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41.
Mycophenolic acid (MPA) is an immunosuppressant drug which powerfully inhibits lymphocyte proliferation. Since the early 1990s it has been used to prevent rejection in organ transplantation. The requirement of therapeutic drug monitoring shown in previous studies raises the necessity of acquiring accurate and sensitive methods to measure MPA and its major metabolite mycophenolic acid glucuronide (MPAG).The authors developed a sample cleanup-free, rapid, and highly specific method for simultaneous measurement of MPA and MPAG in human plasma and serum using the novel technology of ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry. MPA- and MPAG-determinations were performed during a 2.0-min run time. Multiple calibration curves for the analysis of MPA and MPAG exhibited consistent linearity and reproducibility in the range of 0.05-100 (r > 0.999) mg L−1 and 4-4000 mg L−1 (r > 0.999), respectively. Limits of Detection were 0.014 mg L−1 for MPA and 1.85 mg L−1 for MPAG. Lower Limits of Quantification were 0.05 mg L−1 for MPA and 2.30 mg L−1 for MPAG. Interassay imprecision was <10% for both substances. Mean recovery was 103.6% (range 78.1-129.7%) for MPA and 111.1% (range 73.0-139.6%) for MPAG. Agreement was good for MPA and MPAG between the presented method and a validated HPLC-MS/MS method. The Passing-Bablok regression line for MPA and MPAG was HPLC-MS/MS = 1.14 UPLC-MS/MS—0.14 [mg L−1], r = 0.96, and HPLC-MS/MS = 0.77 UPLC-MS/MS + 0.50 [mg L−1], r = 0.97, respectively. This sample cleanup-free and robust LC-MS/MS assay facilitates the rapid, accurate and simultaneous determination of MPA and MPAG in human body fluids. 相似文献
42.
Muriel De Bock Marie-Alice Meuwis Tran Quang Minh Jean-Paul Chapelle Michel Malaise Marianne Fillet 《Talanta》2010,82(1):245-594
In most diseases, the clinical need for serum/plasma markers has never been so crucial, not only for diagnosis, but also for the selection of the most efficient therapies, as well as exclusion of ineffective or toxic treatment. Due to the high sample complexity, prefractionation is essential for exploring the deep proteome and finding specific markers.In this study, three different sample preparation methods (i.e., highly abundant protein precipitation, restricted access materials (RAM) combined with IMAC chromatography and peptide ligand affinity beads) were investigated in order to select the best fractionation step for further differential proteomic experiments focusing on the LMW proteome (MW inferior to 40,000 Da). Indeed, the aim was not to cover the entire plasma/serum proteome, but to enrich potentially interesting tissue leakage proteins. These three methods were evaluated on their reproducibility, on the SELDI-TOF-MS peptide/protein peaks generated after fractionation and on the information supplied.The studied methods appeared to give complementary information and presented good reproducibility (below 20%). Peptide ligand affinity beads were found to provide efficient depletion of HMW proteins and peak enrichment in protein/peptide profiles. 相似文献
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G. Dajk 《Radiation measurements》1997,28(1-6):133-136
Etching solutions of different compositions were applied at room temperature (22°C) for electrochemical etching. The background developed during electrochemical etching in a CR-39 track detector was investigated. Detectors irradiated with alphas of 5.49 MeV were measured also. It was found that the PEW solutions (potassiumhydroxid, ethylalcohol, water) showed good sensitivity. One of them (PEW20/40 was applied for neutrons from a 252Cf source. The achieved registration sensitivity was about 10−5 spot/n after 3 hours of etching time. 相似文献
44.
钯 铂 卟啉络合物在室温下发射长寿命 (ms)、长波长的光 ,这些特点使其在生物分析方面成为有用的探针。本文综述了该探针在光免疫标记、肿瘤诊断、DNA测定、生物传感器及其它方面的研究进展。引用文献 4 3篇 相似文献
45.
Dr. Eva Alvarez de Eulate Dr. Debbie S. Silvester Prof. Dr. Damien W. M. Arrigan 《Angewandte Chemie (International ed. in English)》2015,54(49):14903-14906
At the water–trihexyl(tetradecyl)phosphonium tris(pentafluoroethyl)trifluorophosphate ([P14,6,6,6][FAP]) ionic liquid interface, the unusual electrochemical transfer behavior of protons (H+) and deuterium ions (D+) was identified. Alkali metal cations (such as Li+, Na+, K+) did not undergo this transfer. H+/D+ transfers were assisted by the hydrophobic counter anion of the ionic liquid, [FAP]?, resulting in the formation of a mixed capacitive layer from the filling of the latent voids within the anisotropic ionic liquid structure. This phenomenon could impact areas such as proton‐coupled electron transfers, fuel cells, and hydrogen storage where ionic liquids are used as aprotic solvents. 相似文献
46.
标题化合物C26H26O5以2,3-萘二甲醛和5-甲基-1,3-环己二酮为原料,在醋酸溶剂中,室温下经搅拌多组分一锅法合成得到.其结构通过单晶X-射线衍射法确定,晶体属单斜晶系,空间群P21,相对分子质量Mr=418.47,晶胞参数a=0.990 04(8) nm,b=1.090 98(9)nm,c=1.042 46(11) nm,V=1.087 53(17) nm3,Z=2,晶胞密度Dc=1.278 g/cm3,吸收系数μ=0.088mm-1,单胞中电子的数目F(000) =444.晶体结构用直接法解出,经全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R1 =0.053 3,wR2=0.129 3.在晶体结构中新形成的吡喃环为半椅式构象,而茚中五元环则为信封式构象. 相似文献
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49.
The electrocatalysis oxidation of guanosine‐5′‐monophosphate (GMP) was investigated on Mg‐Al layered double hydroxide (LDH) functionalized with sodium dodecyl sulfate (SDS) and room temperature ionic liquid (RTIL) modified glass carbon electrode (GCE). The cyclic voltammogram of GMP on the modified electrode (RTIL/ LDH‐SDS/GCE) exhibited a well defined anodic peak at 1.091 V in 0.2 mol·L?1 pH 4.4 acetate buffer solution. The GMP oxidation was enhanced in the presence of anionic surfactant in the ?lms. The results suggest that the surfactant molecules intercalate the LDH layers to preconcentrate GMP molecules and the RTIL showed good ionic conductivity. The experimental parameters were optimized, the kinetic parameters were investigated and the probable oxidation mechanism was proposed. Under the optimized conditions, the oxidation peak current was proportional to GMP concentration in the range from 5.0×10?7 to 1.0×10?4 mol·L?1 with the correlation coefficient of 0.9987 and the detection limit was 1.0×10?7 mol·L?1. The RTIL/LDH‐SDS/GCE showed a good electrochemical response to the oxidation of GMP and would be developed into a new biosensor. 相似文献
50.