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Surowiec I Baena JR Frank J Laurell T Nilsson J Trojanowicz M Lendl B 《Journal of chromatography. A》2005,1080(2):132-139
A flow-through microdispenser has been coupled to a micro HPLC separation system and used as a solvent elimination interface for Fourier transform infrared (FTIR) and Raman spectroscopic detection of the separated compounds. Using the microdispenser picoliter sized droplets can be generated and deposited on an appropriate target placed on a computerized x, y-stage. Evaporation of volatile solvent and buffer is rapid and allows analysis of the obtained dry deposits by various techniques. Due to the destruction free character of Raman and FTIR spectroscopy they can be applied sequentially to interrogate the same deposit. In the reported application five phenolic acids typically present in wine have been separated on a C-18 column technique using a mixture of water, methanol and acetic acid as mobile phase. For spectrum acquisition infrared and Raman microscopes have been used. The spectra recorded from the dried deposits of the separated compounds agreed well with the reference spectra of corresponding components. 相似文献
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Reactions of 23R- and 23S-23-spirostanols in the 25R and 25S series with lead tetraacetate-iodine were studied. The reactions carried out at low temperature afforded d-seco-iododialdehydes and C22 lactones, while similar reactions performed in refluxing tetrachloromethane yielded 20-chlorolactones and their 21-acetoxy derivatives irrespective of the hydroxyl group configuration at C-23. The reaction mechanisms are discussed. 相似文献
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Grayna Wjcik Izabella Mossakowska 《Acta Crystallographica. Section C, Structural Chemistry》2007,63(2):o123-o125
The crystal structure of 1‐chloro‐2‐nitrobenzene, C6H4ClNO2, is made up of molecules which are linked by N—O⋯Cl halogen bonds. These molecular chains are involved in aromatic π–π stacking; the intermolecular O⋯Cl distance is 3.09 Å. Such short halogen bonds are not common. A rigid‐body analysis including the non‐rigidly attached rigid group provides the mean‐square amplitudes of the molecular translations and librations, and of the internal torsional vibrations of the nitro group. The results reveal the driving role of the torsional vibrations of the nitro group in the phase transition to the liquid phase. 相似文献
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Elionai Cassiana de Lima Gomes Izabella Ercole de Carvalho Silvia Ligório Fialho Jamile Barbosa Maria Irene Yoshida Armando da Silva Cunha Júnior 《Journal of Thermal Analysis and Calorimetry》2018,131(3):2123-2128
Most of the pharmaceutical products are formulated as solid dosage form, which may present drug–excipient interactions that lead to changes in the chemical nature of the drug, such as solubility and bioavailability and may compromise its safety and effectiveness. Differential scanning calorimetry (DSC) is a widely used method for the rapid evaluation of the drug-excipient compatibility and the stability of the mixture formed; however, there is no consensus on the preparation methods of the drug–excipient mixtures. The aim of this study was to investigate the influence of the mixing method on the drug–excipient compatibility studies by means of DSC analysis, using tenofovir disoproxil fumarate as a drug model. Statistical analysis revealed significant differences in the heat of fusion of the drug in the mixtures prepared by several mixing methods. Vortex Mixer with a Pop-Off Cup used for 3 min proved to be very satisfactory for these studies. A polymorphic transition was observed in the mixture prepared with the mortar and pestle. Therefore, this method should be avoided since it may induce errors in the interpretation of DSC results. In this way, the mixing method used to prepare a mixture for studies of interactions between the API and the excipients in a pharmaceutical formulation has a great influence on the results and it must be chosen carefully. 相似文献
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Zsolt PAP Andreea RADU Izabella Jolan HIDI Georgian MELINTE Lucian DIAMANDESCU Traian POPESCU Lucian BAIA Virginia DANCIU Monica BAIA 《催化学报》2013,34(4):734-740
TiO2 -Au aerogels containing different amounts of gold nanoparticles of different sizes (5 and 16 nm) were successfully synthesized using a sol-gel procedure, and were tested for salicylic acid photodegradation under UV irradiation. The structure and morphology of the obtained materials were investigated using X-ray diffraction, transmission electron microscopy, and N2 adsorption-desorption measurements. UV-Vis spectroscopy was used to study the optical properties. The effects of the gold nanoparticles on the TiO2 crystallization process were twofold, as follows: (i) the number of crystallized zones was strongly related to the concentration of the gold nanoparticles, and (ii) the smaller gold particles increased the time taken for the crystallization of the samples. It was found that the noble metal-doped samples exhibited higher degradation rates compared with bare titania. It was found that the most active photocatalyst in each studied system was the sample with the highest concentration of gold nanoparticles. Additionally, the highest degradation rate value was obtained with the smallest Au nanoparticles (46.4 10-3 μmol/(L·s). 相似文献
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We investigate Fuglede's spectral set conjecture in the special case when the set in question is a union of finitely many unit intervals in dimension 1. In this case, the conjecture can be reformulated as a statement about multiplicative properties of roots of associated with the set polynomials with (0,1) coefficients. Let be an N-term polynomial. We say that {θ1,θ2,…,θN−1} is an N-spectrum for A(x) if the θj are all distinct and
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Roles of steroid hormones, and compounds that can influence their levels in cells, are of increasing interest in e.g. cancer research, partly because resistance to hormone therapies often complicates treatment. To elucidate the processes involved, the hormones and related compounds need to be accurately measured. Reversed-phase liquid chromatography with dynamic multiple reaction monitoring mass spectrometric detection in electrospray mode is capable of providing such measurements. Therefore, LC-MS/MS was developed for sensitive, selective analysis of 11 steroid hormones, cholesterol and two prostaglandins. The effects of the tissue matrix, and solid-phase extraction (SPE) sample clean-up, on the LC-MS/MS signals of the hormones were also investigated. The results show that the developed LC-MS/MS method, following SPE clean-up to reduce matrix interference, can detect selected steroids in extracts of mouse tissues. The method provides linear measurements of the steroids at concentrations up to few ng/μL, and limits of detection in the range 0.03-0.2 pg/μL (for some compounds lower than those of previously reported methods). 相似文献