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21.
Summary A new and highly sensitive HPLC method for the simultaneous determination of pirarubicine (THP-doxorubicin) and its metabolites, adriamycin and adriamycinol, in human plasma, is described. Samples were treated by liquid-liquid extraction, the organic phase removed and the residue dissolved in methanol. Separation was on a Lichrocart Supersher RP 8 column, (250×4 mm) 4 m, with a mobile phase of acetonitrile/methanol/formate-buffer. 相似文献
22.
Simultaneous isolation and determination of esculin and rutin in natural materials using SPE and HPLC 总被引:1,自引:0,他引:1
Summary Esculin (ESC) and rutin (RUT) have been simultaneously isolated from pharmaceutical natural materials by solid phase extraction (SPE). Determination of both substances was performed by reversed phase high performance liquid chromatography (RPHPLC) with UV detection. Optimization of the separation conditions showed that simultaneous isolation and determination of rutin and esculin from pharmaceutical material was possible. The recovery obtained was not lower than 95±2%. 相似文献
23.
R. Matissek 《Chromatographia》1989,28(1-2):34-38
Summary Antimicrobially active formulations based on 2-methyl-3(2H)-isothiazolone and 5-chloro-2-methyl-3(2H)-isothiazolone (Kathon CG, Euxyl K 100) are incorporated into manufactured cosmetics as preservatives. In this paper we report on the analysis of these active components by means of liquid chromatography. It is conventional for the original methylisothiazolone components in cosmetics to be analyzed by reversed phase high-performance liquid chromatography after column chromatographic separation and flash chromatographic purification. In our new analytical method the methylisothiazolones are converted into the respective -thiosubstituted acrylamide derivatives, which are ionic substances, with the help of the nucleophilic reagent hydrogensulfite. An ion pair high-performance liquid chromatographic method has been developed for the separation and quantification of these derivatives. 相似文献
24.
Comprehensive two-dimensional liquid chromatographic separation by means of a combination of ion-exchange chromatography (IEC)
and reversed-phase liquid chromatography (RPLC) has been realized and applied to the analysis of components of a traditional
Chinese medicine Flos Lonicera. In the first dimension the components of a Flos Lonicera extract is separated on strong anion-exchange (SAX) column according to the charge-exchange properties of the components.
In the second dimension the components are further fractionated by reversed-phase liquid chromatography (on ODS) on the basis
of their hydrophobicity. The RPLC effluent is desalted and split and the components are identified on-line by use of both
diode-array detection and mass spectrometry with atmospheric pressure chemical ionization (APCI–MS). In this way, the extract
of Flos Lonicera can be rapidly separated, desalted, and analyzed, with determination of molecular weight. More than 58 components of an extract
of Flos Lonicera were well resolved and six were tentatively identified from their UV and mass spectra. 相似文献
25.
M. Piñeiro-Iglesias M. Miñones-Vázquez E. Vázquez-Blanco S. Muniategui-Lorenzo P. López-Mahía D. Prada-Rodríguez 《Chromatographia》2002,56(7-8):483-488
Summary The aim of this work is to establish the best conditions for concentration and purification steps in the trace analysis of
aliphatic and polycyclic aromatic hydrocarbons (PAH) from atmospheric particulate matter by gas chromatography-flame ionisation
detection (GC-FID) and high performance liquid chromatography with ultraviolet and fluorescence detection (HPLC-UV-FL). The
best results for the more volatile compound were obtained with a combination of rotary evaporation and a stream of nitrogen
(near to 100% for aliphatic hydrocarbons and from 70 to 105% for PAH). Two types of solid phase extraction (SPE)cartridges
(Supelclean
tm
LC-Silica SPE tubes and Sep-Pak? Plus silica cartridges) and glass column were examined for the purification and fractionation step. Blank chromatograms of
both types of cartridges analysed by GC-FID made this study difficult, because a PSS (programmed split-splitless) injector
was employed thereby increasing the sensitivity. This problem was not observed in the HPLC-UV-FL blank chromatograms of these
cartridges. Glass columns filled with silica and alumina were chosen because no interference was found in the GC-FID blank
chromatograms and the best recoveries in the fractionation of both aliphatic hydrocarbons and PAH were achieved. This is especially
important when aliphatic hydrocarbons concentrations are lower than 1 μg mL−1. Finally, the selected conditions were applied to the analysis of hydrocarbons in real atmospheric particulate samples. 相似文献
26.
Summary A method for determining histamine in wine by precolumn derivatization with PITC (phenylisothiocyanate) with reversed-phase HPLC and UV detection is reported. Histamine can be determined together with the 24 amino acids within 40 min, or separately in a shorter time (less than 4 min) if a prior solid phase extraction clean-up is used. 相似文献
27.
Summary Chiral stationary phases (CSPs) for liquid chromatography were prepared by the way of an activated carbamate intermediate.
The amino group of aminopropylsilyl silica gel was first activated by carbamylation with disuccinimido carbonate (DSC). The
obtained activated carbamate silica gel (ACsil) proved useful as an intermediate for the preparation of urea-type CSPs. The
reaction of ACsil with (S)- of (R)-1-(α-naphthyl)-ethylamine gave naphthylethylurea type CSPs. These CSPs were also obtained
directly from aminopropylsilyl silica gel by its reaction with optically active (S)- or (R)-succinimido 1-(α-naphthyl)ethyl
carbamate (SINEC). Several phenylthiohydantoin amino acid enantiomers and p-bromophenylcarbamyl amino acid enantiomers were
resolved on the CSPs by elution with aqueous mobile phase. 相似文献
28.
Summary This paper reports the results of a study on the use of a new polymer-based, strong anion-exchange, stationary phase for rapid
and selective separation of carbohydrates and related compounds by high-pH, anion-exchange chromatography with pulsed amperometric
detection. The new adsorbent has been obtained by direct nitration of 2.8 μm, spherical non-porous highly cross-linked, styrene-divinylbenzene
copolymer beads, followed by reduction of superficially introduced nitro groups with nascent hydrogen and quaternization of
the resultant amino groups with iodomethane. It is reported that by optimizing the ionic strength of the mobile phase, columns
packed with the new anion-exchanger can be successfully employed to separate, either in isocratic or gradient elution mode,
oligosaccharides, positional isomers of gluco-disaccharides, as well as uronic acids and sugar monophosphates. 相似文献
29.
Resolution of enantiomers by HPLC on cellulose derivatives 总被引:4,自引:0,他引:4
Summary Various polysaccharide derivatives, particularly cellulose derivatives, were synthesized and used as chiral stationary phases
for optical resolution by HPLC after being adsorbed on macroporous silica gel. Cellulose triacetate (CTA-II), which was synthesized
under homogeneous conditions, showed a chiral recognition ability for many racemates. Other cellulose derivatives such as
cellulose tribenzoate (OB), cellulose-trisphenylcarbamate (OC), cellulose tribenzyl ether (OE), and cellulose tricinnamate
(OK) also showed unique chiral recognition. Among other polysaccharide derivatives, curdlan triacetate was also exhibited
an effective chiral recognition.
Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984 相似文献
30.
Summary 2,8-Dihydroxyadeninuria and xanthinuria are inborn enzyme disorders which must be under lifelong therapeutic control. Quantitative
determination of 2,8-DHA and xanthine using reversed phase HPLC was performed. A new application for the separation of purines
shortens analysis-time. Examples of the determination of 2,8-DHA and xanthine before and under certain therapies are shown.
Long term monitoring of the patients offers the possibility of a reliable prophylaxis against stone recurrence. 相似文献