全文获取类型
收费全文 | 2487篇 |
免费 | 329篇 |
国内免费 | 135篇 |
专业分类
化学 | 949篇 |
晶体学 | 90篇 |
力学 | 618篇 |
综合类 | 38篇 |
数学 | 460篇 |
物理学 | 796篇 |
出版年
2024年 | 7篇 |
2023年 | 23篇 |
2022年 | 52篇 |
2021年 | 39篇 |
2020年 | 70篇 |
2019年 | 53篇 |
2018年 | 44篇 |
2017年 | 71篇 |
2016年 | 97篇 |
2015年 | 81篇 |
2014年 | 125篇 |
2013年 | 164篇 |
2012年 | 130篇 |
2011年 | 138篇 |
2010年 | 127篇 |
2009年 | 145篇 |
2008年 | 145篇 |
2007年 | 140篇 |
2006年 | 140篇 |
2005年 | 164篇 |
2004年 | 134篇 |
2003年 | 129篇 |
2002年 | 104篇 |
2001年 | 88篇 |
2000年 | 84篇 |
1999年 | 59篇 |
1998年 | 74篇 |
1997年 | 58篇 |
1996年 | 46篇 |
1995年 | 45篇 |
1994年 | 31篇 |
1993年 | 22篇 |
1992年 | 16篇 |
1991年 | 23篇 |
1990年 | 15篇 |
1989年 | 8篇 |
1988年 | 14篇 |
1987年 | 8篇 |
1986年 | 8篇 |
1984年 | 6篇 |
1983年 | 2篇 |
1982年 | 6篇 |
1981年 | 3篇 |
1979年 | 4篇 |
1977年 | 1篇 |
1976年 | 1篇 |
1975年 | 1篇 |
1973年 | 1篇 |
1957年 | 2篇 |
1936年 | 1篇 |
排序方式: 共有2951条查询结果,搜索用时 15 毫秒
61.
62.
Summary A simple and rapid capillary zone electrophoretic method with UV detection has been developed for determination of tosufloxacin
and trovafloxacin. The separation was performed in fused-silica capillaries (57 cm length × 75μm i.d.); the running buffer
was 35mm borate + 35mm phosphate buffer solution, pH 8.6, containing 6% (v/v) acetonitrile. The applied potential was 15 kV, the temperature 30°C, and detection was at 262 nm. Piromidic acid was used
as the internal standard. Response was linearly dependent on concentration in the range 1.0–120.0 μg mL−1 and the detection limit was 0.2 μg mL−1 for both compounds. The analysis was highly reproducible (RSD between 3.41 and 1.25%). The method was applied to the determination of tosufloxacin and trovafloxacin in human and rat urine.
The method was validated by using HPLC as a reference method. Recovery was between 96.8 and 102%. 相似文献
63.
Kremser L Brückner A Heger A Grunert T Buchacher A Josic D Allmaier G Rizzi A 《Electrophoresis》2003,24(24):4282-4290
The isoforms distribution of the glycoprotein antithrombin III (ATIII) derived from human plasma was investigated by means of isoelectric focusing (IEF) in polyacrylamide gels with immobilized pH gradients (IPG) and two-dimensional gel electrophoresis (2-DE) as well as capillary electrophoretic methods. It turned out that the presence of high concentrations of chaotropics (urea, thiourea) and zwitterionic detergents (3-[(3-cholamidepropyl)dimethylammonio]-1-propanesulfonate (CHAPS)) was decisive for attaining good resolution of the protein isoforms. Resolution by IPG-IEF was obtained with excellent reproducibility and pI differences down to 0.01 pH units could be distinguished. ATIII-alpha and ATIII-beta-fractions preseparated by heparin affinity chromatography showed an analogous but shifted spot pattern consisting each of one major and three minor isoforms. The main isoforms of ATIII-alpha and ATIII-beta exhibit pI values of 5.18 and 5.32, respectively, both values determined in the presence of high concentrations of urea. The pI difference of 0.14 pH units correspond to the effect of two sialic acids absent in ATIII-beta. The formation and occurrence of ATIII dimers and trimers turned out to be dependent on the sample preparation. The results obtained by 2-DE were compared with those of capillary zone electrophoresis (CZE) and capillary IEF (CIEF). Quantitative analysis regarding the CZE separated isoforms of plasma derived ATIII yielded a content of about 70% ATIII-alpha main isoform and about 6.6% of ATIII-beta. The pI values of ATIII determined by CIEF with internal calibration were in fair agreement with the pI values of the main isoforms achieved with 2-DE. 相似文献
64.
The model proteins cytochrome c, myoglobin, ovalbumin, and beta-lactoglobulin were investigated with regard to their adsorption properties on capillaries for electrophoresis. The model compounds were selected to cover a wide range of properties. Cytochrome c is a basic protein (isoelectric point (pI): 9.6; M(r): 11.7 kDa), beta-lactoglobulin is rather acidic (pI: 5.4, M(r): 18.4 kDa), myoglobin was chosen as a neutral reference protein (pI: 6.8-7.4, M(r): 17.8 kDa), and ovalbumin (pI: 5.1, M(r): 45.0 kDa) was selected as a relatively larger analyte. First, the pH dependence of adsorption was investigated for the bare fused silica. A clear correlation to the respective pIs was noted. For myoglobin and ovalbumin, none or negligible adsorption was found above the pI, whereas strong adsorption was noted just below this parameter. Cytochrome c and beta-lactoglobulin already showed distinct adsorption above their pIs. However, none of the proteins showed any significant adsorption more than one pH unit above the pIs. For linear polyacrylamide-coated capillaries, a decreased but not a complete lack of adsorption was observed. Here, pH-dependent adsorption was noted as well. Regeneration of the capillaries by rinsing with buffers containing 200 mM SDS was also investigated. This method was completely successful for myoglobin, but that too for only freshly-adsorbed protein. After a storage time of 24 h and due to the aging of the adsorbate, a sufficient regeneration was no longer possible. 相似文献
65.
PengZHANG JiCunREN ZuoJunSHEN 《中国化学快报》2004,15(9):1091-1094
In this paper, we first presented a novel method for quantification of circulating DNA in human serum based on capillary zone electrophoresis with laser-induced fluorescence detection (CZE-LIF). The serum was digested by proteinase to release free DNA, and then CZE-LIF system was used for the quantification of total circulating DNA. This method was successfully used to quantify the circulating DNA levels in sera from healthy individuals and certain cancer patients.We found the significantly elevated circulating DNA levels in certain prostate cancer patients. Our results demonstrated that CZE-LIF system has good linearity, excellent sensitivity (0.5 ng/mL DNA),satisfactory reproducibility (RSDs in one day and between days were both less than 5%) and reliability, and is well suitable to the quantification of the circulating DNA in human serum or plasma. 相似文献
66.
67.
Chiral separation method development is usually very time-consuming due to the diversity in chemical structures of pharmaceutical drug substances as well as the suitable separation conditions and the problem to choose the appropriate chiral selector. This paper shows capillary zone electrophoresis (CZE) which was developed for chiral separation of a basic compound - rivastigmine (RIV) using 30 cm × 50 μm i.d. polyacrylamide (PAA)-coated fused-silica capillary (effective length 20 cm), amine-modified phosphate buffer of pH 2.5 and sulfated-β-CD (S-β-CD) as chiral selector. Other selected native or derivatized cyclodextrins (CDs) were also tested: β-CD (5, 30 mM), carboxymethyl-β-CD (5, 30 mM), dimethyl-β-CD (15 mM), hydroxypropyl-β-CD (5, 30 mM), hydroxypropyl-α-CD (5, 30 mM) and hydroxypropyl-γ-CD (5, 30 mM). Complete enantiomeric separation of RIV was achieved at 20 kV, 18 °C and detection at 200 nm within 8 min with R.S.D. for the absolute migration time reproducibility of less than 2.1%. Rectilinear calibration range was 5.0-500.0 μM of each enantiomer (r = 0.9994-0.9995). The CZE method proposed was used for the control of chiral purity of pharmaceutically active S-RIV and for the analysis of Exelon caps preparation. 相似文献
68.
A scheme for separation and detection of eleven priority phenols using capillary zone electrophoresis (CZE) coupled with amperometric detection is described. With a capillary of I.D. 50 μm and length 62.5 cm at 9 kV and an electrophoretic buffer of 20 mM CHES (pH 10.1), complete separation of the eleven compounds was achieved in less than 17 min. Amperometric detection was carried out using a carbon fiber microelectrode of diameter 9 μm inserted into the end of the detection capillary. Linearity over two orders of magnitude was generally obtained for the eleven priority phenols. With an electrode potential+1.10 V (vs. Ag/AgCl reference), the concentration limits of detection were in the sub-ppm (10?6 M) level. This method was successfully applied to analysis of priority phenols in industrial waste water. 相似文献
69.
合并带流动注射分光光度法研究硫羟乳酸掩蔽性能 总被引:1,自引:1,他引:1
本文运用合并带流动注射分析技术,建立了以Yb^3+XO显色体系为参考体系研究硫羟乳酸掩蔽性能的方法,在pH5.6硫羟乳酸能掩蔽Sn^4+,Bi^3+,Tl^3+,Hg^2+,Cu^2+,Cr^3+和Cd^2+测定Yb^3+的线性范围为1.36×10^-6~2.72×10^-5mol/L,采样频率可达120次/h。 相似文献
70.