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941.
万古霉素和替考拉宁都属于糖肽类的大环抗生素,具有立体的环状结构和多个手性中心,是两种常见的手性识别材料,广泛应用于对映体的色谱手性分离分析。该文以万古霉素和替考拉宁为手性选择剂,哌嗪为单体,4,4'-二苯基甲烷二异氰酸酯(MDI)、1,6-己二异氰酸酯(HDI)和2,4-甲苯二异氰酸酯(TDI)为交联剂,通过界面聚合反应形成网状层包裹硅胶载体的方法制得6种高效液相色谱手性固定相,用于分离外消旋化合物,并与MDI直接交联万古霉素和替考拉宁在硅胶表面所得固定相进行了比较。结果表明,利用"网包法"和直接交联法制备的手性柱与商品万古霉素和替考拉宁柱之间具有互补性,均对不同的外消旋体有不同程度的拆分。 相似文献
942.
反相高效液相色谱检测丹参药材中4种丹参酮的含量 总被引:6,自引:0,他引:6
建立了测定丹参药材中4种丹参酮含量的反相高效液相色谱法,色谱条件:流动相为水(含0.5%三乙胺)-甲醇-四氢呋喃(45/55/5,V/V/V),流速为1mL/min;PDA检测波长254m;4种成分丹参酮Ⅰ、丹参酮ⅡA、隐丹参酮和二氢丹参酮的加样回收率在95.1%-101.2%之间,线性范围为0.08-2μg。该方法准确,稳定,重现性好。根据该色谱条件,测定了不同产地的丹参药材,结果表明:该色谱方法准确检测了生药中4种丹参酮的含量,适合于丹参药材的质量控制。 相似文献
943.
Determination of triclosan in foodstuffs 总被引:1,自引:0,他引:1
Sanches-Silva A Sendón-García R López-Hernández J Paseiro-Losada P 《Journal of separation science》2005,28(1):65-72
A reverse-phase high-performance liquid chromatographic (RP-HPLC) method coupled with an ultraviolet detector was developed to determine triclosan which had migrated into foodstuffs from packaging materials. The method includes extraction with hexane, followed by evaporation to dryness and residue re-dissolution in ACN 90%. Chromatographic separation was performed with a Kromasil 100 C18 column (15 cm x 0.4 cm ID, 5 microm particle size) at 30 degrees C and using ACN and water as mobile phases. Regarding recoveries, good results (higher than 83% and lower than 112%) were obtained for the three representative food matrixes selected (orange juice, chicken breast meat, and Gouda cheese). 相似文献
944.
Summary Using the example of perhydrophenanthrene, perhydroanthracene and cyclopentanodecalin isomers a possibility is shown to use
packed capillary columns containing graphitized thermal carbon black for a complete separation of high-boiling mixtures of
polycyclic saturated hydrocarbon isomers in accordance with the geometric structure of their molecules. 相似文献
945.
946.
I. M. Mutton 《Chromatographia》1998,47(5-6):291-298
Summary Rapid analyses were performed using reversed-phase liquid chromatography with short (20–100 mm) columns swept by fast yet
shallow gradients, and the results compared with those obtained with 150 mm columns and slow gradients. The resolution losses
incurred with shorter columns were minimised by employing elevated flow rates, to ensure that comparable mean retention factors
were experienced by individual analytes during gradients run on different columns. This conserves gradient steepness. High
quality performance was obtained with turn-around times of 5–10 minutes. An overall 5-fold enhancement in the rate of information
generation was obtained. The relevance of instrumental parameters and of column and packing dimensions, upon the potential
for improved performance is discussed. Some implications for the rapidly developing technique of capillary electrochromatography
are briefly indicated. 相似文献
947.
酶联免疫吸附法直接测定血清雌二醇 总被引:20,自引:0,他引:20
本合成了3种不同载体蛋白的雌二醇抗原,研究了载体蛋白免疫原性对雌二醇抗体产生的影响。应用酶联免疫吸附分析法测定了血清中雌二醇,浓度范围为5-160ng/ml(1.8×10^-^8-5.9×10^-^7mol/L).RSD%小于10.%,检测限为1.97ng/ml,相当于98.5pg/孔(按空白平均值的二倍标准偏差计算)。另外,本还建立了一种用考马斯亮蓝G-250测定半抗原与蛋白结合比的方法,提 相似文献
948.
Voltammetric behaviour and determination of moxifloxacin in pharmaceutical products and human plasma
Erk N 《Analytical and bioanalytical chemistry》2004,378(5):1351-1356
The oxidative behaviour of moxifloxacin was studied at a glassy carbon electrode in different buffer systems using cyclic, differential pulse, and Osteryoung square-wave voltammetry. The oxidation process was shown to be irreversible over the entire pH range studied (2.0–10.0) and was diffusion-controlled. The methods were performed in Britton–Robinson buffer and the corresponding calibration graphs were constructed and statistical data were evaluated. When the proposed methods were applied at pH 6.0 linearity was achieved from 4.4×10–7 to 1.0×10–5 mol L–1. Applicability to tablets and human plasma analysis was illustrated. Furthermore, a high-performance liquid chromatographic method with diode-array detection was developed. A calibration graph was established from 4.0×10–6 to 5.0×10–5 mol L–1 moxifloxacin. The described methods were successfully employed with high precision and accuracy for estimation of the total drug content of human plasma and for pharmaceutical dosage forms of moxifloxacin. 相似文献
949.
顶空固相微萃取-气相色谱-质谱法测定废水中痕量挥发性烷基硫化物 总被引:3,自引:0,他引:3
建立了顶空固相微萃取(HS-SPME)和气相色谱/质谱(GC/MS)联用测定人工湿地废水中的痕量挥发性烷基硫化物的方法。针对废水中两种主要的挥发性烷基硫化物(二甲基硫、二甲基二硫),详细研究了萃取纤维头的种类、萃取时间、萃取温度、pH值、离子强度、样品量及解析条件对HS-SPME的影响。载气为高纯氦气,流速为1.0mL/min,色谱柱为DB-5ms毛细管柱(0.25μm,30m×0.32mm),柱温:25℃(5min)■40℃(1min)■60℃(5min);在优化的实验条件下,本法测定二甲基硫及二甲基二硫的线性范围分别为10~10000ng/L和1~10000ng/L;检出限(3σ)分别为1.9ng/L和1.8ng/L;相对标准偏差小于10%;回收率分别为81.0%~94.6%和84.0%~100.9%。用二乙基硫为内标物质,将本法用于人工湿地废水中主要的烷基硫化物二甲基硫和二甲基二硫的测定,获得满意结果。 相似文献
950.