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181.
Analytical quality by design in the development of a cyclodextrin‐modified capillary electrophoresis method for the assay of metformin and its related substances
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Serena Orlandini Benedetta Pasquini Roberto Gotti Alessandro Giuffrida Ferdinando Paternostro Sandra Furlanetto 《Electrophoresis》2014,35(17):2538-2545
Quality by Design (QbD) is a new paradigm of quality to be applied to pharmaceutical products and processes, recently encouraged by International Conference on Harmonisation guidelines. In this paper QbD approach was applied to the development of a CE method for the simultaneous assay of metformin hydrochloride (MET) and its main impurities. QbD strategy was focused on electrophoretic process understanding, and the analytical method was thoroughly evaluated by applying risk assessment and chemometric tools. Method scouting allowed CD‐CZE based on the addition of carboxymethyl‐β‐CD to Britton‐Robinson acidic buffer to be chosen as operative mode. Seven critical process parameters (CPPs) were selected, related to capillary, injection, BGE and instrumental settings. The effect of the different levels of the CPPs on critical quality attributes (CQAs), e.g. critical resolution values and analysis time, was evaluated in a screening study. Response surface methodology led to draw contour plots and sweet spot plots. The definition of design space was accomplished by applying Monte‐Carlo simulations, thus identifying by risk of failure maps a multivariate zone where the CQAs fulfilled the requirements with a selected probability. Finally, a control strategy was designed and the method was applied to a real sample of MET tablets. 相似文献
182.
3D‐printed photo‐spectroelectrochemical devices for in situ and in operando X‐ray absorption spectroscopy investigation
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183.
Gentili PL Presciutti F Evangelisti F Costantino F 《Chemistry (Weinheim an der Bergstrasse, Germany)》2012,18(14):4296-4307
A new family of layered metal(III)-phosphono-carboxylate nanostructures (M=Y, Eu, Tb, Er, and Yb) was hydrothermally synthesized and their structures and morphologies were characterized by X-ray powder diffraction and TEM. 4-[Bis(phosphonomethyl)amino]caproic acid and 4- [bis(phosphonomethyl)amino]undecanoic acid, with general formula (H(2)O(3)PCH(2))(2)NR (R=C(5)H(10)COOH(P2CAPR) and C(10)H(22)COOH(P2UND), respectively) were used as building blocks for the preparation of novel layered hybrid materials in which the inorganic layers were composed of MO(7) or MO(8) polyhedra and PO(3)C tetrahedra. The interlayer region was occupied by carboxyalkyl chains. These layered compounds were easily dispersed as stable solutions in alkylamine/water upon ultrasonication. These dispersions were constituted of rectangular elongated nanoparticles (NPs), which showed a distribution of sizes ranging from 20-500 nm. These new materials had interesting photophysical properties because they were multiluminescent compounds. These properties gave rise to several emission bands, which were spread over the broad spectroscopic region, from the near-UV up to the near-IR regions. Each emission band had a specific lifetime, which ranged from the sub-ps to the ms scale. 相似文献
184.
We investigate how entanglement can be transferred between qubits and continuous-variable (CV) systems. We find that one ebit borne in maximally entangled qubits can be fully transferred to two CV systems which are initially prepared in a pure separable Gaussian field with high excitation. We show that it is possible to retrieve the entanglement back to qubits from the entangled CV systems. The deposition of multiple ebits from qubits to the initially separable CV systems is also pointed out. We show that the entanglement transfer and retrieval are done at a quasisteady state. 相似文献
185.
Girotti R Marrocchi A Minuti L Piermatti O Pizzo F Vaccaro L 《The Journal of organic chemistry》2006,71(1):70-74
[reaction: see text] Diels-Alder reactions of 3-substituted coumarins 1a-g with methyl-1,3-butadienes 2a-c carried out in water alone and in CH2Cl2 under 9 kbar pressure are reported. In aqueous medium satisfactory results were obtained by operating at 150 degrees C, whereas under high pressure the cycloadditions were complete at 60-70 degrees C with excellent yields (85-95%). The reactions with isoprene (2b) always resulted in the exclusive formation of para cycloadducts, whereas with (E)-piperylene (2c) only ortho products were detected. The cycloaddition of 3-phenylsulfonylcoumarin (1a) with (E)-piperylene (2c) allowed the endo adduct to be obtained exclusively, whereas 3-carboxycoumarin (1b) reacted with 2c to give a mixture of the corresponding endo/exo adducts in a 58:42 ratio in water and in a 45:55 ratio under high-pressure condition. 相似文献
186.
Francesco Ciccarello G. Massimo Palma Mauro Paternostro Michelangelo Zarcone Yasser Omar 《Solid State Sciences》2009,11(5):931-934
We present a scheme for generating entanglement between two magnetic impurities in a solid-state system via electron scattering. The scheme applies to impurities of arbitrary quantum spin number. We show that resonance conditions yield generation of a maximally entangled state of the impurities' spins, regardless of the value of the electron–impurity coupling constant and the impurity spin quantum number. The mechanism behind the scheme is explained in terms of resonance-induced selection rules. 相似文献
187.
Curcumin, a well-known Indian spice, holds a variety of properties in many different fields from medicinal chemistry to dye industry. The peculiar electronic structure makes curcumin a valuable metal chelator. The principal aim of this work is a computational study of the structural and electronic properties of the ground and the first singlet excited states of the curcuminoidic core. Concerning the ground state, tautomeric equilibrium, vibrational and thermochemical analysis and electronic absorption spectra (with ab initio and semi-empirical methodologies) have been studied. A full geometry optimization of the first singlet excited states was obtained, with different computational methodologies. Solvent effects are also implicitly considered. An accurate comparison of the results is presented. Interesting aspects emerge, which suggest successive investigation about the nature of the excited states. The obtained results may be of large applicative interest. If curcuminoids are considered as potential ligands for complexes formation with metallic ions of pharmaceutical, medical–physical and technological interest, exciting the system with photons of appropriate frequencies, a photomodulated release of the metallic ion in the environment might be guessed, because of an important photoinduced geometrical modification. 相似文献
188.
Rosa Sparaco Antonia Scognamiglio Angela Corvino Giuseppe Caliendo Ferdinando Fiorino Elisa Magli Elisa Perissutti Vincenzo Santagada Beatrice Severino Paolo Luciano Marcello Casertano Anna Aiello Gilberto De Nucci Francesco Frecentese 《Molecules (Basel, Switzerland)》2023,28(1)
We recently identified 6-nitrodopamine and other nitro-catecholamines (6-nitrodopa, 6-nitroadrenaline), indicating that the endothelium has the ability to nitrate the classical catecholamines (dopamine, noradrenaline, and adrenaline). In order to investigate whether drugs could be subject to the same nitration process, we synthesized 4-nitro- and 7-nitropropranolol as probes to evaluate the possible nitration of the propranolol by the endothelium. The separation of the enantiomers in very high yields and excellent enantiopurity was achieved by chiral HPLC. Finally, we used Riguera’s method to determine the absolute configuration of the enantiomers, through double derivatization with MPA and NMR studies. 相似文献
189.
190.
Cluster techniques are used in hotspot spatial analysis to detect hotspots as areas on the map; an extension of the Fuzzy C-means that the clustering algorithm has been applied to locate hotspots on the map as circular areas; it represents a good trade-off between the accuracy in the detection of the hotspot shape and the computational complexity. However, this method does not measure the reliability of the detected hotspots and therefore does not allow us to evaluate how reliable the identification of a hotspot of a circular area corresponding to the detected cluster is; a measure of the reliability of hotspots is crucial for the decision maker to assess the need for action on the area circumscribed by the hotspots. We propose a method based on the use of De Luca and Termini’s Fuzzy Entropy that uses this extension of the Fuzzy C-means algorithm and measures the reliability of detected hotspots. We test our method in a disease analysis problem in which hotspots corresponding to areas where most oto-laryngo-pharyngeal patients reside, within a geographical area constituted by the province of Naples, Italy, are detected as circular areas. The results show a dependency between the reliability and fluctuation of the values of the degrees of belonging to the hotspots. 相似文献