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71.
Zacarias León Jon de Vlieger Alberto Chisvert Amparo Salvador Henk Lingeman Hubertus Irth Martin Giera 《Chromatographia》2010,71(1-2):55-63
Nowadays, 2-ethylhexyl 4-(N,N-dimethylamino)benzoate (EDP) is one of the most widely used UV filters in sunscreen cosmetics and other cosmetic products. However, undesirable processes such as percutaneous absorption and biological activity have been attributed to this compound. The in vitro metabolism of EDP was elucidated in the present work. First of all, the phase I biotransformation was studied in rat liver microsomes and two metabolites, N,N-dimethyl-p-aminobenzoic acid (DMP) and N-monomethyl-p-aminobenzoic acid (MMP), were identified by GC-MS analysis. Secondly, the phase II metabolism was investigated by means of LC-MS. The investigated reactions were acetylation and glucuronidation working with rat liver cytosol and with both human and rat liver microsomes, respectively. Analogue studies with p-aminobenzoic acid (PABA) were carried out in order to compare the well established metabolic pathway of PABA with the unknown biotransformation of EDP. In addition, a method for the determination of EDP and its two phase I metabolites in human urine was developed. The methodology requires a solid-phase extraction prior to LC-MS analysis. The method is based on standard addition quantification and has been fully validated. The repeatability of the method, expressed as relative standard deviation, was in the range 3.4–7.4% and the limit of detection for all quantified analytes was in the low ng mL?1 range. 相似文献
72.
Falck D de Vlieger JS Giera M Honing M Irth H Niessen WM Kool J 《Analytical and bioanalytical chemistry》2012,403(2):367-375
In this study, an integrated approach is developed for the formation, identification and biological characterization of electrochemical
conversion products of p38α mitogen-activated protein kinase inhibitors. This work demonstrates the hyphenation of an electrochemical
reaction cell with a continuous-flow bioaffinity assay and parallel LC-HR-MS. Competition of the formed products with a tracer
(SKF-86002) that shows fluorescence enhancement in the orthosteric binding site of the p38α kinase is the readout for bioaffinity.
Parallel HR-MSn experiments provided information on the identity of binders and non-binders. Finally, the data produced with this on-line
system were compared to electrochemical conversion products generated off-line. The electrochemical conversion of 1-{6-chloro-5-[(2R,5S)-4-(4-fluorobenzyl)-2,5-dimethylpiperazine-1-carbonyl]-3aH-indol-3-yl}-2-morpholinoethane-1,2-dione resulted in eight products,
three of which showed bioaffinity in the continuous-flow p38α bioaffinity assay used. Electrochemical conversion of BIRB796
resulted, amongst others, in the formation of the reactive quinoneimine structure and its corresponding hydroquinone. Both
products were detected in the p38α bioaffinity assay, which indicates binding to the p38α kinase. 相似文献
73.
Harald Günzel Hubertus Th. Jongen Oliver Stein 《Central European Journal of Operations Research》2007,15(3):271-280
In generalized semi-infinite programming the feasible set is known to be not closed in general. In this paper, under natural
and generic assumptions, the closure of the feasible set is described in explicit terms.
Oliver Stein gratefully acknowledges support through a Heisenberg grant of the Deutsche Forschungsgemeinschaft. 相似文献
74.
Jan Kuliga Stephen Massicot Rajan Adhikari Michael Ruppel Prof. Dr. Norbert Jux Prof. Dr. Hans-Peter Steinrück Dr. Hubertus Marbach 《Chemphyschem》2020,21(5):423-427
The adsorption behavior and the mobility of 2H-Tetranaphthylporphyrin (2HTNP) on Cu(111) was investigated by scanning tunneling microscopy (STM) at room temperature (RT). The molecules adsorb, like the structurally related 2HTPP, in the “inverted” structure with the naphthyl plane restricted to an orientation parallel to the Cu surface. The orientation of the four naphthyl groups yields altogether 16 possible conformations. Due to the existence of rotamer pairs, 10 different appearances are expected on the surface, and all of them are identified by STM at RT. Most interestingly, the orientation of the naphthyl groups significantly influences the diffusion behavior of the molecules on Cu(111). We identify three different groups of conformers, which are either immobile, medium or fast diffusing at RT. The mobility seems to decrease with increasing size of the footprint of the conformers on the surface. 相似文献
75.
76.
We study two approaches to replace a finite mathematical programming problem with inequality constraints by a problem that contains only equality constraints. The first approach lifts the feasible set into a high-dimensional space by the introduction of quadratic slack variables. We show that then not only the number of critical points but also the topological complexity of the feasible set grow exponentially. On the other hand, the second approach bases on an interior point technique and lifts an approximation of the feasible set into a space with only one additional dimension. Here only Karush–Kuhn–Tucker points with respect to the positive and negative objective function in the original problem give rise to critical points of the smoothed problem, so that the number of critical points as well as the topological complexity can at most double. 相似文献
77.
In the screening of complex mixtures, for example combinatorial libraries, natural extracts, and metabolic incubations, different
approaches are used for integrated bioaffinity screening. Four major strategies can be used for screening of bioactive mixtures
for protein targets—pre-column and post-column off-line, at-line, and on-line strategies. The focus of this review is on recent
developments in post-column on-line screening, and the role of mass spectrometry (MS) in these systems. On-line screening
systems integrate separation sciences, mass spectrometry, and biochemical methodology, enabling screening for active compounds
in complex mixtures. There are three main variants of on-line MS based bioassays: the mass spectrometer is used for ligand
identification only; the mass spectrometer is used for both ligand identification and bioassay readout; or MS detection is
conducted in parallel with at-line microfractionation with off-line bioaffinity analysis. On the basis of the different fields
of application of on-line screening, the principles are explained and their usefulness in the different fields of drug research
is critically evaluated. Furthermore, off-line screening is discussed briefly with the on-line and at-line approaches. 相似文献
78.
Roland Hord Gerhard Cordier Kathrin Hofmann Alexander Buckow Gwendolyne Pascua Hubertus Luetkens Prof. Dr. Lambert Alff Prof. Dr. Barbara Albert 《无机化学与普通化学杂志》2011,637(9):1114-1117
Through low‐temperature synthesis in CsOH flux, lanthanum cuprate La2CuO4 can be obtained in a metastable form, the so‐called T′ modification (tetragonal, I4/mmm, no. 139, a = 400.95(2) pm, c = 1254.08(7) pm). When heated, this T′ phase transforms into a K2NiF4‐type modification, whose crystal structure was now refined from X‐ray powder data (tetragonal, I4/mmm, no. 139, a = 383.29(3) pm, c = 1331.3(2) pm at T = 1073 K). The well‐known orthorhombic phase (s.g. Cmce, no. 64, a = 536.14(3) pm, b = 1315.53(8) pm, c = 540.20(3) pm) – usually obtained via conventional solid state synthesis – was observed to form upon cooling from the K2NiF4‐type modification. High‐temperature powder diffractometry allowed crystal structure refinements for all of the three phases. 相似文献
79.
Jan W. Post Hubertus V.M. Hamelers Cees J.N. Buisman 《Journal of membrane science》2009,330(1-2):65-72
Reverse electrodialysis is a membrane-based technique for production of sustainable electricity from controlled mixing of a diluted electrolyte solution (e.g., river water) and a concentrated electrolyte solution (e.g., sea water). Reverse electrodialysis has been investigated with pure sodium chloride solutions. In practice, however, in most cases also other ions are present in both feed solutions. In the present paper, the effect of multivalent ions on the performance of a reverse electrodialysis stack was investigated. Results show that, besides a higher stack resistance in presence of multivalent ions, especially the presence of multivalent ions in the dilute solution has a lowering effect on the stack voltage. This can be explained by an observed transport of these ions from the diluted electrolyte solution to the concentrated electrolyte solution. In order to prevent or hamper this transport against the activity gradient, monovalent-selective membranes can be used. This shows indeed better results with respect to the stack voltage. Therefore, it would be beneficial to use monovalent-selective membranes in reverse electrodialysis, especially in the case of a relatively high content of multivalent ions in the dilute (i.e., in the first stages of the installation where the sodium chloride content in the dilute is still relatively low). 相似文献
80.