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91.
Simultaneous isolation and determination of esculin and rutin in natural materials using SPE and HPLC 总被引:1,自引:0,他引:1
Summary Esculin (ESC) and rutin (RUT) have been simultaneously isolated from pharmaceutical natural materials by solid phase extraction (SPE). Determination of both substances was performed by reversed phase high performance liquid chromatography (RPHPLC) with UV detection. Optimization of the separation conditions showed that simultaneous isolation and determination of rutin and esculin from pharmaceutical material was possible. The recovery obtained was not lower than 95±2%. 相似文献
92.
The monodisperse, porous poly(chloromethylstyrene-co-divinylbenzene) beads of 7.9 microm were prepared by a single-step swelling and polymerization method. The seed particles prepared by dispersion polymerization exhibited good absorption of the monomer phase. Based on this media, a weak cation-exchange (WCX) stationary phase for HPLC was synthesized by a new chemically modified method. The prepared resin has advantages of biopolymer separation, high column efficiency, low column backpressure, high protein mass recovery, and good resolution for proteins. The dynamic protein-loading capacity of the synthesized WCX packings was 18.2 mg/g. Five proteins were separated in 3.0 min using the synthesized WCX stationary phase. The experimental results show that the obtained WCX resin has very weak hydrophobicity. The WCX resin was also used for the rapid separation and purification of lysozyme from egg white in 5.0 min with only one step. The purity and specific bioactivity of the purified lysozyme were found to be more than 93% and 70 245 U/mg, respectively. 相似文献
93.
细胞色素C的电化学行为研究 总被引:7,自引:0,他引:7
本文评述了细胞色素C电化学研究的发展概况,重点介绍了细胞色素C在促进剂作用下的电化学行为,促进剂种类,影响促进作用的因素及促进机理。 相似文献
94.
Immobilized polysiloxane-anchored permethyl-β-cyclodextrin (Chirasil-Dex) with a cyclodextrin content of approximately 30 % by weight, previously employed as a versatile chiral stationary phase for the separation of enantiomers by GC, has been used for the separation of enantiomers by capillary supercritical fluid chromatography (SFC). A considerable number of racemates could be resolved, e.g. aromatic alcohols, amino alcohols (TFA derivatives), and underivatized acids. Many pharmaceutical compounds were among those analyzed, including several NSAIDs (e.g. ibuprofen and ketoprofen), a steroidal drug (nor-gestrel), a barbiturate (hexobarbital), and others. Among the racemates resolved were many which cannot be analyzed by GC owing to low volatility or decomposition at elevated temperatures. For two racemates, analysis temperature and mobile phase density were systematically varied to give constant analysis times or capacity factors k. Low temperatures (ca 60 °C) yielded the best separation in term of separation factor, α, or resolution, Rs, even though higher densities had to be used. In comparison with GC, capillary SFC was able to furnish higher separation factors and similar resolution. The applicability of capillary SFC for the analysis of mixtures of cyclodextrin derivatives, e.g. those used in the synthesis of Chirasil-Dex, was, furthermore, demonstrated. 相似文献
95.
R. Matissek 《Chromatographia》1989,28(1-2):34-38
Summary Antimicrobially active formulations based on 2-methyl-3(2H)-isothiazolone and 5-chloro-2-methyl-3(2H)-isothiazolone (Kathon CG, Euxyl K 100) are incorporated into manufactured cosmetics as preservatives. In this paper we report on the analysis of these active components by means of liquid chromatography. It is conventional for the original methylisothiazolone components in cosmetics to be analyzed by reversed phase high-performance liquid chromatography after column chromatographic separation and flash chromatographic purification. In our new analytical method the methylisothiazolones are converted into the respective -thiosubstituted acrylamide derivatives, which are ionic substances, with the help of the nucleophilic reagent hydrogensulfite. An ion pair high-performance liquid chromatographic method has been developed for the separation and quantification of these derivatives. 相似文献
96.
97.
98.
离子色谱法同时测定水中六种阳离子 总被引:3,自引:0,他引:3
研究了用抑制电导离子色谱法一次进样同时测定水中Li^ ,Na^ , NH4^ ,Mg^2 ,Ca^2 的色谱法条件,相对标准偏差小于0.5%,加标回收率在97.5%-104.0%。在水质分析中运用t检验法,比较了用钙、镁离子浓度计算和传统方法测定的总硬度之间是否存在显著性差异。 相似文献
99.
M. Piñeiro-Iglesias M. Miñones-Vázquez E. Vázquez-Blanco S. Muniategui-Lorenzo P. López-Mahía D. Prada-Rodríguez 《Chromatographia》2002,56(7-8):483-488
Summary The aim of this work is to establish the best conditions for concentration and purification steps in the trace analysis of
aliphatic and polycyclic aromatic hydrocarbons (PAH) from atmospheric particulate matter by gas chromatography-flame ionisation
detection (GC-FID) and high performance liquid chromatography with ultraviolet and fluorescence detection (HPLC-UV-FL). The
best results for the more volatile compound were obtained with a combination of rotary evaporation and a stream of nitrogen
(near to 100% for aliphatic hydrocarbons and from 70 to 105% for PAH). Two types of solid phase extraction (SPE)cartridges
(Supelclean
tm
LC-Silica SPE tubes and Sep-Pak? Plus silica cartridges) and glass column were examined for the purification and fractionation step. Blank chromatograms of
both types of cartridges analysed by GC-FID made this study difficult, because a PSS (programmed split-splitless) injector
was employed thereby increasing the sensitivity. This problem was not observed in the HPLC-UV-FL blank chromatograms of these
cartridges. Glass columns filled with silica and alumina were chosen because no interference was found in the GC-FID blank
chromatograms and the best recoveries in the fractionation of both aliphatic hydrocarbons and PAH were achieved. This is especially
important when aliphatic hydrocarbons concentrations are lower than 1 μg mL−1. Finally, the selected conditions were applied to the analysis of hydrocarbons in real atmospheric particulate samples. 相似文献
100.
The carbobenzyloxy (cbz) protecting group is evaluated for it's potential to enhance the resolution of chiral amine enantiomers using high-performance liquid chromatography (HPLC) and supercritical fluid chromatography (SFC). A series of cbz derivatives of commercially available racemates was prepared and analyzed by enantioselective chromatography using a variety of mobile phases and polysaccharide and Pirkle-type chiral stationary phases (CSPs). The cbz-derivatized product consistently demonstrated enhanced chiral resolution under HPLC and SFC conditions. Improved selectivity and resolution combined with an automated preparative HPLC or SFC system can lead to the rapid generation of highly purified enantiomers of desirable starting materials, intermediates or final products. 相似文献