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81.
Christopher S. Lancefield O. Stephen Ojo Fanny Tran Nicholas J. Westwood 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2015,127(1):260-264
Functionalized phenolic monomers have been generated and isolated from an organosolv lignin through a two‐step depolymerization process. Chemoselective catalytic oxidation of β‐O‐4 linkages promoted by the DDQ/tBuONO/O2 system was achieved in model compounds, including polymeric models and in real lignin. The oxidized β‐O‐4 linkages were then cleaved on reaction with zinc. Compared to many existing methods, this protocol, which can be achieved in one pot, is highly selective, giving rise to a simple mixture of products that can be readily purified to give pure compounds. The functionality present in these products makes them potentially valuable building blocks. 相似文献
82.
N. Stoppacher R. D. Josephs A. Daireaux T. Choteau S. W. Westwood R. I. Wielgosz 《Analytical and bioanalytical chemistry》2013,405(25):8039-8051
It is common practice to quantify the mass concentration of a peptide solution through quantitative determination of selected chemically stable amino acids produced following complete hydrolysis of the parent peptide. This is because there is generally an insufficient quantity of material available to allow for the obvious alternative of a direct purity analysis characterization of the parent peptide, and the subsequent constitution of a calibration solution. However, selected accurately characterized pure peptide reference materials are required to establish reference points for the dissemination of metrologically traceable measurements and to develop reference measurement systems for laboratory medicine. In principle, purity assignment of a peptide can be performed by using the so-called mass balance approach, by employing a range of analytical techniques to obtain an estimate of the mass fraction content of all impurities present in the intact peptide, and by utilizing the difference from the theoretical limit value to assign the mass fraction content of the main peptide. Liquid chromatography–high-resolution tandem mass spectrometry (LC-hrMS/MS) is a key technique for the detection, identification, and determination of structurally related impurities present in a peptide material, and experiments characterizing the model peptide hormone angiotensin I (ANG I) are described in the present work. Degradation products that were generated from ANG I after storage at elevated temperatures were screened. The formation of peptide fragments such as ANG II or ANG III was determined by comparison of measured mass values with calculated mass values. The use of a data-dependent acquisition technique enabled the detection and structural characterization of ANG II and other peptide fragments as major impurities in the same LC-hrMS/MS analysis run. Subsequent quantification using external calibration allowed the mass fraction of the major impurities in a candidate reference material to be estimated as 10.4 mg/g. Failure to correct for these impurities would lead to a 1 % error in the determination of the concentration of the peptide in solution by amino acid analysis techniques. Figure
Angiotensin I (ANG I): hrMS/MS spectrum, chemical formula, and amino acid sequence 相似文献
83.
Suzanne OConnor Yann-Vaï Le Bihan Isaac M. Westwood Manjuan Liu Oi Wei Mak Gabriel Zazeri Ana P. R. Povinelli Alan M. Jones Rob van Montfort Jhannes Reynisson Ian Collins 《Molecules (Basel, Switzerland)》2022,27(3)
Heat Shock Protein 70s (HSP70s) are key molecular chaperones that are overexpressed in many cancers and often associated with metastasis and poor prognosis. It has proven difficult to develop ATP-competitive, drug-like small molecule inhibitors of HSP70s due to the flexible and hydrophilic nature of the HSP70 ATP-binding site and its high affinity for endogenous nucleotides. The aim of this study was to explore the potential for the inhibition of HSP70 through alternative binding sites using fragment-based approaches. A surface plasmon resonance (SPR) fragment screen designed to detect secondary binding sites in HSP70 led to the identification by X-ray crystallography of a cryptic binding site in the nucleotide-binding domain (NBD) of HSP70 adjacent to the ATP-binding site. Fragment binding was confirmed and characterized as ATP-competitive using SPR and ligand-observed NMR methods. Molecular dynamics simulations were applied to understand the interactions with the protein upon ligand binding, and local secondary structure changes consistent with interconversion between the observed crystal structures with and without the cryptic pocket were detected. A virtual high-throughput screen (vHTS) against the cryptic pocket was conducted, and five compounds with diverse chemical scaffolds were confirmed to bind to HSP70 with micromolar affinity by SPR. These results identified and characterized a new targetable site on HSP70. While targeting HSP70 remains challenging, the new site may provide opportunities to develop allosteric ATP-competitive inhibitors with differentiated physicochemical properties from current series. 相似文献
84.
Tingye Li AT&T Middletown NJ USA Zisen Zhao Wuhan Research Institute of Post Telecommunications Fiberhome Wuhan ChinaJianjun Yu ZTE USA Inc. wood ave. south FL Iselin NJ USA ZTE Inc. Beijing China 《中国光学快报(英文版)》2010,(9):815-815
<正>Fiber optics underpins the communications infrastructure for the information society today. Cables consisting of hair-like fibers speed data around the globe in the form of rapid pulses of light. Modern telecom 相似文献
85.
Evans KM Haraldsen JD Pearson RJ Slawin AM Ward GE Westwood NJ 《Organic & biomolecular chemistry》2007,5(13):2063-2069
The use of phenotype-based screens as an approach for identifying novel small molecule tools is reliant on successful protein target identification strategies. Here we report on the synthesis and chemical characterisation of a novel reagent for protein target identification based on a small molecule inhibitor of human cell invasion by the parasite Toxoplasma gondii. A detailed (1)H NMR study and biological testing confirmed that incorporation of an amino-containing functional group into the aryl ring of this inhibitor was possible without loss of biological activity. Interesting chemical reactivity differences were identified resulting from incorporation of the new substituent. The amine functionality was then used to prepare a biotinylated reagent that is central to our current protein target identification studies with this inhibitor. 相似文献
86.
NJ Oldham 《Rapid communications in mass spectrometry : RCM》1999,13(16):1694-1698
Ion/molecule reactions leading to formation of the diagnostically useful [C(3)H(4)N](+) ion (m/z 54), from acetonitrile CI plasma, have been studied using a tandem quadrupole mass spectrometer. Evidence is presented to demonstrate that [C(3)H(4)N](+) is produced from an ion/molecule reaction between [C(2)H(2)N](+) (m/z 40) and neutral acetonitrile, via a [C(4)H(5)N(2)](+) (m/z 81) intermediate. Loss of HCN, where the H atom arises from neutral acetonitrile and the CN group from [C(2)H(2)N](+) (m/z 40), leads to the production of [C(3)H(4)N](+) (m/z 54). These results are consistent with a proposed concerted elimination of HCN, generating m/z 54 as a methylene vinylidene ammonium ion. Copyright 1999 John Wiley & Sons, Ltd. 相似文献
87.
Mantica P Gorini G Hogeweij GM Lopes Cardozo NJ Schilham AM 《Physical review letters》2000,85(21):4534-4537
Layers of reduced electron heat transport ("transport barriers") have been observed in the Rijnhuizen Tokamak Project when the plasma is dominantly heated by electron cyclotron heating (ECH). Experiments into the properties of the transport barriers are reported. Modulation of the ECH power was used to probe electron heat transport in the barriers by means of propagating electron temperature perturbations. The observed propagation shows that transport inside the barriers is dominated by heat convection. This convection is inward, i.e., up the temperature gradient. 相似文献
88.
89.
A method for extracting the normal modes of acoustic propagation in the shallow ocean from sound recorded on a vertical line array (VLA) of hydrophones as a source travels nearby is presented. The mode extraction is accomplished by performing a singular value decomposition (SVD) of individual frequency components of the signal's temporally averaged, spatial cross-spectral density matrix. The SVD produces a matrix containing a mutually orthogonal set of basis functions, which are proportional to the depth-dependent normal modes, and a diagonal matrix containing the singular values, which are proportional to the modal source excitations and mode eigenvalues. The conditions under which the method is expected to work are found to be (1) sufficient depth sampling of the propagating modes by the VLA receivers; (2) sufficient source-VLA range sampling, and (3) sufficient range interval traversed by the source. The mode extraction method is applied to data from the Area Characterization Test II, conducted in September 1993 in the Hudson Canyon Area off the New Jersey coast. Modes are successfully extracted from cw tones recorded while (1) the source traveled along a range-independent track with constant bathymetry and (2) the source traveled up-slope with gradual changes in bathymetry. In addition, modes are successfully extracted at multiple frequencies from ambient noise. 相似文献
90.