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Sagar Suman Panda Venkata Varaha Ravi Kumar Bera Sarwar Beg Omkar Mandal 《液相色谱法及相关技术杂志》2017,40(9):479-485
A reversed-phase ultrafast liquid chromatography method was developed for quantification of lansoprazole in pharmaceutical dosage form using analytical quality by design approach. Systematic planning and experimentation using design of experiment approach were used for method development and optimization studies. A central composite design was used for optimizing the chromatography, by choosing organic phase proportion and flow rate as the critical method variables for evaluating their effect on critical analytical attributes like resolution, plate number, and tailing factor. The optimal chromatography was accomplished on a C-18 column (250?×?4.6?mm, 5?µm) using methanol:water (70:30, v/v) as mobile phase at a flow rate of 1.0?mL/min. Photo diode array (PDA) detection was performed at 284?nm. Caffeine was used as the internal standard. Method validation studies revealed that the calibration curve was linear over 1.0–300?µg/mL. The method was found accurate with average recovery between 98.99 and 102.87%. The percent relative standard deviation values obtained for precision were as per ICH guideline and within the acceptance limits (<2%). Results of system suitability indicated superior method robustness. In a nutshell, the method was found to be highly suitable for its applicability in the determination of lansoprazole in bulk and tablet dosage form. 相似文献
44.
In the present work, we investigated the development of a bioanalytical HPLC method of rosuvastatin (RSV) calcium as per the Quality by Design (QbD)-based systematic chemometric tools. At first, the method objectives were framed and critical analytical attributes (CAAs) were chosen. Risk assessment and factor screening was performed using Hybrid Risk Matrix and Plackett–Burman design for identifying vital factors influencing the critical method parameters (CMPs). Monte-Carlo simulation analysis was conducted which confirmed excellent process robustness (Ppk >1.33) for the studied ranges of CMPs. Furthermore, systematic method development was carried out using custom experimental design, where mobile phase ratio, pH, and injection volume were taken as CMPs at three levels. The obtained trials were evaluated for peak area, retention time, theoretical plates, and peak tailing as CAAs. Mathematical response surface modeling was carried out and optimal chromatographic solution was identified using response optimizer plots. Method transfer was made to bioanalytical scale for estimation of the analyte in rat plasma samples. Extensive method validation was performed as per the ICH Q2 guideline, which indicated validation parameters within the acceptable limits. Overall, the studies construed successful development of QbD compliant HPLC method of rosuvastatin with potential utility bioanalytical testing. 相似文献
45.
Application of power ultrasound, offers potential in the degree of control over the preparation and properties of nanocrystalline zeolites, which have become increasingly important due to their diverse emerging applications. Synthesis of silicalite-1 nanocrystals from a clear solution was carried out at 348 K in the absence and presence of ultrasound of 300 and 600 W, in an attempt to investigate the effects of sonication, in this respect. Variation of the particle size and particle size distribution was followed with respect to time using a laser light scattering device with a detector set to collect back-scattered light at an angle of 173°. Product yield was determined and the crystallinity was analyzed by X-ray diffraction for selected samples collected during the syntheses. Nucleation, particle growth and crystallization rates all increased as a result of the application of ultrasound and highly crystalline silicalite-1 of smaller average particle diameter could be obtained at shorter synthesis times. The particle size distributions of the product populations, however, remained similar for similar average particle sizes. The rate of increase in yield was also speeded up in the presence of ultrasound, while the final product yield was not affected. Increasing the power of ultrasound, from 300 to 600 W, increased the particle growth rate and the crystalline domain size, and decreased both the final particle diameter and the time required for the particle growth to reach completion, while its effect on nucleation was unclear. 相似文献
46.
H. Sawada T. Yabuuchi S.P. Regan K. Anderson M.S. Wei R. Betti J. Hund M.H. Key A.J. Mackinnon H.S. McLean R.R. Paguio P.K. Patel K.M. Saito R.B. Stephens S.C. Wilks F.N. Beg 《High Energy Density Physics》2012,8(2):180-183
Results on diagnoses of laser-driven, shock-heated foam plasma with time-resolved Al 1s-2p absorption spectroscopy are reported. Experiments were carried out to produce a platform for the study of relativistic electron transport. In cone-guided Fast Ignition (FI), relativistic electrons generated by a high-intensity, short-pulse igniter beam must be transported through a cone tip to an imploded core. Transport of the energetic electrons could be significantly affected by the temperature-dependent resistivity of background plasmas. The experiment was conducted using four UV beams of the OMEGA EP laser at the Laboratory For Laser Energetics. One UV beam (1.2 kJ, 3.5 ns square) was used to launch a shock wave into a foam package target, consisting of 200 mg/cm3 CH foam with aluminum dopant and a solid plastic container surrounding the foam layer. The other three UV beams with the total energy of 3.2 kJ in 2.5 ns pulse duration were tightly focused onto a Sm dot target to produce a point X-ray source in the energy range of 1.4–1.6 keV. The quasi-continuous X ray signal was transmitted through the shock-heated Al-doped, foam layer and recorded with an X-ray streak camera. The measured 1s-2p Al absorption features were analyzed using an atomic physics code FLYCHK. Electron temperature of 40 eV inferred from the spectral analysis is consistent with 2-D DRACO Radiation-hydrodynamic simulations. 相似文献
47.
Md Amjad Beg Shivangi Obaid Afzal Md Sayeed Akhtar Abdulmalik S. A. Altamimi Afzal Hussain Md Ali Imam Mohammad Naiyaz Ahmad Sidharth Chopra Fareeda Athar 《Molecules (Basel, Switzerland)》2022,27(14)
The emergence of drug resistance and the limited number of approved antitubercular drugs prompted identification and development of new antitubercular compounds to cure Tuberculosis (TB). In this work, an attempt was made to identify potential natural compounds that target mycobacterial proteins. Three plant extracts (A. aspera, C. gigantea and C. procera) were investigated. The ethyl acetate fraction of the aerial part of A. aspera and the flower ash of C. gigantea were found to be effective against M. tuberculosis H37Rv. Furthermore, the GC-MS analysis of the plant fractions confirmed the presence of active compounds in the extracts. The Mycobacterium target proteins, i.e., available PDB dataset proteins and proteins classified in virulence, detoxification, and adaptation, were investigated. A total of ten target proteins were shortlisted for further study, identified as follows: BpoC, RipA, MazF4, RipD, TB15.3, VapC15, VapC20, VapC21, TB31.7, and MazF9. Molecular docking studies showed that β-amyrin interacted with most of these proteins and its highest binding affinity was observed with Mycobacterium Rv1636 (TB15.3) protein. The stability of the protein-ligand complex was assessed by molecular dynamic simulation, which confirmed that β-amyrin most firmly interacted with Rv1636 protein. Rv1636 is a universal stress protein, which regulates Mycobacterium growth in different stress conditions and, thus, targeting Rv1636 makes M. tuberculosis vulnerable to host-derived stress conditions. 相似文献
48.
Serkan Levent Ulviye Acar Çevik Begüm Nurpelin Sağlık Özgür Devrim Can Ümide Demir Özkay 《Phosphorus, sulfur, and silicon and the related elements》2017,192(4):469-474
The present study was undertaken to synthesize some novel lipophilic piperazine and piperidinedithiocarbamates and investigate their inhibitory potencies against cholinesterase enzymes. In the synthetic studies, 44 new compounds were isolated. The structures of the synthesized compounds were confirmed by spectroscopic analyses. Enzymatic studies were carried out using modified Ellman's assay against Acetylcholinesterase (AChE) and Butrylcholinesterase (BChE) enzymes, and it was observed that some of the compounds selectively inhibit AChE. Theoretical ADME predictions were calculated for selected compounds in the series. Enzyme kinetics and molecular docking studies were performed for the most active compound C41 and nature of inhibition and interactions between enzyme and ligand were explained. 相似文献
49.
Let E be a directed vector space with the Riesz decomposition property and F be a complete v?ctor lattice. It is proved that if G is a solid subspace of E then the subspace of all regular operators annihilating on G is a component in the space of all regular operators from E into F.12 相似文献
50.
Fasih A. Siddiqi N. Lakshminarayanaiah Mohammad N. Beg 《Journal of polymer science. Part A, Polymer chemistry》1971,9(10):2869-2875
Membrane potentials arising across four parchment-supported ferrocyanide membranes of manganese, cobalt, silver, and cadmium when they separate 1:1 electrolyte solutions of concentration C1 and C2 such that C1 = 10C2, have been measured. The data have been used according to the procedure prescribed by one of the theories of membrane potential due to Teorell and Meyers and Sievers to derive values for the quantity of charge present on the membranes. An alternative procedure employed by Altug and Hair has been considered and found to overestimate the value for the charge on the membranes. 相似文献