and the non-Arrhenian behavior of σT near Tg are interpreted in terms of structural modifications occurring at elevated temperatures in the glass. 相似文献
107.
Jongejan A Lim HD Smits RA de Esch IJ Haaksma E Leurs R 《Journal of chemical information and modeling》2008,48(7):1455-1463
A three-dimensional homology model of the human histamine H 4 receptor was developed to investigate the binding mode of a series of structurally diverse H 4-agonists, i.e. histamine, clozapine, and the recently described selective, nonimidazole agonist VUF 8430. Mutagenesis studies and docking of these ligands in a rhodopsin-based homology model revealed two essential points of interactions in the binding pocket, i.e. Asp3.32 and Glu5.46 (Ballesteros-Weinstein numbering system). It is postulated that Asp3.32 interacts in its anionic state, whereas Glu5.46 interacts in its neutral form. The hypothesis was tested with the point mutations D3.32N and E5.46Q. For the D3.32N no binding affinity toward any of the ligands could be detected. This is in sharp contrast to the E5.46Q mutant, which discriminates between various ligands. The affinity of histamine-like ligands was decreased approximately a 1000-fold, whereas the affinity of all other ligands remained virtually unchanged. The proposed model for agonist binding as well as ab initio calculations for histamine and VUF 8430 explain the observed differences in binding to the H 4R mutants. These studies provide a molecular understanding for the action of a variety of H 4 receptor-ligands. The resulting H 4 receptor model will be the basis for the development of new H 4 receptor-ligands. 相似文献
108.
Bizzarri M Cavaliere C Foglia P Guarino C Samperi R Laganà A 《Analytical and bioanalytical chemistry》2008,391(5):1969-1976
A label-free absolute quantitation method based on matrix-assisted laser desorption/ionization time-of-flight mass spectrometry
(MALDI-TOF MS) has been developed. This methodology was applied to mouse heart in order to quantify cardiac troponin T (cTnT),
which is considered to be a sensitive marker of heart damage. The cTnT was extracted, isolated by reversed-phase high-performance
liquid chromatography, digested, and analyzed by MALDI-TOF MS. The MS-based quantitation was performed using matrix-matched
calibration curves (due to a matrix effect) of two synthetic peptides, one cTnT-specific peptide and one internal standard
peptide, respectively. Recoveries at three spiking levels ranged from 87–96%, with relative standard deviations of below 10%.
The method detection limit and the method quantitation limit, expressed as the amount of cTnT for the amount of total sarcomeric
protein extract, were 0.03 mg g−1 and 0.15 mg g−1, respectively. This method appears to be accurate and generally suitable for improving absolute protein quantitation. 相似文献
109.
Maria R. di Nunzio Dr. Pier L. Gentili Dr. Aldo Romani Dr. Gianna Favaro Prof. 《Chemphyschem》2008,9(5):768-775
The photochromic and thermochromic behavior of four commercially available Reversacol dyes are presented. The compounds studied belong to the class of spirooxazines and naphthopyrans, which are typically thermoreversible photochromic molecules. On stimulation with UV light, these compounds become colored and exhibit spectra which extend over the whole visible region. Increasing the temperature causes spontaneous coloration (thermochromism). Herein, absorption and fluorescence spectra, molar absorption coefficients of the colorless and colored forms, fluorescence and photochemical quantum yields, and kinetic parameters of thermal bleaching (rate constant, frequency factor, and activation energy) are determined in acetonitrile solution. The thermal ground‐state reaction is exhaustively described in terms of thermodynamic parameters (equilibrium constant, free energy, enthalpy, and entropy). Temperature effects on photochemical and thermal colorabilities are evaluated. The results indicate that the two spirooxazines are good photochromes below room temperature, whereas they are efficient thermochromic compounds above room temperature. Naphthopyrans are better photochromes but worse thermochromic compounds than spirooxazines. 相似文献
110.
Bacaloni A Cavaliere C Cucci F Foglia P Samperi R Laganà A 《Journal of chromatography. A》2008,1179(2):182-189
A sensitive and reliable liquid chromatography-tandem mass spectrometric with electrospray ionization method for determining aflatoxins in hazelnuts has been developed. Three different extraction techniques, such as homogenization, ultrasonic extraction, and matrix solid phase dispersion have been tested and compared in terms of recovery, matrix effect, accuracy and precision. Ultrasound extraction was the most performing sample preparation method. Absolute recoveries for analytes and I.S. ranged from 93 to 101%. Accuracy and precision were calculated using matrix matched calibration, and ranged 91-102% and 2-11%, respectively. CC alpha and CC beta for aflatoxin B1 (EU limit=2 microg/kg) were 2.15 and 2.33 microg/kg, respectively. A ruggedness test performed on three other matrices demonstrated that sonication time was critical and a matrix matched calibration must be constructed for every sort of matrix. 相似文献