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991.
Boronate affinity solid phase microextraction (BA-SPME) is a new format appeared recently with great potential for specific extraction of cis-diol-containing compounds. Unlike conventional SPME, BA-SPME relies on covalent interactions and thereby features with specific selectivity, eliminated matrix effect and manipulable capture/release. However, only on-fiber BA-SPME and its off-line combination with high performance liquid chromatography (HPLC) have been reported so far. In this study, we report on-line coupling of in-tube BA-SPME with HPLC-electrospray ionization tandem mass spectroscopy (in-tube BA-SPME-HPLC-ESI-MS/MS) for the specific and sensitive determination of cis-diol-containing biomolecules. A boronate affinity extraction phase was prepared onto the inner surface of the capillary by copolymerization of vinylphenylboronic acid (VPBA) and ethylene glycol dimethacrylate (EDMA). The extraction conditions were optimized by choosing appropriate extraction/desorption solutions and extraction time. The extraction capacity, linear range, reproducibility and life-time were investigated. The developed method was successfully applied for the determination of dopamine in urine samples. Since many cis-diol-containing compounds are of great biological importance, the in-tube BA-SPME-HPLC method can be a promising tool. 相似文献
992.
From the whole plants of E. ritro L., the three new sesquiterpenoids (3α,4α,6α)‐3,13‐dihydroxyguaia‐7(11),10(14)‐dieno‐12,6‐lactone ( 1 ), (3α,4α,6α,11β)‐3‐hydroxyguai‐1(10)‐eno‐12,6‐lactone ( 2 ), and (11α)‐11,13‐dihydroarglanilic acid methyl ester (=(4β,6α,11α)‐4,6‐dihydroxy‐1‐oxoeudesm‐2‐en‐12‐oic acid methyl ester; 3 ), together with eight known sesquiterpenoids, were isolated. Their structures were elucidated through analysis of spectroscopic data including extensive 2D‐NMR. 相似文献
993.
In the proposed method, an extraction solvent with a lower toxicity and density than the solvents typically used in dispersive liquid-liquid microextraction was used to extract seven polychlorinated biphenyls (PCBs) from aqueous samples. Due to the density and melting point of the extraction solvent, the extract which forms a layer on top of aqueous sample can be collected by solidifying it at low temperatures, which form a layer on top of the aqueous sample. Furthermore, the solidified phase can be easily removed from the aqueous phase. Based on preliminary studies, 1-undecanol was selected as the extraction solvent, and a series of parameters that affect the extraction efficiency were systematically investigated. Under the optimized conditions, enrichment factors for PCBs ranged between 494 and 606. Based on a signal-to-noise ratio of 3, the limit of detection for the method ranged between 3.3 and 5.4 ng L−1. Good linearity, reproducibility and recovery were also obtained. 相似文献
994.
Ye-Zhong Zhang Nian-Xia Zhang A-Qiong Ren Jing Zhang Jie Dai Yi Liu 《Journal of solution chemistry》2010,39(4):495-510
The interaction between 2,4-dichlorophenol (DCP) and bovine serum albumin (BSA) was investigated by fluorescence spectroscopy combined with UV-vis absorption and circular dichroism (CD) spectroscopy under simulative physiological conditions. The experiment results show that the fluorescence intensity of BSA is dramatically decreased owing to the formation of a DCP–BSA complex. The corresponding effective quenching constants (K a) between DCP and BSA at four different temperatures (292, 298, 304 and 310 K) were determined to be 10.08×104, 9.082×104, 8.177×104, and 7.260×104 L?mol?1, respectively. The thermodynamics parameters enthalpy change (ΔH) and entropy change (ΔS) were calculated to be ?13.64 kJ?mol?1 and 49.08 J?mol?1?K?1, which suggested that hydrophobic interaction was the predominant intermolecular force. Site marker competitive experiments indicated that the binding of DCP to BSA primarily takes place in subdomain IIA. The binding distance (r) between DCP and the tryptophan residue of BSA ias 4.09 nm according to Förster’s theory of non-radioactive energy transfer. The conformational investigation demonstrated that the presence of DCP decreased the α-helical content of BSA and induced a slight unfolding of the polypeptides of protein, which confirmed the occurrence some micro environmental and conformational changes of BSA molecules. 相似文献
995.
Copper nanoparticles (Cu-NPs) were incorporated into chitosan hydrogel to form a film on the surface of a glassy carbon electrode (GCE) leading to a sensing element for D-arabinitol with excellent oxidative catalytic activity. The electrochemical response to D-arabinitol was studied by cyclic voltammetry and differential pulse voltammetry. Operational parameters affecting the response were examined and optimized, and a simple and sensitive method was established for the determination of D-arabinitol. Response is linear in the concentration range from 10 μmol·L?1 to 10 mmol·L?1, and the limit of detection is 1.0 μmol·L?1. The method may be combined with separation techniques in order to analyze for the ratio of D- and L-arabinitol which is a diagnostic marker for candidiasis. 相似文献
996.
Wong SY Moskowitz JS Veselinovic J Rosario RA Timachova K Blaisse MR Fuller RC Klibanov AM Hammond PT 《Journal of the American Chemical Society》2010,132(50):17840-17848
Here we present a new bifunctional layer-by-layer (LbL) construct made by combining a permanent microbicidal polyelectrolyte multilayered (PEM) base film with a hydrolytically degradable PEM top film that offers controlled and localized delivery of therapeutics. Two degradable film architectures are presented: (1) bolus release of an antibiotic (gentamicin) to eradicate initial infection at the implant site, or (2) sustained delivery of an anti-inflammatory drug (diclofenac) to cope with inflammation at the site of implantation due to tissue injury. Each degradable film was built on top of a permanent base film that imparts the implantable device surface with microbicidal functionality that prevents the formation of biofilms. Controlled-delivery of gentamicin was demonstrated over hours and that of diclofenac over days. Both drugs retained their efficacy upon release. The permanent microbicidal base film was biocompatible with A549 epithelial cancer cells and MC3T3-E1 osteoprogenitor cells, while also preventing bacteria attachment from turbid media for the entire duration of the two weeks studied. The microbicidal base film retains its functionality after the biodegradable films have completely degraded. The versatility of these PEM films and their ability to prevent biofilm formation make them attractive as coatings for implantable devices. 相似文献
997.
Dispersive liquid–liquid microextraction (DLLME) based on the solidification of floating organic droplets (DLLME-SFO) combined with gas chromatography-electron-capture detection (GC–ECD) has been developed for extraction and analysis of three dinitrobenzenes. The extraction conditions including extraction solvent, disperser solvent, extraction time, salt effect and temperature were investigated and optimized systematically. The limits of detection were 0.019 μg L?1 for 1,4-dinitrobenzene, 0.079 μg L?1 for 1,3-dinitrobenzene and 0.034 μg L?1 for 1,2-dinitrobenzene. Moreover, it offered good repeatability and high recovery. This method was successfully applied to monitor DNBs in different water samples. 相似文献
998.
We describe here an analytical method of HEK293 α1A AR cell membrane chromatography (HEK293 α1A AR/CMC) combined with reverse phase liquid chromatography (RPLC) for recognition, separation and identification of target components from Traditional Chinese Medicines (TCMs) Radix Caulophylli. The HEK 293 α1A cells with high expressing α1A adrenergic receptors were used to prepare the stationary phase in the CMC model. Retention fractions on the α1A AR–CMC model were collected using an automated fraction collection and injection module (FC/I). And each fraction was analyzed by RPLC under optimized conditions. 5-Methylurapidil (5-MU) and tamsulosin hydrochloride were used as standard compounds to investigate the suitability and reliability of the HEK 293 α1A AR–CMC–RPLC method prior to screening target component from Radix Caulophylli total alkaloid. The results indicated that caulophine was the target component acting on the α1A AR. This method could be an efficient way in drug discovery using natural medicinal herbs as a source of novel compounds. 相似文献
999.
Shu-Guang Wang Wei-Dong Zhang Zheng Li Zhong-Qi Ren Hong-Xia Liu 《Applied biochemistry and biotechnology》2010,162(7):2015-2026
The synthesis of butyl oleate was studied in this paper with immobilized lipase. Five types of membrane were used as support
to immobilize Rhizopus arrhizus lipase by following a procedure combining filtration and protein cross-linking. Results showed that hydrophobic polytetrafluoroethene
membrane with nonwoven fabric (HO-PTFE-NF) was the favorite choice in terms of higher protein loading, activity, and specific
activity of immobilized lipase. The factors including solvent polarity, lipase dosage, concentration, and molar ratio of substrate
and temperature were found to have significant influence on conversion. Results showed that hexane (logP = 3.53) was a favorable solvent for the biosynthesis of butyl oleate in our studies. The optimal conditions were experimentally
determined of 50 U immobilized lipase, molar ratio of oleic acid to butanol of 1.0, substrate concentration of 0.12 mol/L,
temperature of 37 °C, and reaction time of 2 h. The conversion was beyond 91% and decreased slightly after 18 cycles. Lipase
immobilization can improve the conversion and the repeated use of immobilized lipase relative to free lipase. 相似文献
1000.
Jing Bai Jean Chrysostome Ndamanisha Lin Liu Li Yang Liping Guo 《Journal of Solid State Electrochemistry》2010,14(12):2251-2256
The potential application of ordered mesoporous carbon (OMC)-modified glassy carbon electrode (OMC/GCE) in electrochemistry
as a novel electrode material was investigated. X-ray diffraction, transmission electron micrographs, and cyclic voltammetry
were used to characterize the structure and electrochemical behaviors of this material. Compared to GC electrode, the peak
currents of potassium ferricyanide (K3[Fe(CN)6]) increase and the peak potential separation (ΔE
p) decreases at the OMC/GC electrode. These phenomena suggest that OMC-modified GC electrode possesses larger electrode area
and faster electron transfer rate, as compared with bare GC electrode. Furthermore, riboflavin was detected using OMC/GC electrode
in aqueous solutions. The results showed that, under an optimum condition (pH 7.0), the OMC/GC electrode exhibited excellent
response performance to riboflavin in the concentration range of 4.0 × 10−7 to 1.0 × 10−6 M with a high sensitivity of 769 μA mM−1. The detection limit was down to around 2 × 10−8 M. With good stability and reproducibility, the present OMC/GC electrode was applied in the determination of vitamin B2 content in vitamin tablets, and satisfactory results were obtained. 相似文献