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991.
Partial least squares model and design of experiments toward the analysis of the metabolome of Jatropha gossypifolia leaves: Extraction and chromatographic fingerprint optimization 下载免费PDF全文
Fausto Carnevale Neto Rafael Teixeira Freire Patrícia Cardoso Renato Lajarim Carneiro Vanderlan Da Silva Bolzani Ian Castro‐Gamboa 《Journal of separation science》2016,39(6):1023-1030
A major challenge in metabolomic studies is how to extract and analyze an entire metabolome. So far, no single method was able to clearly complete this task in an efficient and reproducible way. In this work we proposed a sequential strategy for the extraction and chromatographic separation of metabolites from leaves Jatropha gossypifolia using a design of experiments and partial least square model. The effect of 14 different solvents on extraction process was evaluated and an optimized separation condition on liquid chromatography was estimated considering mobile phase composition and analysis time. The initial conditions of extraction using methanol and separation in 30 min between 5 and 100% water/methanol (1:1 v/v) with 0.1% of acetic acid, 20 μL sample volume, 3.0 mL min?1 flow rate and 25°C column temperature led to 107 chromatographic peaks. After the optimization strategy using i‐propanol/chloroform (1:1 v/v) for extraction, linear gradient elution of 60 min between 5 and 100% water/(acetonitrile/methanol 68:32 v/v with 0.1% of acetic acid), 30 μL sample volume, 2.0 mL min?1 flow rate, and 30°C column temperature, we detected 140 chromatographic peaks, 30.84% more peaks compared to initial method. This is a reliable strategy using a limited number of experiments for metabolomics protocols. 相似文献
992.
Advanced solvent signal suppression for the acquisition of 1D and 2D NMR spectra of Scotch Whisky 下载免费PDF全文
Will Kew Nicholle G.A. Bell Ian Goodall Dušan Uhrín 《Magnetic resonance in chemistry : MRC》2017,55(9):785-796
A simple and robust solvent suppression technique that enables acquisition of high‐quality 1D 1H nuclear magnetic resonance (NMR) spectra of alcoholic beverages on cryoprobe instruments was developed and applied to acquire NMR spectra of Scotch Whisky. The method uses 3 channels to suppress signals of water and ethanol, including those of 13C satellites of ethanol. It is executed in automation allowing high throughput investigations of alcoholic beverages. On the basis of the well‐established 1D nuclear Overhauser spectroscopy (NOESY) solvent suppression technique, this method suppresses the solvent at the beginning of the pulse sequence, producing pure phase signals minimally affected by the relaxation. The developed solvent suppression procedure was integrated into several homocorrelated and heterocorrelated 2D NMR experiments, including 2D correlation spectroscopy (COSY), 2D total correlation spectroscopy (TOCSY), 2D band‐selective TOCSY, 2D J‐resolved spectroscopy, 2D 1H, 13C heteronuclear single‐quantum correlation spectroscopy (HSQC), 2D 1H, 13C HSQC‐TOCSY, and 2D 1H, 13C heteronuclear multiple‐bond correlation spectroscopy (HMBC). A 1D chemical‐shift‐selective TOCSY experiments was also modified. The wealth of information obtained by these experiments will assist in NMR structure elucidation of Scotch Whisky congeners and generally the composition of alcoholic beverages at the molecular level. 相似文献
993.
Lenka Kulhánková Jonáš Tokarský Petra Vilímová Pavlína Peikertová Oldřich Motyka 《Chemical Papers》2017,71(2):317-327
Preparation method of polyaniline/montmorillonite (PANI/MMT) nanocomposite in the form of thin layer deposited on various substrates is optimized in this work to obtain high electrical conductivity. Simple method (i.e. polymerization of anilinium sulfate in the presence of MMT) has been used for the preparation and following four conditions were varied: preparation temperature (T = 10 or 20 °C), preparation time (t = 4 or 6 h), size fraction of MMT (p < 1 or 5 µm), and type of substrate (microscope glass slides, silica glass slides, polyester foils). Therefore, 24 samples were prepared, characterized and their electrical conductivity was compared. Raman spectroscopy and scanning electron microscopy were used for the characterization of the structure of samples. Thickness of layers was measured using atomic force microscopy. Based on the comparison of samples and with respect to the aim of obtaining high electrical conductivity, it was found that the most suitable substrate is polyester foil and preparation conditions are T = 20 °C, t = 6 h, p < 5 µm. To obtain highly conductive layers on glass substrates (although less conductive than layers on foil), preparation time have to be shortened to 4 h. 相似文献
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Surface analysis of ripple pattern on PS and PEN induced with ring‐shaped mask due to KrF laser treatment 下载免费PDF全文
O. Neděla P. Slepička P. Sajdl M. Veselý V. Švorčík 《Surface and interface analysis : SIA》2017,49(1):25-33
The approach for ripple nanopattern construction on surface of two polymer substrates [polyethylene naphthalate (PEN) and polystyrene (PS)] exposed by a KrF pulse excimer UV laser through a contact lithographic mask with circular slit was proposed in this paper. Thin layer of gold was deposited on samples after the laser treatment. Changes in the morphology of the surface of both the shielded and exposed areas of the substrates, as well as the dimensions of the laser‐induced periodic surface structures, were determined (by atomic force microscopy, laser confocal microscopy and scanning electron microscopy), compared with observations and measurements made on samples treated directly (without a contact mask) under the same conditions. The morphology of the interface between the treated and untreated regions was also closely studied. Surface chemistry of treated samples was studied in detail by X‐ray Photoelectron Spectroscopy. The detailed study of surface chemistry of modified PEN and PS revealed a significant increase of oxygen concentration for laser treated PS and increase of carboxyl groups in case of PEN. The potential application of this research can be found in biotechnology, micro technology and several other fields. Copyright © 2016 John Wiley & Sons, Ltd. 相似文献
996.
Santiago V. Luis Juan C. Frías Rosa V. Salvador Michael Bolte 《Journal of chemical crystallography》1999,29(4):403-408
The crystal structures of 1,4,7,10,13,16-hexaoxa-cyclooctadecane dicyano mercury(II) monohydrate, C14H24HgN2O6·H2O, 1, and 2,5,8,11,18,21,24,27-octaoxa-tricyclo[26.4.0.012,17]-dotriconta-1(28),12,14,16,29,31-hexaene dicyano mercury(II) monohydrate, C26H32HgN2O8·H2O, 2, were determined: 1 crystallizes in the trigonal space group R3¯ with cell dimensions a = 11.7842(1) and c = 12.0316(1) Å. 2 crystallizes in the monoclinic space group P21/c with cell dimensions a = 11.156(3) Å, b = 8.417(2), c = 30.901(8) Å, and = 93.279°. In spite of the different cyclic systems, similar complexes are formed where the Hg atom is coordinated by two CN groups and six oxygen atoms of the crown ether. The structure of 1 is isostructural with the crystal structures of 18C6—HgCl2, 18C6—CdBr2, 18C6—Sr(BH4)2, and 18C6—Ba(BH4)2. Furthermore, 1 is very similar to other 18C6—HgX2 complexes. 相似文献
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Residual‐based stabilization of the finite element approximation to the acoustic perturbation equations for low Mach number aeroacoustics 下载免费PDF全文
Oriol Guasch Patricia Sánchez‐Martín Arnau Pont Joan Baiges Ramon Codina 《国际流体数值方法杂志》2016,82(12):839-857
The acoustic perturbation equations (APE) are suitable to predict aerodynamic noise in the presence of a non‐uniform mean flow. As for any hybrid computational aeroacoustics approach, a first computational fluid dynamics simulation is carried out from which the mean flow characteristics and acoustic sources are obtained. In a second step, the APE are solved to get the acoustic pressure and particle velocity fields. However, resorting to the finite element method (FEM) for that purpose is not straightforward. Whereas mixed finite elements satisfying an appropriate inf–sup compatibility condition can be built in the case of no mean flow, that is, for the standard wave equation in mixed form, these are difficult to implement and their good performance is yet to be checked for more complex wave operators. As a consequence, strong simplifying assumptions are usually considered when solving the APE with FEM. It is possible to avoid them by resorting to stabilized formulations. In this work, a residual‐based stabilized FEM is presented for the APE at low Mach numbers, which allows one to deal with the APE convective and reaction terms in its full extent. The key of the approach resides in the design of the matrix of stabilization parameters. The performance of the formulation and the contributions of the different terms in the equations are tested for an acoustic pulse propagating in sheared‐solenoidal mean flow, and for the aeolian tone generated by flow past a two‐dimensional cylinder. Copyright © 2016 John Wiley & Sons, Ltd. 相似文献