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961.
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964.
Evaluation of liquid chromatography–ion trap–time of flight hybrid mass spectrometry on the quantitative analysis for ginsenosides
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Yan Liang Rong Xing Tai Rao Lijun Zhou Qian Wang Hanxu Fu Wei Ye Guangji Wang 《Biomedical chromatography : BMC》2014,28(7):1003-1010
It is ideal and desirable for a single instrument to meet the requirement of both qualitative and quantitative analysis of complicated components in pharmacokinetic research for herbal medicine. Liquid chromatography combined with hybrid ion trap and time‐of‐flight mass spectrometry (LCMS‐IT‐TOF) was recently confirmed as a very powerful tool for the qualitative analysis of both target and nontarget components in herbal medicines. The present study was designed to investigate the feasibility of LCMS‐IT‐TOF on quantitative analysis of ginsenosides in biological matrices. A simple liquid–liquid extraction procedure was followed by injection of the extracts onto a C18 column with gradient elution and detection based on LCMS‐IT‐TOF system in negative scan mode. The developed method was validated with respect to the limit of quantification, linear dynamic range, precision, accuracy, matrix effects and stabilities. All the results suggested that the presently developed method was sufficiently sensitive and robust enough to simultaneously monitor 15 ginsenosides with diverse properties and a large range of concentration differences. Therefore, this method would be expected to be highly useful for comprehensive studies of ginsenosides in complicated matrix. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
965.
Chun‐Wei Lin Pi‐Tai Chou Prof. Yong‐Hong Liao Ying‐Chih Lin Prof. Ching‐Ting Chen Yu‐Chun Chen Chin‐Hung Lai Dr. Bo‐So Chen Yi‐Hung Liu Dr. Chih‐Chieh Wang Prof. Mei‐Lin Ho Prof. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2010,16(12):3770-3782
Strategically designed salen ligand 2,3‐bis[4‐(di‐p‐tolylamino)‐2‐hydroxybenzylideneamino]maleonitrile ( 1 ), which has pronounced excited‐state charge‐transfer properties, shows a previously unrecognized form of photoisomerization. On electronic excitation (denoted by an asterisk), 1Z *→ 1E isomerization takes place by rotation about the C2? C3 bond, which takes on single‐bond character due to the charge‐transfer reaction. The isomerization takes place nonadiabatically from the excited‐state ( 1Z ) to the ground‐state ( 1E ) potential‐energy surface in the singlet manifold; 1Z and 1E are neither thermally inconvertible at ambient temperature (25–30 °C), nor does photoinduced reverse 1E *→ 1Z (or 1Z *) isomerization occur. Isomers 1Z and 1E show very different coordination chemistry towards a ZnII precursor. More prominent coordination chemistry is evidenced by a derivative of 1 bearing a carboxyl group, namely, N,N′‐dicyanoethenebis(salicylideneimine)dicarboxylic acid ( 2 ). Applying 2Z and its photoinduced isomer 2E as building blocks, we then demonstrate remarkable differences in morphology (sphere‐ and needlelike nanostructure, respectively) of their infinite coordination polymers with ZnII. 相似文献
966.
967.
A simple and sensitive liquid chromatographic method is described for the quantitative analysis of gabapentin in human plasma. Gabapentin (GBP) is an anticonvulsant and widely used in the treatment of epilepsy. No peculiar chromophore is available on gabapentin moiety for direct analysis by absorption spectrophotometry. In human plasma after deproteinisation with acetonitrile, gabapentin was derivatized with a fluorescent reagent, (2-naphthoxy)acetyl chloride (NAC) in borate buffer (pH 10.0). The resulting naphthoxy derivative of gabapentin was separated on a phenyl-hexyl column with a mobile phase consisting of a mixture of sodium acetate buffer (100 mM; pH 5.0)-methanol (32:68, v/v) used in isocratic mode. Using fluorimetric detection (excitation at 225 nm and emission at 360 nm), a low detection limit of about 0.04 microM (S/N = 3, 10 microl injected) was reached. The relative standard deviations (RSD) of the method for intra- and inter- day analyses (n = 5) are between 2.7 and 4.0%, respectively. The method was successfully applied to the analysis of gabapentin in plasma from dosed patients for therapeutic drug monitoring. 相似文献
968.
The gravitational force exerts an important effect on the counter-current chromatography (CCC) and has been used to retain the stationary phase and improve the efficiency in the various CCC separations. This paper deals with the effect of gravitational force on type-J CCC, one of the most popular CCC methods by the mathematical analysis for the first time. The theoretical analyses reveal a close relationship between the effect of gravitational force, the placed orientation of type-J CCC apparatus, and the revolutional speed. Two placed orientations are more suitable for preparative CCC separation: one is common horizontal, and the other upright. Thus, there are three optimum conditions for type-J CCC separation, the first using horizontal apparatus at very low revolutional speed around 10rpm in the gravitational filed, the second by use of upright apparatus at moderate revolutional speed around 100rpm in the three-dimensional complex force field composed of centrifugal and orthogonal gravitational force, and the third employing the apparatus placed at any orientation including horizontal and upright CCC apparatus at high revolutional speed above 300rpm in the centrifugal force field. Therefore, we should consider the effect of gravitation force on CCC at the selection of proper operational conditions according to properties of two immiscible phases, the desired revolutional speed and the parameters of apparatus in order to utilize efficiently the effect of gravitational force. These analyses and results will benefit to improve the efficiency of CCC separation, especially large-scale industrial preparation. 相似文献
969.
We describe phenomena of colloidal particle transport and separation inside single microdroplets of water floating on the surface of dense fluorinated oil. The experiments were performed on microfluidic chips, where single droplets were manipulated with alternating electric fields applied to arrays of electrodes below the oil. The particles suspended in the droplets were collected in their top region during the evaporation process. Experimental results and numerical simulations show that this microsepration occurs as a result of a series of processes driven by mass and heat transfer. An interfacial tension gradient develops on the surface of the droplet as a result of the nonuniform temperature distribution during the evaporation. This gradient generates an internal convective Marangoni flow. The colloidal particles transported by the flow are collected in the top of the droplets by the hydrodynamic flux, compensating for evaporation through the exposed top surface. The internal flow pattern and temperature distribution within evaporating droplets were simulated using finite element calculations. The results of the simulation were consistent with experiments using tracer particles. Such microseparation processes can be used for on-chip synthesis of advanced particles and innovative microbioassays. 相似文献
970.
Direct analysis of mercury in Traditional Chinese Medicines using thermolysis coupled with on-line atomic absorption spectrometry 总被引:1,自引:0,他引:1
The purpose of this study is to develop and apply a mercury analyzer system capable of quantitative analysis of mercury in Traditional Chinese Medicines (TCM) drugs in the concentrations range from ng g−1 to mg g−1. No sample pre-treatment was needed and this greatly simplifies the analytical procedure and minimizes potential sources of contamination. The precisions of analyzing solid mercury standard sample and real TCM materials were 2.1% and 2.5-8.2%, respectively; and the recovery based on the analysis of standard reference materials ranged from 95.2% to 105%. The performance of the method has been compared with inductively coupled plasma-mass spectrometry (ICP-MS) technique and excellent agreements were observed between the two methods. The method has been applied to the investigation of Hg content in several TCM drugs containing or not containing cinnabar. Mercury concentration in the same TCM products differs widely with different manufacturers, suggesting that external contamination and the Hg presence in raw herbal materials are the main sources of Hg. In addition, comparison of mercury thermal releasing profiles between TCM drug and cinnabar suggests that mercury conversion from cinnabar to biological matrices-bound Hg could occur because of the aid of other ingredients in the formulated drug. 相似文献