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271.
Development and validation of a bioanalytical method by LC‐MS/MS for the quantification of the LAFIS 10 – an antimalarial candidate – and its pharmacokinetics first evaluation 下载免费PDF全文
J. V. Laureano F. Barreto S. Gnoatto L. Tasso T. Dalla Costa B. V. de Araujo 《Biomedical chromatography : BMC》2015,29(5):664-670
A rapid and highly sensitive method by LC‐MS/MS was developed and validated for the quantification of an antimalarial candidate (LAFIS10) in rat plasma using dexamethasone as internal standard (IS). The chromatographic separation was performed with a Poroshell 120 EC‐C18 column. The mobile phase consisted of water (A) and acetonitrile (B), both containing 10 m m of ammonium formate and 0.1% formic acid, delivered in the form of elution gradient. The LAFIS10 was monitored using an electrospray ionization interface operating in the positive mode in multiple reaction monitoring mode, monitoring the transitions 681.47 → 538.2 for LAFIS10 and 393.20 → 355.30 for the IS. The flow rate was 500 μL/min. The column temperature was kept at 40 °C and the injection volume was 2 μL. The lower limit of quantification was of 10 ng/mL and linearity between 10 and 1000 ng/mL was observed, with an R2 > 0.99. The accuracy of the method was >90%. The relative standard deviations intra‐ and interday were <8.80 and <6.37%, respectively. The method showed sensitivity, linearity, precision, accuracy and selectivity required to quantify LAFIS 10 in preclinical pharmacokinetic studies according to criteria established by the US Food and Drug Administration and European Medicines Agency. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
272.
Mathias Kersemans Wim Van Paepegem Koen Van Den Abeele Lincy Pyl Filip Zastavnik Hugo Sol Joris Degrieck 《Ultrasonics》2014
The ultrasonic polar scan (UPS), either in transmission, reflection or backscatter mode, is a promising non-destructive testing technique for the characterization of composites, providing information about the mechanical anisotropy, the viscoelastic damping, the surface roughness, and more. At present, the technique is merely being used for qualitative purposes. The limited quantitative exploration and use of the technique can be primarily ascribed to limitations of current theoretical models as well as the difficulty to perform accurate, and more importantly, reproducible UPS experiments. Over the last years, we have identified several potential pitfalls in the experimental implementation of the technique which severely deteriorate the accurateness and reproducibility of a UPS. In this paper, we make an inventory of the most important difficulties, illustrate each of them by a real experiment and present a feasible mediation, either numerical or experimental in nature. Once the experimental set-up is fine-tuned to overcome these pitfalls, it is expected that the recording of high-level UPS experiments, in combination with numerical computations, will facilitate the technique to become a fully quantitative non-destructive characterization method. 相似文献
273.
Anneli Kruve Riin Rebane Karin Kipper Maarja-Liisa Oldekop Hanno Evard Koit Herodes Pekka Ravio Ivo Leito 《Analytica chimica acta》2015
This is the part II of a tutorial review intending to give an overview of the state of the art of method validation in liquid chromatography mass spectrometry (LC–MS) and discuss specific issues that arise with MS (and MS–MS) detection in LC (as opposed to the “conventional” detectors). The Part II starts with briefly introducing the main quantitation methods and then addresses the performance related to quantification: linearity of signal, sensitivity, precision, trueness, accuracy, stability and measurement uncertainty. The last section is devoted to practical considerations in validation. With every performance characteristic its essence and terminology are addressed, the current status of treating it is reviewed and recommendations are given, how to handle it, specifically in the case of LC–MS methods. 相似文献
274.
Automatic methods of photoelasticity have had a significant progress with the development of automatic acquisition and image processing methods. This article concerns RGB photoelasticity, which allows the determination of the photoelastic retardation using, usually, a single acquisition of the isochromatic fringes in white light by a colour camera. In particular, the article presents an overview of the main characteristics of RGB photoelasticity that is influence of the quarter-wave plate error, number of acquisitions, type of light source, determination of low and high fringe orders, methods for searching the retardation, scanning procedures, calibration on a material different from that under test, combined use of the RGB and phase shifting methods. A short section on the applications of RGB photoelasticity completes the article. 相似文献
275.
Velusamy B. Subramanian Naresh Kumar Katari Thirupathi Dongala Sreekantha B. Jonnalagadda 《Biomedical chromatography : BMC》2020,34(1):e4719
A quality by design (QbD) based high-resolution HPLC method is described for determination of impurities in apixaban (APX) in the tablet dosage form. Employing a simple and stability-indicating HPLC method, nine known impurities were quantified with good peak resolution. Mobile phase A (MP-A) was prepared with buffer and acetonitrile 90:10 v/v, while mobile phase B (MP-B) contained water and acetonitrile 10:90 v/v. The gradient program was 0 min, MP-A 75%, B 25%; 20 min, MP-A 65%, B 35%; 30 min, MP-A 40%, B 60%; 40min, MP-A 40%, B 60%; 42 min, MP-A 75%, B 25%; and 50 min, MP-A 75%, B 25%. The chromatographic separation was achieved using a Zorbax RX C18 250 × 4.6 mm column, 5 μm (1.0 ml min−1, 280 nm, 50 μl) and a column temperature of 40°C. Several separation studies were carried out using design of experiments to optimize the method. Validation results confirm the applicability of the developed method for quality analysis and stability studies of the regular product on the manufacturing stream. 相似文献
276.
277.
Bikash Debnath Waikhom Somraj Singh Manik Das Sanchari Goswami Mahesh Kumar Singh Debasish Maiti Kuntal Manna 《Materials Today Chemistry》2018
Alkaloids are plant secondary metabolite. They are well known nitrogen-containing natural bioactive compounds. Cutting edge research is going on alkaloids to unravel novel therapeutic approaches. Literature reveals that alkaloids contribute multiple biological activities and some alkaloids transform into active metabolites too. In this review, we have focused on marketed and experimental alkaloids. We have summarized sources and biological activities of reported alkaloids in past decades. 相似文献
278.
《Journal of separation science》2018,41(6):1257-1265
Asenapine is a recent drug approved in the European Union for the treatment of bipolar disorder. An original approach has been developed for asenapine analysis in patients treated with the drug, including miniaturized microsampling procedures, separation and quantitation of drug enantiomers. An original enantioselective method based on high‐performance liquid chromatography with diode array detection was developed and applied to the determination of asenapine enantiomer levels in innovative haematic samples: four micromatrices have been tested, two based on dried matrix spots (dried blood spots and dried plasma spots) and two based on volumetric absorptive microsampling (from blood and plasma). Chiral separation was achieved on a cellulose‐tris(3,5 dimethylphenylcarbamate) column, with a mobile phase containing bicarbonate buffer and acetonitrile. The method was validated with satisfactory results of linearity and precision on all matrices that showed also a significant performance in terms of stability, feasibility and reliability, when compared to fluid plasma sampling, handling and processing. Among micromatrices, both volumetric absorptive microsampling types were superior to dried matrix spots in terms of data reproducibility and correspondence with plasma levels. The bioanalytical approach proposed herein provides for the first time a chiral high‐performance liquid chromatographic method for the determination of asenapine enantiomers, coupled to a very effective microsampling strategy. 相似文献
279.
Polymethoxyflavones (PMFs), which exist exclusively in the citrus genus, have biological activities including anti-inflammatory, anticarcinogenic, and antiatherogenic properties. A validated RPLC method was developed for quantitative analysis of six major PMFs, namely nobiletin, tangeretin, sinensetin, 5,6,7,4'-tetramethoxyflavone, 3,5,6,7,3',4'-hexamethoxyflavone, and 3,5,6,7,8,3',4'-heptamethoxyflavone. The polar embedded LC stationary phase was able to fully resolve the six analogues. The developed method was fully validated in terms of linearity, accuracy, precision, sensitivity, and system suitability. The LOD of the method was calculated as 0.15 microg/mL and the recovery rate was between 97.0 and 105.1%. This analytical method was successfully applied to quantify the individual PMFs in four commercially available citrus peel extracts (CPEs). Each extract shows significant difference in the PMF composition and concentration. This method may provide a simple, rapid, and reliable tool to help reveal the correlation between the bioactivity of the PMF extracts and the individual PMF content. 相似文献
280.
Stilbenes and zeranol are nonsteroidal estrogenic growth promoters which are banned in the European Union (EU) for use in
food-producing animals by Council Directive 96/22/EC. A liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was
developed for the screening and confirmation of stilbenes (diethylstilbestrol, dienestrol, hexestrol) and resorcylic acid
lactones (zeranol and its metabolites taleranol and zearalanone as well as the mycotoxins α-zearalenol, β-zearalenol and zearalenone)
in bovine urine. The method permits the confirmation and quantification of stilbenes and resorcylic acid lactones at levels
below 1 μg L−1 and 1.5 μg L−1, respectively. The validation was carried out according to Commission Decision 2002/657/EC, Chap. 3.1.3 “alternative validation”
by a matrix-comprehensive in-house validation concept. Decision limit CCα, detection capability CCβ, recovery, repeatabiliy,
within-laboratory reproducibility and the uncertainty of measurement were calculated. Furthermore, a factorial effect analysis
was carried out to identify factors that have a significant influence on the method. Factors considered to be relevant for
the method in routine analysis (e.g. operator, matrix condition, storage duration of the extracts before measurement, different
cartridge lots, hydrolysis conditions) were systematically varied on two levels. The factorial analysis showed that different
cartridge lots, storage durations and matrix conditions can exert a relevant influence on the method. 相似文献