全文获取类型
收费全文 | 973篇 |
免费 | 26篇 |
国内免费 | 99篇 |
专业分类
化学 | 997篇 |
晶体学 | 6篇 |
力学 | 1篇 |
综合类 | 8篇 |
物理学 | 86篇 |
出版年
2023年 | 9篇 |
2022年 | 26篇 |
2021年 | 15篇 |
2020年 | 14篇 |
2019年 | 16篇 |
2018年 | 23篇 |
2017年 | 26篇 |
2016年 | 32篇 |
2015年 | 34篇 |
2014年 | 48篇 |
2013年 | 78篇 |
2012年 | 102篇 |
2011年 | 59篇 |
2010年 | 50篇 |
2009年 | 63篇 |
2008年 | 74篇 |
2007年 | 66篇 |
2006年 | 54篇 |
2005年 | 47篇 |
2004年 | 45篇 |
2003年 | 44篇 |
2002年 | 29篇 |
2001年 | 26篇 |
2000年 | 21篇 |
1999年 | 11篇 |
1998年 | 13篇 |
1997年 | 15篇 |
1996年 | 10篇 |
1995年 | 6篇 |
1994年 | 12篇 |
1993年 | 4篇 |
1992年 | 7篇 |
1990年 | 7篇 |
1989年 | 1篇 |
1988年 | 3篇 |
1986年 | 1篇 |
1985年 | 4篇 |
1984年 | 1篇 |
1978年 | 1篇 |
1977年 | 1篇 |
排序方式: 共有1098条查询结果,搜索用时 15 毫秒
81.
82.
Ping Wang Yi-Zeng Liang Ben-Mei Chen Neng Zhou Lun-Zhao Yi Yan Yu Zhi-Biao Yi 《Chromatographia》2007,65(3-4):209-215
A rapid, simple and specific liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) method has been developed
and validated for the simultaneous determination of enalapril and its major active metabolite enalaprilat in human plasma.
Benazepril hydrochloride was used as the internal standard. Plasma was deproteinized with acetone and centrifuged. The supernatant
was transferred and evaporated to dryness and the residue dissolved in mobile phase. Samples were separated on a C18 column
with a mobile phase of methanol–20 mM ammonium acetate (53:47, v/v) containing 0.15% trifluoracetic acid (v/v) with a pH of 3.0. Enalapril, enalaprilat and the internal standard were measured by electrospray positive selective ion
monitoring mode. The method was validated over a linear range of 1.56–400 ng mL−1 and the limits of quantification were 1.56 ng mL−1 for both enalapril and enalaprilat using 0.1 mL plasma. Extraction efficiency was more than 84% and recoveries were in range
of 93.65–101.17%. The intra-day relative standard deviations (RSD) were less than 8.16 and 7.05% and inter-day RSDs were within
8.42 and 5.72% for enalapril and enalaprilat, respectively. The storage stability of QC samples was investigated under various
conditions. The method was successfully applied for the evaluation of the pharmacokinetics and bioequivalence of enalapril
and enalaprilat in 20 healthy volunteers after an oral dose of 20 mg enalapril maleate. 相似文献
83.
In this study, we developed an analytical method for the enantioseparation of ofloxacin, using capillary electrophoresis with fluorescence detection. The optimum background electrolyte was obtained to be 60 mM hydroxylpropyl‐β‐cyclodextrin (HP‐β‐CD) in 50 mM phosphate buffer at pH 2.30. Under these conditions, the (+) and (‐) ofloxacin were completely separated, with the detection limit of 10 nM when the sample was prepared in deionized water. The linear ranges of levofloxacin in deionized water and untreated urine were 10?7 to 5 × 10?3 M with R2 = 0.9989 and 5 × 10?6to 5 × 10?3 M with R2 = 0.9943, respectively. We also applied this method to investigate the purity of a commercial drug. The results revealed that the ratio between (+)‐ofloxacin and (‐)‐ofloxacin (levofloxacin) was 99.9:0.1, and there is about 93 mg levofloxacin per tablet (200 mg). The concentration of levofloxacin in patient's urine was founded to be 7.9 × 10?4M, and the ratio between the two optical isomers was 99.3:0.7. 相似文献
84.
采用自组装以及电聚合的方法,在磷酸盐缓冲液(PBS)中以3,4-乙烯二氧噻吩(EDOT)为功能单体,盐酸阿霉素(DOX)为模板,在金电极表面电聚合制备DOX印迹敏感膜(MIPs),构建了一种选择性检测DOX的分子印迹电化学传感器.采用循环伏安法(CV)及交流阻抗法(EIS)对其性能进行了表征.优化实验条件后,在含0.005 mol/L K3[Fe(CN)_6]及0.1 mol/L KCl的PBS中,应用差分脉冲伏安法(DPV)测试了该传感器的响应性能.实验结果表明,该传感器检测DOX的线性范围为4.0×10~(-7)~1.0×10~(-6)mol/L,相关系数为0.9967,检出限(S/N=3)达6.5×10~(-8)mol/L;采用电化学洗脱法可使传感器再生,对DOX的测定具有良好重现性及稳定性;该传感器对于干扰物长春碱、放线菌素D及5-氟尿嘧啶有微弱的电流响应,显示出良好的选择性.将该传感器用于人体血样中盐酸阿霉素的分析,回收率为96.0%~106.7%,表明其具有潜在的实用价值. 相似文献
85.
DL-lysine hydrochloride crystals were studied by Raman spectroscopy under hydrostatic pressure using a diamond anvil cell from ambient pressure up to 9.8 GPa in the spectral range from 1150 to 40 cm−1. Changes in the Raman spectrum were observed in all spectral regions analyzed. In particular, modifications in the lattice modes indicate that the crystal undergoes a phase transition. The classification of the vibrational modes, the behavior of their band wavenumber as a function of the pressure and the reversibility of the phase transitions are also discussed. 相似文献
86.
高压坩埚-草酸-盐酸羟胺法提取粘土中的游离氧化铁 总被引:2,自引:0,他引:2
为更准确地测定粘土中的游离氧化铁,提出一个提取游离氧化铁的新方法。该方法是:在高压坩埚中用草酸和盐酸羟胺混合液作为提取剂,于130℃的密封条件下提取粘土中的游离氧化铁,浸提时间为0.5h。实验表明;本法较常用的连二亚硫酸钠-柠檬酸钠-重碳酸钠法能更有效地分解粘土中铁的氧化物,使游离氧化铁的浸出更完全。方法的RSD小于2.5%。 相似文献
87.
盐酸羟胺的间接分光光度法测定 总被引:2,自引:1,他引:2
拟定了在铁(Ⅲ)—2-[2-(6-甲基苯并噻唑)偶氮]-5-二乙氨基苯甲酸(6MeBTAEB)络合物和十二烷基硫酸钠存在下盐酸羟胺的间接分光光度测定方法,回收试验表明该法准确可靠,方便快捷。同时测定了盐酸羟胺与Fe(Ⅲ)-6_Me_BTAEB络合物的反应比。 相似文献
88.
J. A. De Schutter F. De Croo G. Van der Weken W. Van den Bossche P. De Moerloose 《Chromatographia》1985,20(3):185-192
Summary A rapid and specific reversed-phase high-performance liquid chromatographic method (RPHPLC) is described for the determination of mebeverine hydrochloride in tablets. Elution was performed on an octyl silane column with a methanol-water mixture (75-25), containing 0.05% hexylamine as silanol-blocking agent, adjusted to pH 5.0 with phosphoric acid. The method gave accurate, precise and reproducible results. The mean recovery of the drug from six synthetic tablet mixtures was 100.0% with a relative standard deviation (RSD) of 0.94%. In order to test the specificity of the method, the interference of the degradation compounds of mebeverine hydrochloride and of the intermediates from the synthesis was investigated. None of them did interfere. By means of mass spectrometry and UV-spectrophotometry, the degradation compounds of mebeverine were identified as veratric acid and as 4-|ethyl-[2-(4-methoxyphenyl)-1-methylethyl]amino| 1-butanol. The stability study proved that mebeverine hydrochloride is very stable in tablets; the tablets still contain more than 95% of the declared drug potency after storage for more than one year at 50°C.Colofac; Duspatal; Duspatalin 相似文献
89.
R. Shanmugam J. Ganesamurthi T.-W. Chen S.-M. Chen M. Balamurugan M.A. Ali A.M. Al-Mohaimeed W.A. Al-onazi K. Alagumalai 《Materials Today Chemistry》2022
Herein, we reported the fabrication of porous iron oxide/carbon black (P–Fe2O3/CB) composite through a two-step engineering method. At first, Prussian blue microcubes were used as a precursor and further calcined to form P–Fe2O3 microcubes. The intercalation of CB nanoparticles with P–Fe2O3 nanocubes was processed through the ultrasonication method. The obtained P–Fe2O3/CB were successfully scrutinized through various physiochemical characterization methods. The proposed P–Fe2O3/CB-modified glassy carbon electrode sensor was successfully implemented in the electrochemical sensing of chlorpromazine hydrochloride due to its very low charge transfer resistance (Rct) compared to the other electrode modifiers. The sensitive detection of CPMH through differential pulse voltammetry exemplifies an excellent electroanalytical performance such as a wide linear range of 0.5–1472 μM, a lower detection limit (0.001 μM), and an appraisable sensitivity of 1.99 μA/μM cm?2 due to its availability of a high number of active sites and its large surface area, respectively. It also expresses excellent selectivity, repeatability, reproducibility, and stability results. Moreover, the practical feasibility of the as-fabricated P–Fe2O3/CB/glassy carbon electrode sensor shows exquisite recovery (98.1–100.8%) results with an appraisable current response in various biological, pharmaceutical, and environmental samples. 相似文献
90.
《Arabian Journal of Chemistry》2022,15(4):103712
Although recent decades have witnessed the synthesis of 1,3,4-thiadiazoles via phosphorus POCl3-promoted cyclization reaction, simultaneous access to 2-amino-1,3,4-thiadiazole and 2-amino-1,3,4-oxadiazole analogs remains unexpected and elusive. Herein, a detailed regiocontrolled synthesis of 2-amino-1,3,4-thiadiazoles in good to high yields with good regioselectivities from readily available thiosemicarbazides using POCl3 was disclosed. Meantime, to establish a comprehensive structure–activity relationship, 2-amino-1,3,4-oxadiazole derivatives as single regioisomers were prepared via EDCI·HCl-triggered cyclization of the thiosemicarbazide intermediates. The in vitro anti-influenza assays proved that the selected compounds with the pyrazine/pyridine ring exhibited certain inhibitory activities against influenza A virus strains A/HK/68 (H3N2) and A/PR/8/34 (H1N1) in MDCK cells. Among them, N-(adamantan-1-yl)-5-(5-(azepan-1-yl)pyrazin-2-yl)-1,3,4-thiadiazol-2-amine (4j) was the most active compound, and exhibited favorable activity with EC50 values of 3.5 μM and 7.5 μM, respectively. In addition, the molecular docking results explained the reason why compound 4j had dual inhibitory activity and revealed the reasonable binding mode of this compound with the M2-S31N and M2-WT ion channels. This compound had the potential to be further developed as an anti-influenza drug. 相似文献