首页 | 本学科首页   官方微博 | 高级检索  
文章检索
  按 检索   检索词:      
出版年份:   被引次数:   他引次数: 提示:输入*表示无穷大
  收费全文   38856篇
  免费   2459篇
  国内免费   2911篇
化学   36124篇
晶体学   438篇
力学   1304篇
综合类   137篇
数学   477篇
物理学   5746篇
  2024年   56篇
  2023年   385篇
  2022年   896篇
  2021年   741篇
  2020年   1100篇
  2019年   1081篇
  2018年   1095篇
  2017年   1451篇
  2016年   1779篇
  2015年   1494篇
  2014年   1490篇
  2013年   3266篇
  2012年   2474篇
  2011年   2192篇
  2010年   1892篇
  2009年   2349篇
  2008年   2089篇
  2007年   2360篇
  2006年   2000篇
  2005年   1772篇
  2004年   1579篇
  2003年   1366篇
  2002年   1106篇
  2001年   868篇
  2000年   859篇
  1999年   787篇
  1998年   713篇
  1997年   608篇
  1996年   615篇
  1995年   594篇
  1994年   488篇
  1993年   405篇
  1992年   347篇
  1991年   350篇
  1990年   254篇
  1989年   221篇
  1988年   221篇
  1987年   216篇
  1986年   136篇
  1985年   114篇
  1984年   119篇
  1983年   41篇
  1982年   83篇
  1981年   45篇
  1980年   32篇
  1979年   29篇
  1978年   18篇
  1976年   11篇
  1974年   5篇
  1973年   11篇
排序方式: 共有10000条查询结果,搜索用时 15 毫秒
991.
Ethnopharmacological relevanceMetabolic syndrome is closely related to the intestinal microbiota and disturbances in the host metabolome. Hyperuricemia (HUA), a manifestation of metabolic syndrome, can induce various cardiovascular diseases and gout, seriously affecting a patient’s quality of life. Astragalus membranaceus has a long history as a commonly used traditional Chinese medicine to treat kidney disease in China and East Asia.Materials and methodsWe compared the therapeutic effect of benzbromarone and two different doses Astragalus membranaceus ultrafine powder (AMUP) in rats with HUA. Ultra-performance liquid chromatography-mass spectrometer was used to analyze the AMUP metabolism in the plasma, urine, and feces. Further, 16S ribosome RNA sequencing and feces metabolomic were performed to capture the variation of the gut microbiota and metabolites changes before and after drug administration.ResultsAMUP had a notable impact on reducing blood uric acid levels while protecting the liver and kidney. Drug metabolism analysis demonstrated that effective constituent flavonoids are distributed in the blood, whereas saponins remain in the intestine. Gut microbiota analysis showed that low-dose AMUP ameliorated HUA-induced gut dysbiosis by reducing the abundance of harmful bacteria and increasing that of some beneficial bacteria with anti-inflammatory properties, such as Clostridia, Lachnospiraceae, and Muribaculaceae. In addition, HUA-induced changes in metabolite contents in bile acid and adrenal hormone biosynthesis pathways were restored after treatment with AMUP.ConclusionLow-dose AMUP exerts remarkable therapeutic effects on HUA by regulating the gut microbiome and mediating gut metabolism pathways associated with uric acid excretion.  相似文献   
992.
An automated sequential injection (SI) on-line solvent extraction-back extraction separation/preconcentration procedure is described. Demonstrated for the assay of cadmium by electrothermal atomic absorption spectrometry (ETAAS), the analyte is initially complexed with ammonium pyrrolidinedithiocarbamate (APDC) in citrate buffer and the chelate is extracted into isobutyl methyl ketone (IBMK), which is separated from the aqueous phase by means of a newly designed dual-conical gravitational phase separator. A metered amount of the organic eluate is aspirated and stored in the PTFE holding coil (HC) of the SI-system. Afterwards, it is dispensed and mixed with an aqueous back extractant of dilute nitric acid containing Hg(II) ions as stripping agent, thereby facilitating a rapid metal-exchange reaction with the APDC ligand and transfer of the Cd into the aqueous phase. The aqueous phase is separated in a second dual-conical gravitational phase separator, and 30 μl of it is entrapped and metered in a sample loop (SL) and subsequently introduced via air segmentation into the graphite tube for analyte quantification. The ETAAS determination is performed in parallel with the separation/preconcentration process of the ensuing sample. An enrichment factor of 21.4, a detection limit of 2.7 ng l−1, along with a sampling frequency of 13 h−1 were obtained at a sample flow rate of 6.0 ml min−1. The precision (R.S.D.) at the 0.4 μg l−1 level was 1.8% as compared to 3.2% when quantifying the organic extractant directly. The applicability of the procedure is demonstrated for the determination of trace levels of cadmium in three certified reference materials.  相似文献   
993.
The direct coupling of a headspace sampler with a mass spectrometer is proposed as a screening tool for the rapid detection of soil pollution by hydrocarbons from petroleum and derivatives. The samples are subjected to the headspace generation process, with no prior treatment, and the volatiles generated are introduced directly into the mass spectrometer, thereby obtaining a fingerprint of the sample analysed. Suitable treatment of the signal by chemometric techniques allows unequivocal characterisation of the different types of sample. The use of fast gas chromatography with a mass spectrometer detector coupled to the headspace sampler allows identification of the major hydrocarbons present in the mineral and organic polluted samples, interpretation of the results obtained, and demonstrates the analytical potential of headspace-mass spectrometry coupling.  相似文献   
994.
Summary Clenbuterol has been determined in urine by solidphase extraction on a C18 cartridge, diazotization of the eluate with nitrite, coupling of the diazonium ion with 1-(naphthyl)ethylenediamine, and separation of the azo dye formed by HPLC with a C18 column and a micellar mobile phase containing 0.1 M sodium dodecyl sulphate, 12%n-butanol and 0.05 M citrate buffer, pH 3. Recoveries higher than 90% were obtained by mixing the samples with a 20% 0.2 M NaOH before extraction. Limits of detection of 51 and 6.7 ng L−1 were obtained with spectrophotometric and thermal lens spectrometric detection, respectively; respective repeatabilities were 3.1% (5 μg mL−1) and 5.6% (0.16 μg mL−1).  相似文献   
995.
Mignardi S  Masi U 《Talanta》1995,42(12):2059-2061
An analytical procedure for dissolving wolframite in order to determine trace elements by atomic absorption is reported. After decomposition of the mineral by alkaline fusion, the cooled flux is dissolved by heating with aqua regia. The finely crystalline precipitate of tungstite, which forms on standing, is filtered and dissolved by heating with aqua regia. Tungstite forms again in the latter solution and the filtration and solubilization are repeated until the solution contains negligible amounts of trace elements. Following this procedure, trace elements in 35 samples of natural wolframite have been dissolved and the solutions obtained have been analyzed by atomic absorption spectrometry for Fe, Mn, Cu, Zn, Pb, Co, Ni and Cd.  相似文献   
996.
997.
A room temperature ionic liquid N‐butylpyridinium hexafluorophosphate (BPPF6) was used as a binder to make an ionic liquid modified carbon paste electrode (IL‐CPE), which showed good characteristics such as simple preparation procedure, fast electrochemical response and good conductivity. The electrochemical oxidation of ascorbic acid (AA) on the new IL‐CPE was carefully studied. The oxidation peak potential of AA on the IL‐CPE appeared at 109 mV (vs. SCE), which was about 338 mV decrease of the overpotential compared to that obtained on the traditional carbon paste electrode (CPE) and the oxidation peak current was increased for about four times. The electrochemical parameters of AA on the IL‐CPE were calculated with the charge transfer coefficient (α) and the electrode reaction rate constant (ks) as 0.87 and 0.800 s?1, respectively. Based on the relationship of the oxidation peak current and the concentration of AA a sensitive analytical method was established with cyclic voltammetry. The linear range for AA determination was in the range from 1.0×10?5 to 3.0×10?3 mol/L with the linear regression equation as Ip (μA)=?2.52–0.064C (μmol/L) (n=13, γ=0.9942) and the detection limit was calculated as 8.0×10?6 mol/L (3σ). The proposed method was free of the interferences of coexisting substances such as dopamine (DA) and amino acids etc., and successfully applied to the vitamin C tablets determination.  相似文献   
998.
Quinoline derivatives were efficiently prepared through acid-catalyzed Friedlander reaction in ionic liquid ([bmim] [BF4]). It is shown that the proposed method is operationally simple and environmentally benign in that the reaction media and the catalyst can be recovered and be reused effectively for at least four times.  相似文献   
999.
The thermal stability of cellulose/N-methylmorpholine-N-oxide (NMMO) solutions were investigated using UV/VIS spectrometry with a temperature programming cuvette and caloric measurements by means of the Systag calorimeter RADEX (mini-autoclave). Both analytical methods allow to characterize the influences of stabilizers and additives. With the temporal course of the optical density, temperature and pressure thermal runaway reactions with gas evolution and accumulation of chromophoric degradation products were recognized. Kinetic model calculations compared with UV/VIS measurements demonstrate the existence of autocatalytic reactions in cellulose/NMMO solutions. Varying the heating rate autocatalysis can be proved by dynamic caloric measurements as well.  相似文献   
1000.
Summary The present research studies the possibility of using the correlation dependence between molecular parameters of unsubstituted polyaromatic hydrocarbons (PAH) and their retention in reversed-phase liquid chromatography to optimize the conditions for the separation and identification of unknown peaks on the chromatograms of multicomponent mixtures. A linear correlation equation, that takes the number and environment of the carbon atom in the PAH molecule into account as well as the differences in the specific interactions of isomeric molecules with polar eluent, has been proposed. The adequacy of the proposed PAH retention model was verified by comparing the calculated retention values with the experimental data. The possibility of identifying unsubstituted PAH according to the number of carbon atoms of various types and according to the values of the molecules lengths (calculated on the basis of the retention of these substances under different eluent compositions) was exemplified by various chromatographic systems (reversed phase-eluent-PAH molecules).  相似文献   
设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号