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991.
Long Yuan Mohammed Jemal Anne‐Francoise Aubry 《Rapid communications in mass spectrometry : RCM》2012,26(12):1465-1474
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L. A. Parry‐Jones S. M. Beldon P. D. Brimicombe D. Rodriguez‐Martin S. J. Elston 《Liquid crystals》2013,40(7):767-773
X‐ray diffraction studies are carried out in order to probe the smectic layer structure in liquid crystal devices filled with FLC mixture SCE8 and AFLC mixture CS4001, at a temperature just above the SmA?–SmC? phase transtion. The data gathered are time‐resolved in synchronization with a bipolar voltage pulse applied across the device. The layers are observed to move dynamically and reversibly with voltage application and removal, giving evidence for temporary vertical chevron formation due to the electroclinic effect on a timescale consistent with this phenomenon. 相似文献
997.
The steric effect of an aryloxido group on the synthesis and molecular structures of ytterbium aryloxides supported by β‐diketiminato ligand L (L = [N(2,6‐Me2C6H3)C(Me)]2CH?) is reported. Reactions of β‐diketiminatoytterbium dichloride, LYbCl2(THF)2, with NaOAr1 in THF (Ar1 = [2,6‐tBu2‐4‐MeC6H2], THF = tetrahydrofuran) at 60°C gave the corresponding ytterbium complexes LYb(OAr1)Cl(THF) ( 1 ) and LYb(OAr1)2 (1), depending on the molar ratio of dichloride to sodium aryloxide, respectively, while the same reactions with NaOAr2 and NaOAr3 (Ar2 = [2,6‐iPr2C6H3], Ar3 = [2,6‐Me2C6H3]) in 1:1 or 1:2 molar ratio in THF afforded only bisaryloxide complexes LYb(OAr2)2(THF) (1) and LYb(OAr3)2(THF) ( 4 ) in good yields, respectively. Complexes 1 , 2 , 3 , 4 were fully characterized, including X‐ray crystal structure analyses. All the complexes are efficient pre‐catalysts for the catalytic addition of amines to carbodiimides giving guanidines. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
998.
Shi‐jia Liu Ling Zhou Jun Zhang Chang‐yin Li Zi‐xiu Liu Wen‐zheng Ju 《Biomedical chromatography : BMC》2013,27(4):515-519
A highly sensitive liquid chromatography–tandem mass spectrometry method was developed and validated for the determination of limonin in beagle dog plasma using nimodipine as internal standard. The analyte and internal standard (IS) were extracted with ether followed by a rapid isocratic elution with 10 mm ammonium acetate buffer–methanol (26:74, v/v) on a C18 column (150 × 2.1 mm i.d.) and subsequent analysis by mass spectrometry in the multiple reaction monitoring mode. The precursor to product ion transitions of m/z 469.4 → 229.3 and m/z 417.2 → 122.0 were used to measure the analyte and the IS. The assay was linear over the concentration range of 0.625–100 ng/mL for limonin in dog plasma. The lower limit of quantification was 0.312 ng/mL and the extraction recovery was >90.4% for limonin. The inter‐ and intra‐day precision of the method at three concentrations was less than 9.9%. The method was successfully applied to pharmacokinetic study of limonin in dogs. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
999.
Ultra‐high pressure LC for astaxanthin determination in shrimp by‐products and active food packaging
A. Sanches‐Silva T. Ribeiro T. G. Albuquerque P. Paseiro R. Sendón A. Bernaldo de Quirós J. López‐Cervantes D. I. Sánchez‐Machado H. Soto Valdez I. Angulo G. P. Aurrekoetxea H. S. Costa 《Biomedical chromatography : BMC》2013,27(6):757-764
Nowadays, there is increasing interest in natural antioxidants from food by‐products. Astaxanthin is a potent antioxidant and one of the major carotenoids in crustaceans and salmonids. An ultra‐high pressure liquid chromatographic method was developed and validated for the determination of astaxanthin in shrimp by‐products, and its migration from new packaging materials to food simulants was also studied. The method uses an UPLC® BEH guard‐column (2.1 × 5 mm, 1.7 µm particle size) and an UPLC® BEH analytical column (2.1 × 50 mm, 1.7 µm particle size). Chromatographic separation was achieved using a programmed gradient mobile phase consisting of (A) acetonitrile–methanol (containing 0.05 m ammonium acetate)–dichloromethane (75:20:5, v/v/v) and (B) ultrapure water. This method was evaluated with respect to validation parameters such as linearity, precision, limit of detection, limit of quantification and recovery. Low‐density polyethylene films were prepared with different amounts of the lipid fraction of fermented shrimp waste by extrusion, and migration was evaluated into food simulants (isooctane and ethanol 95%, v/v). Migration was not detected under the tested conditions. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
1000.
Ji‐Xin Tian Can Peng Lei Xu Yuan Tian Zun‐Jian Zhang 《Biomedical chromatography : BMC》2013,27(6):775-783
In this report, the in vitro metabolism of Strychnos alkaloids was investigated using liquid chromatography/high‐resolution mass spectrometry for the first time. Strychnine and brucine were selected as model compounds to determine the universal biotransformations of the Strychnos alkaloids in rat liver microsomes. The incubation mixtures were separated by a bidentate‐C18 column, and then analyzed by on‐line ion trap/time‐of‐flight mass spectrometry. With the assistance of mass defect filtering technique, full‐scan accurate mass datasets were processed for the discovery of the related metabolites. The structural elucidations of these metabolites were achieved by comparing the changes in accurate molecular masses, calculating chemical component using Formula Predictor software and defining sites of biotransformation based upon accurate MSn spectral information. As a result, 31 metabolites were identified, of which 26 metabolites were reported for the first time. These biotransformations included hydroxylation, N‐oxidation, epoxidation, methylation, dehydrogenation, de‐methoxylation, O‐demethylation, as well as hydrolysis reactions. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献