全文获取类型
收费全文 | 167873篇 |
免费 | 14142篇 |
国内免费 | 23692篇 |
专业分类
化学 | 133148篇 |
晶体学 | 3199篇 |
力学 | 5822篇 |
综合类 | 1595篇 |
数学 | 25676篇 |
物理学 | 36267篇 |
出版年
2023年 | 2192篇 |
2022年 | 2544篇 |
2021年 | 4505篇 |
2020年 | 5214篇 |
2019年 | 6005篇 |
2018年 | 4597篇 |
2017年 | 5969篇 |
2016年 | 6060篇 |
2015年 | 5799篇 |
2014年 | 7394篇 |
2013年 | 13505篇 |
2012年 | 9952篇 |
2011年 | 10785篇 |
2010年 | 8984篇 |
2009年 | 10872篇 |
2008年 | 11133篇 |
2007年 | 11597篇 |
2006年 | 10210篇 |
2005年 | 8623篇 |
2004年 | 8159篇 |
2003年 | 6881篇 |
2002年 | 5458篇 |
2001年 | 4438篇 |
2000年 | 3894篇 |
1999年 | 3240篇 |
1998年 | 2816篇 |
1997年 | 2628篇 |
1996年 | 2577篇 |
1995年 | 2559篇 |
1994年 | 2298篇 |
1993年 | 1822篇 |
1992年 | 1819篇 |
1991年 | 1304篇 |
1990年 | 1012篇 |
1989年 | 936篇 |
1988年 | 840篇 |
1987年 | 635篇 |
1986年 | 569篇 |
1985年 | 683篇 |
1984年 | 545篇 |
1983年 | 274篇 |
1982年 | 555篇 |
1981年 | 704篇 |
1980年 | 592篇 |
1979年 | 605篇 |
1978年 | 482篇 |
1977年 | 370篇 |
1976年 | 333篇 |
1974年 | 123篇 |
1973年 | 212篇 |
排序方式: 共有10000条查询结果,搜索用时 62 毫秒
991.
Screening anti‐tumor compounds from Ligusticum wallichii using cell membrane chromatography combined with high‐performance liquid chromatography and mass spectrometry 下载免费PDF全文
Tao Zhang Yuanyuan Ding Hongli An Liuxin Feng Sicen Wang 《Journal of separation science》2015,38(18):3247-3253
Tyrosine 367 Cysteine‐fibroblast growth factor receptor 4 cell membrane chromatography combined with high‐performance liquid chromatography and mass spectrometry was developed. Tyrosine 367 Cysteine‐HEK293 cells were used as the cell membrane stationary phase. The specificity and reproducibility of the cell membrane chromatography was evaluated using 1‐tert‐butyl‐3‐{2‐[4‐(diethylamino)butylamino]‐6‐(3,5‐dimethoxyphenyl)pyrido[2,3‐d]pyrimidin‐7‐yl}urea, nimodipine and dexamethasone acetate. Then, anti‐tumor components acting on Tyrosine 367 Cysteine‐fibroblast growth factor receptor 4 were screened and identified from extracts of Ligusticum wallichii. Components from the extract were retained on the cell membrane chromatographic column. The retained fraction was directly eluted into high‐performance liquid chromatography with mass spectrometry system for separation and identification. Finally, Levistolide A was identified as an active component from Ligusticum wallichii extracts. The 3‐(4,5‐dimethylthiazol‐2‐yl)‐2,5‐diphenyl‐tetrazolium bromide‐formazan colorimetric assay revealed that Levistolide A inhibits proliferation of overexpressing the mutated receptor cells with dose‐dependent manner. Phosphorylation of fibroblast growth factor receptor 4 was also decrease under Levistolide A treatment. Flex dock simulation verified that Levistolide A could bind with the tyrosine kinase domain of fibroblast growth factor receptor 4. Therefore, Levistolide A screened by the cell membrane chromatography combined with high‐performance liquid chromatography and mass spectrometry can arrest cell growth. In conclusion, the two‐dimensional high‐performance liquid chromatography method can screen and identify potential anti‐tumor ingredients that specifically act on the tyrosine kinase domain of the mutated fibroblast growth factor receptor 4. 相似文献
992.
Elution profiles of lanthanides with α‐hydroxyisobutyric acid by ion exchange chromatography using fine resin 下载免费PDF全文
Rahul Trikha Bal Krishan Sharma Kanwal Nain Sabharwal Krishan Prabhu 《Journal of separation science》2015,38(21):3810-3814
Experiments were carried out using a strong acid cation exchange resin with a particle size of 75–150 μm, termed as “fine resin” in hydrogen ion form for the elution of individual lanthanides Sm, Eu, Gd, Tb, and Dy that are produced as fission products in the spent nuclear fuel and generated in the effluent during reprocessing of spent nuclear fuel. Batch experiments were carried out to study the effect of concentration of nitric acid on distribution coefficient. The distribution coefficient values for these individual lanthanides were determined in nitric acid medium in the concentration range of 0.01–4.0 N. Uptake of each individual lanthanide by resin was increased with increased nitric acid concentration from 0.01 to 0.5 N and remained similar from 0.5 to 1.0 N and decreased thereafter up to 4.0 N. Column experiments were also carried out using the same resin to study the parameters like pH of the eluent, flow rate, and resin bed height under isocratic elution conditions for eluting lanthanide elements using α‐hydroxyisobutyric acid as eluent. The results of this study have indicated the possibility for the elution of individual lanthanides. 相似文献
993.
Enrichment of adenosine using thermally responsive chromatographic materials under friendly pH conditions 下载免费PDF全文
Yanli Liang Fangfang Geng Rongji Dai Yulin Deng 《Journal of separation science》2015,38(23):4036-4042
A thermally responsive boronate affinity chromatographic material, which showed thermal sensitivity, had been successfully applied for the enrichment and separation of cis‐diol‐containing compounds, and the capture and release process could be facilitated by adjusting the temperature. However, in this system, the pH of the mobile phase must be higher than 9.8, and alkaline media can lead to the degradation of labile compounds; the use of silica beads also limits its use. In this study, thermally responsive boronate affinity chromatographic material, namely poly(N‐isopropylacrylamide‐co‐N‐acryloyl‐3‐aminophenylboronic acid) grafted silica, was successfully prepared by atom transfer radical polymerization. Its structure was confirmed by IR spectroscopy and the graft ratio was 20.8%, determined by thermogravimetric analysis. Furthermore, the capture/release of adenosine, a cis‐diol, was performed from pH 5.0–9.0 and 10–50°C. The elution of adenosine was remarkably retarded at decreased temperatures and adenosine could be captured completely at 10°C at pH values of 5.0–9.0. The enrichment of adenosine could be achieved by simply changing the temperature from 10 to 50°C. Therefore, this material not only improved the stability of the silica, but was also suitable for the capture of oxidation‐sensitive biological analytes. Moreover, it could be used for the enrichment of cis‐diol‐containing compounds in LC with MS. 相似文献
994.
Application of chromatography technology in the separation of active alkaloids from Hypecoum leptocarpum and their inhibitory effect on fatty acid synthase 下载免费PDF全文
Qiulong Zhang Guangxiang Luan Tao Ma Na Hu Yourui Suo Xiaoyan Wang Xiaofeng Ma Chenxu Ding 《Journal of separation science》2015,38(23):4063-4070
A method that involved the combination of pH‐zone‐refining counter‐current chromatography and semipreparative reversed‐phase liquid chromatography has been established for the preparative separation of alkaloids from Hypecoum leptocarpum. From 1.2 g of crude sample, 31 mg N‐feruloyltyramine, 27 mg oxohydrastinine, 47 mg hydroprotopine, 25 mg leptopidine, and 18 mg hypecocarpine have been obtained. The structure of the new compound, hypecocarpine, is confirmed based on the analysis of spectroscopic data, including NMR, UV, and IR spectroscopy and positive electrospray ionization mass spectrometry. The known chemical structures were characterized on the basis of 1H and 13C NMR spectroscopy. The purities of the five alkaloids are all over 92.7% as determined by high‐performance liquid chromatography. The alkaloids’ cytotoxicity in breast cancer cells is assessed by using a Cell Counting Kit assay and their inhibitory effect on fatty acid synthase expression is assessed by a Western blot assay. These results suggest that leptopidine could suppress growth and induce cytotoxicity in breast cancer cells and that the cytotoxicity of leptopidine may be related to its inhibitory effect on fatty acid synthase expression. 相似文献
995.
Zhihong Shi Lingna Qiu Dan Zhang Mengyuan Sun Hongyi Zhang 《Journal of separation science》2015,38(16):2865-2872
A novel dispersive liquid–liquid microextraction method based on amine‐functionalized Fe3O4 magnetic nanoparticles was developed for the determination of six phenolic acids in vegetable oils by high‐performance liquid chromatography. Amine‐functionalized Fe3O4 was synthesized by a one‐pot solvothermal reaction between Fe3O4 and 1,6‐hexanediamine and characterized by transmission electron microscopy and Fourier transform infrared spectrophotometry. A trace amount of phosphate buffer solution (extractant) was adsorbed on bare Fe3O4‐NH2 nanoparticles by hydrophilic interaction to form the “magnetic extractant”. Rapid extraction could be achieved while the “magnetic extractant” on amine‐functionalized Fe3O4 nanoparticles was dispersed in the sample solution by vortexing. After extraction, the “magnetic extractant” was collected by application of an external magnet. Some important parameters, such as pH and volume of extraction and desorption solvents, the extraction and desorption time needed were carefully investigated and optimized to achieve the best extraction efficiency. Under the optimal conditions, satisfactory extraction recoveries were obtained for the six phenolic acids in the range of 84.2–106.3%. Relative standard deviations for intra‐ and inter‐day precisions were less than 6.3 and 10.0%, respectively. Finally, the established method was successfully applied for the determination of six phenolic acids in eight kinds of vegetable oils. 相似文献
996.
997.
998.
999.
Supramolecular Polyelectrolyte Complexes of Bone Morphogenetic Protein‐2 with Sulfonated Polyrotaxanes to Induce Enhanced Osteogenic Differentiation 下载免费PDF全文
1000.