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991.
A triterpenoid saponin, guaianin O (1), oleanolic acid 3-O-{α-L-rhamnopyranosyl-(1 → 2)-[β-D-glucopyranosyl-(1 → 3)]-α-L-arabinopyranoside}-28- O-[β-D-glucopyranosyl]-ester, was isolated from the n-butanol extract of flowers of Guaiacum officinale L. The structural elucidation of 1 was accomplished by extensive studies of both one and two dimensional 1H, 13C-NMR spectra, the FAB mass spectrum, and alkaline and acid hydrolyses. 相似文献
992.
A simple, rapid and efficient sample preparation technique, dispersive liquid-liquid microextraction, coupled with gas chromatography-flame ionization detection has been developed to determine N-methylpyrrolidine in cefepime. The effect of various experimental factors on the preparation procedure, such as the nature and volume of extraction and disperser solvents, extraction time, the nature of buffer and its pH, and salt effect, was investigated, optimized and the following results were obtained: extraction solvent, chloroform; dispersive solvent and solvent for dissolving cefepime, a mixture of methanol/water (88:12, v/v); salting out agent, NaCl; and buffer, carbonate/bicarbonate (C=0.5?M, pH=12). The optimized conditions were applied to the real sample (cefepime) for the extraction and determination of N-methylpyrrolidine. The calibration graph is linear from 0.02 to 850?mg/L with the square of correlation coefficient 0.999. LOD and LOQ are 6.4 and 21.2?μg/L in solution, respectively, and 0.2 (2×10(-5) ) and 0.6 (6×10(-5) ) μg/g (%, w/w) in cefepime powder, respectively, using sample size 50?mg. Repeatability of the method is good and RSD% for six repeated experiments (C=170?mg/L) is 6.35%. 相似文献
993.
Mohd Marsin Sanagi Mazidatulakmam Miskam Wan Aini Wan Ibrahim Dadan Hermawan Hassan Y. Aboul‐Enein 《Journal of separation science》2010,33(14):2131-2139
A three‐phase hollow fiber liquid‐phase microextraction method coupled with CE was developed and used for the determination of partition coefficients and analysis of selected nitrophenols in water samples. The selected nitrophenols were extracted from 14 mL of aqueous solution (donor solution) with the pH adjusted to pH 3 into an organic phase (1‐octanol) immobilized in the pores of the hollow fiber and finally backextracted into 40.0 μL of the acceptor phase (NaOH) at pH 12.0 located inside the lumen of the hollow fiber. The extractions were carried out under the following optimum conditions: donor solution, 0.05 M H3PO4, pH 3.0; organic solvent, 1‐octanol; acceptor solution, 40 μL of 0.1 M NaOH, pH 12.0; agitation rate, 1050 rpm; extraction time, 15 min. Under optimized conditions, the calibration curves for the analytes were linear in the range of 0.05–0.30 mg/L with r2>0.9900 and LODs were in the range of 0.01–0.04 mg/L with RSDs of 1.25–2.32%. Excellent enrichment factors of up to 398‐folds were obtained. It was found that the partition coefficient (Ka/d) values were high for 2‐nitrophenol, 3‐nitrophenol, 4‐nitrophenol, 2,4‐dinitrophenol and 2,6‐dinitrophenol and that the individual partition coefficients (Korg/d and Ka/org) promoted efficient simultaneous extraction from the donor through the organic phase and further into the acceptor phase. The developed method was successfully applied for the analysis of water samples. 相似文献
994.
Ali Reza Fakhari Saeed Nojavan Samad Nejad Ebrahimi Christopher John Evenhuis 《Journal of separation science》2010,33(14):2153-2159
This study investigated the use of ultrasound‐assisted extraction to improve the extraction efficiency of morphine, codeine and thebaine from the papaver plants. Extraction conditions such as type of solvent, temperature, duration, frequency and power level of ultrasonic were optimized and the influences of different parameters on resolution of alkaloids in CE were studied. The optimized condition for CE separation includes a sodium phosphate buffer (100 mM, pH 3.0) containing 5 mM α‐CD. The optimized extraction conditions for ultrasound‐assisted extraction was an extraction time of 1 h, an ultrasonic frequency of 60 kHz with water–methanol (80:20) at 40°C as the extraction solvent. The LOD for alkaloids was found to be 0.1 μg/mL at a signal‐to‐noise ratio of 3:1. The RSDs for peak areas were in the range of 1.4–4.4%. The amounts of opium alkaloids (mg/100 g dried sample) in four Iranian papaver plants were found to be in the range of 7.8–8.7 (morphine), 5.5–9.5 (codeine) and 1.4–10.4 (thebaine). It should be emphasized that no cleanup of the filtered extract was required; hence, direct determination after extraction drastically simplifies the analytical process. 相似文献
995.
Nazim Hasan Hui-Fen Wu Yi-Hsien Li Mohd Nawaz 《Analytical and bioanalytical chemistry》2010,396(8):2909-2919
We introduce a simplified sample preparation method using bare TiO2 nanoparticles (NPs) to serve as multifunctional nanoprobes (desalting, accelerating, and affinity probes) for effective enrichment
of phosphopeptides from microwave-assisted tryptic digestion of phosphoproteins (α-casein, β-casein and milk) in Electrospray
Ionization Mass Spectrometry (ESI-MS) and Matrix Assisted Laser Desorption Ionization Mass Spectrometry (MALDI-MS). The results
demonstrate that TiO2 NPs can effectively enrich and accelerate the digestion reactions of phosphoproteins in aqueous solutions and also from complex
real samples. After the microwave experiments, we directly injected the resulting solutions into the ESI-MS and MALDI-MS systems
for analysis, and excellent sensitivity was achieved without the need for any washing procedure or separation process. The
reasons are attributed to the high binding affinity and selectivity of TiO2 NPs toward phosphopeptides. Thus, phosphopeptides can be adsorbed onto the TiO2 NP surface. The digested or partially digested phosphoproteins can be concentrated onto the TiO2 NP surface. This results in the effective or complete digestion of phosphoproteins in a short period of time (45 s). In addition,
high sensitivity and sequence coverage of phosphopeptide can be obtained using TiO2 NPs as microwave absorbers and affinity probes in MALDI-MS and ESI-MS. This is due to the photocatalytic nature of the TiO2 NPs because the absorption of microwave radiation that can accelerate the activation of trypsin for efficient digestion of
phosphoproteins and enhances the ionization of phosphopeptides. The lowest concentrations detected for ESI-MS and MALDI-MS
were 0.1 μM and 10 fmol, respectively, for α-casein. Comparing the two-step approach of TiO2 NPs with microscale TiO2 particles, the microscale TiO2 particles shows no effect on the microwave-assisted tryptic digestion of phosphoproteins. The current approach offers multiple
advantages, such as great simplicity, high sensitivity and selectivity, straightforward and separation/washing-free technique
for phosphorpeptide enrichment analysis. 相似文献
996.
Khaled Boughzala Nadia Gmati Khaled Bouzouita Ali Ben Cherifa Pierre Gravereau 《Comptes Rendus Chimie》2010,13(11):1377-1383
Several studies demonstrated the ability of britholites to retain radionuclides such as the caesium and actinides. Therefore, three compounds with formulas Sr8LaCs(PO4)6F2, Sr7La2Cs(PO4)5(SiO4)F2 and Sr2La7Cs(SiO4)6F2, were prepared by solid state reaction. However, it seems that only the mono-silicated composition was obtained in a pure state. In this present work, the X-ray diffraction and magnetic nuclear resonance have been used to investigate the structure for this composition. The results showed that in fact this phase was not pure, but it was mixed with a secondary phase, SrLaCs(PO4)2. The refinement by the Rietveld method allowed also to precise the distribution of La3+ and Cs+ ions between the two cationic sites of the apatite. 相似文献
997.
An HPLC method was developed for the simultaneous determination of nine compounds of Nigella sativa L. The separation was achieved within 23 min by using C18 column material, a water-acetonitrile mobile phase, both containing 0.1% acetic acid gradient system and a temperature of 35 degrees C. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ of nine compounds were in the range of 0.09-10 and 0.3-25 microg/mL, respectively. The wavelength used for quantification with the diode array detector was 205 and 260 nm. LC/MS coupled with electrospray ionization interface method is described for the identification of compounds in N. sativa L. samples. This method involved the use of [M+H]+ and [M+Na]+ ions in the positive ion mode with extracted ion chromatogram. 相似文献
998.
Zafar A. Siddiqi M. Shahid Mohd Khalid Shabana Noor Sarvendra Kumar 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2010,75(1):61-68
The newly prepared homo-bimetallic complexes [M2(imda)2(H2O)4], [M2(imda)2(Bipy)2] (M = Co, Ni or Cu) and [Fe2(imda)2(H2O)3Cl] (H2imda = iminodiacetic acid and Bipy = 2,2′-bipyridine) have been studied employing IR, FAB-mass, 1H and 13C NMR, EPR and ligand field spectra, which indicated a high-spin state of metal ion with hexa-coordinate environment. 57Fe Mössbauer data of the homo-bimetallic complex [Fe2(imda)2(H2O)3Cl] confirm a high-spin configuration with Fe (±3/2 → 1/2) nuclear transitions and the presence of Kramer's double degeneracy. At RT, the spin–spin interactions of the neighbouring nuclei (Fe3+–Fe3+ = S5/2–S5/2) are anti-ferromagnetically coupled. However, at LNT, the complex acquires a mixed-valent [FeIII–FeII] composition corroborated from the X-band EPR data. CV studies indicated the presence of quasi-reversible redox CuII/I, CuII/III, FeIII/II, FeIII/I and FeII/I couples. 相似文献
999.
Zafar A. Siddiqi Mohd Khalid Sarvendra Kumar M. Shahid Shabana Noor 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2010,75(2):841-845
Spectral and molecular model computations on homo-dinuclear complexes [M2L2(H2O)2Cl2] [L = 1-(salicylaldeneamino)-3-hydroxypropane, M = Cr3+, Mn3+, Fe3+, Co3+, Ni3+ or Cu3+] are consistent with a distorted hexa-coordinate geometry. X-band EPR spectral data indicated a rhombic distortion around Cu(II) ion. Magnetic moment and 57Fe Mössbauer data confirmed a high-spin state electronic configuration (t2g3eg2, S = 5/2) and asymmetric ligand environment around Fe(III) with nuclear transitions Fe(±3/2 → 1/2) exhibiting Kramer's double degeneracy. The neighboring Fe(III) nuclei in the homo-dinuclear species are antiferromagnetically coupled. 相似文献
1000.
M. Hussain M. Hanif S. Ali S. Shahzadi M. S. Ahmad B. Mirza H. S. Evans 《Journal of the Iranian Chemical Society》2010,7(1):155-163
New organotin(IV) compounds containing the carboxylate ligand 2,3-methylenedioxybenzoic acid (HL) have been synthesized with the general formula R2SnL2 (R = Me, Et, n-Bu, Ph and n-Oct) and R3SnL (R = n-Bu). All compounds have been studied in the solution state by multinuclear NMR (1H, 13C and 119Sn) by using the non-coordinating solvent and also in solid sate by FTIR, mass spectrometry and X-ray crystallography. Spectroscopic data have shown that methylenedioxy moiety does not coordinate with tin atom and the coordination site is actually -COO group, as is proved by X-ray structure determination. The solid state structure of compound (2) has been determined by X-ray crystallography which shows that the complex (2) has distorted octahedral geometry. These complexes have been evaluated in vitro against crown gall tumor and antibacterial activity. Interesting results were noticed during the bio-activity screenings, which proved their in vitro biological potential and possible use as drugs. 相似文献