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11.
Three standardised, capillary zone electrophoresis-electrospray ionisation mass spectrometry (CZE-ESI-MS) methods were developed for the analysis of six drug candidates and their respective process-related impurities comprising a total of 22 analytes with a range of functional groups and lipophilicities. The selected background electrolyte conditions were found to be: 60/40 v/v 10 mM ammonium formate pH 3.5/organic, 60/40 v/v 10 mM ammonium acetate pH 7.0/organic and 10 mM piperidine, pH 10.5, where the organic solvent is 50/50 v/v methanol/acetonitrile. The coaxial sheath flow consisted of either 0.1% v/v formic acid in 50/50 v/v methanol/water, or 10 mM ammonium acetate in 50/50 v/v methanol/water, depending on the mixture being analysed. Factor analysis and informational theory were used to quantify the orthogonality of the methods and predict their complementarities. The three selected CZE-ESI-MS methods allowed the identification of 21 out of 22 of all the drug candidates and their process-related impurities and provided orthogonality with four established high-performance liquid chromatography-mass spectrometry (HPLC-MS) methods. These methodologies therefore form the basis of a generic approach to impurity profiling of pharmaceutical drug candidates and can be applied with little or no analytical method development, thereby offering significant resource and time savings. 相似文献
12.
[reaction: see text] SIBX is a nonexplosive formulation of IBX that can be used as a suspension in a variety of standard organic solvents such as refluxing EtOAc and THF to oxidize safely alcohols into aldehydes and ketones. The use of hot THF is limited to the oxidation of allylic and benzylic alcohols. Most yields are comparable to those obtained with IBX or DMP. SIBX can also be used to perform oxygenative demethylation of 2-methoxyarenols into orthoquinones and catechols. 相似文献
13.
Karl Pays Caroline Mabille Véronique Schmitt Fernando Leal-Calderon J´erôme Bibette 《Journal of Dispersion Science and Technology》2013,34(1-3):175-186
This paper aims to review the various degradation pathays of emulsions. Aging of emulsions may proceed through three distinct microscopic mechanisms: diffusion or permeation, dewetting, and coalescence, each one being associated with a very characteristic growth scenario. We show within this context how double emulsions are a unique tool to complete the basic understanding of emulsion metastability. 相似文献
14.
N. S. Emel´yanova N. Yu. Shmatko N. A. Sanina S. M. Aldoshin 《Russian Chemical Bulletin》2017,66(10):1842-1846
Possible reactions of the mononuclear iron nitrosyl complex [Fe(SC(NH2)2)2(NO)2]Сl?H2O in an aqueous solution were studied using quantum chemical modeling. The electronic structures of the possible intermediates were examined by the NBO and AIM methods. The substitution of the thio ligand in the iron—sulfur nitrosyl complex by a water molecule and the formation of dimeric intermediate complexes were found to facilitate the NO-donation process. 相似文献
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Prozorova G. F. Korzhova S. A. Pozdnyakov A. S. Emel´yanov A. I. Ermakova T. G. Dubrovina V. I. 《Russian Chemical Bulletin》2015,64(6):1437-1439
Russian Chemical Bulletin - The water-soluble nanocomposite with the uniform distribution of silver nanoparticles in polymer matrix was synthesized on the basis of poly-1-vinyl-1,2,4-triazole.... 相似文献
17.
Ukhin L. Yu. Kuz´mina L. G. Alexeenko D. V. Belousova L. V. Morkovnik A. S. Shepelenko E. N. Podshibyakin V. A. Borodkin G. S. Dmitrieva O. I. 《Russian Chemical Bulletin》2019,68(12):2290-2297
Russian Chemical Bulletin - New potentially bioactive derivatives comprising spatially hindered pyrocatechol linked to hydrazine, acid hydrazides (including isoniazid), and acetylcysteine by a... 相似文献
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The effective diffusion coefficient that gives a steady-state xenon concentration of 0.2-0.3wt% in the recrystallised grains of high burn-up UO 2 fuel is calculated to lie in the range 10 m 24 to 10 m 22 m 2 s m 1 . These values are one to three orders of magnitude lower than the value currently accepted for the radiation-enhanced diffusion coefficient. The time required to reach the steady-state concentration depends on the local fission rate, the grain size distribution and the precise magnitude of the radiation-enhanced diffusion coefficient, and can take from 2 to 10 years. Additional calculations reveal that substantially less than 10% of the fission gas inventory is released from the original UO 2 grains in the outer region of the fuel prior to recrystallisation. In contrast, with a diffusion coefficient of 10 m 22 m 2 s m 1 more than 80% of the fission gas is released from the recrystallised grains of the high burn-up structure in one year. 相似文献
20.
We propose an approach to the data-driven newsvendor problem that incorporates a correction factor to account for rare events, when the decision-maker has few historical data points at his disposal but knows the range of the demand. This mitigates a weakness of pure data-driven methodologies, specifically, the fact that they under-protect the system against tail events, which are in general under-observed in the empirical demand distribution. We test the approach in extensive computational experiments and provide a summary table of the numerical experiments to help the decision maker gain further insights. 相似文献