全文获取类型
收费全文 | 317篇 |
免费 | 25篇 |
国内免费 | 4篇 |
出版年
2023年 | 1篇 |
2021年 | 3篇 |
2020年 | 11篇 |
2019年 | 11篇 |
2018年 | 11篇 |
2017年 | 7篇 |
2016年 | 13篇 |
2015年 | 10篇 |
2014年 | 17篇 |
2013年 | 27篇 |
2012年 | 10篇 |
2011年 | 43篇 |
2010年 | 20篇 |
2009年 | 28篇 |
2008年 | 19篇 |
2007年 | 8篇 |
2006年 | 13篇 |
2005年 | 14篇 |
2004年 | 9篇 |
2003年 | 5篇 |
2002年 | 7篇 |
2001年 | 3篇 |
2000年 | 5篇 |
1999年 | 4篇 |
1998年 | 4篇 |
1997年 | 2篇 |
1995年 | 6篇 |
1994年 | 4篇 |
1993年 | 4篇 |
1991年 | 5篇 |
1990年 | 1篇 |
1989年 | 1篇 |
1988年 | 2篇 |
1987年 | 2篇 |
1986年 | 2篇 |
1985年 | 2篇 |
1984年 | 1篇 |
1982年 | 4篇 |
1981年 | 4篇 |
1979年 | 2篇 |
1973年 | 1篇 |
排序方式: 共有346条查询结果,搜索用时 31 毫秒
1.
《Nucleosides, nucleotides & nucleic acids》2013,32(5-7):427-429
The 3-(D-alditol-1-yl)-4-amino-5-mercapto-1,2,4-triazoles 4 and 5 can be successfully prepared using microwave irradiation. Condensation of 4 and 5 with p-nitrobenzaldehyde afforded Schiff bases 6 and 7, respectively. Reaction 4 and 5 with ethylchloroacetate gave the corresponding alkylated products 10 and 11. Better yields and much less time were the characteristic features of using the microwave heating over the conventional one. The structure of the prepared compounds was confirmed by 1H-NMR, 2D-NMR and mass spectra. 相似文献
2.
Dicoumarol derivatives were synthesized in the InCl3 catalyzed pseudo three-component reactions of 4-hydroxycoumarin with aromatic aldehydes in excellent yields. The reactions were performed in water under microwave irradiation. All synthesized compounds were characterized using NMR, IR, and UV–Vis spectroscopy, as well as with TD-DFT. Obtained dicoumarols were subjected to evaluation of their in vitro lipid peroxidation and soybean lipoxygenase inhibition activities. It was shown that five of ten examined compounds (3e, 3h, 3b, 3d, 3f) possess significant potential of antilipid peroxidation (84–97%), and that compounds 3b, 3e, 3h provided the highest soybean lipoxygenase (LOX-Ib) inhibition (IC50 = 52.5 µM) and 3i somewhat lower activity (IC50 = 55.5 µM). The bioactive conformations of the best LOX-Ib inhibitors were obtained by means of molecular docking and molecular dynamics. It was shown that, within the bioactive conformations interior to LOX-Ib active site, the most active compounds form the pyramidal structure made of two 4-hydroxycoumarin cores and a central phenyl substituent. This form serves as a spatial barrier which prevents LOX-Ib Fe2+/Fe3+ ion activity to generate the coordinative bond with the C13 hydroxyl group of the α-linoleate. It is worth pointing out that the most active compounds 3b, 3e, 3h and 3i can be candidates for further examination of their in vitro and in vivo anti-inflammatory activity and that molecular modeling study results provide possibility to screen bioactive conformations and elucidate the mechanism of dicoumarols anti-LOX activity. 相似文献
3.
Effect of microwave irradiation on the physical properties and morphological structures of cotton cellulose 总被引:1,自引:1,他引:0
Microwave heating has been proved to be more rapid, uniform and efficient, and easily penetrate to particle inside. To investigate the effect of microwave irradiation on the physical property and morphological structure of cotton cellulose, cellulose fabric was treated with microwave irradiation at different conditions. The physical properties of the treated cellulose fabric were investigated. The morphological structures and thermal stabilities of the untreated and treated cellulose were investigated with differential scanning calorimetry (DSC) and X-ray diffraction. The results show that the physical properties of the treated cellulose fabrics were improved and the recoverability had not significant change. The thermal stability of the treated cellulose was changed. The crystallinity and preferred orientation of the treated cotton cellulose increased. 相似文献
4.
Suode Zhang Per I. Arvidsson 《International journal of peptide research and therapeutics》2008,14(3):219-222
A highly efficient and safe methodology for synthesis of various N-protected amino acid ethyl esters have been established in this study. This methodology employs orthoesters as both esterification
reagent and solvent for protected amino acids. The reactions were carried out under microwave irradiation in neutral conditions
for only 2 min, resulting in highly pure crude products in most cases. This strategy works with a variety of N-protecting groups, such as acid labile protecting group: BOC and tBu; base labile protecting group: Fmoc; hydrogenation labile
protecting group: Z and Na/NH3 labile protecting group: Tos, thus providing facile access to numerous valuable building blocks for solid phase synthesis.
Further reduction of the crude protected amino acid ethyl ester by sodium borohydride under mild conditions led to the corresponding
protected β-amino alcohols with excellent yield, as demonstrated by three examples. 相似文献
5.
Chien-Hung Liu Wen-Ming Chen Jo-Shu Chang 《World journal of microbiology & biotechnology》2007,23(5):633-640
Acidic lipase finds its commercial values in medical applications and bioremediation of food wastes. In this work, approaches
for rapid screening of lipase-producing bacteria were developed and the feasibility assessment of the screening methods was
performed. From food waste samples, the proposed screening procedures allowed isolation of sixteen pure bacterial strains
expressing higher lipase activity at acidic pH (pH 6.0) than at alkaline pH (pH 9.0). To enhance the accuracy of lipase activity
determination under acidic conditions, a novel assay procedure was also developed by deactivating lipase activity by microwave
treatment prior to back titration. This additional step could minimize interferences arising from residual lipase activity
during conventional direct back-titration methods in measuring lipase activity at acidic pH. Using the four strategies proposed
in this work, the best acidic-lipase-producing isolate was obtained by strategy C (SSC) and was identified as Aeromonas sp. C14, displaying an optimal lipase activity of 0.7 U/ml at an acidic pH of 6.0. 相似文献
6.
Wei Huang Yong-Mei Xia Hui Gao Yin-Jun Fang Yi Wang Yun Fang 《Journal of Molecular Catalysis .B, Enzymatic》2005,35(4-6):113-116
The enzymatic esterification between n-alcohol homologs and n-caprylic acid catalyzed by lipozyme RM IM (LRI) in microwave field was investigated. Some interesting findings were obtained. The optimum reaction temperature slightly shifted from that in enzymatic esterification by conventional heating. n-Alcohol homologs used in this experiment showed substrate specificity in terms of the odd and even carbon numbers. THF expressed abnormal solvent effect. Whereas in the contrastive enzymatic esterification by conventional heating, the above mentioned substrate specificity and solvent effect were not observed. All the above phenomena could be explained by both thermal and non-thermal effect of microwave on enzyme and substrates. Further investigation revealed that microwave irradiation reduced the apparent activation energy of the enzymatic reaction according to Arrhenius equation, which is considered as one of the causes increasing initial reaction rate. 相似文献
7.
宋扬 《现代生物医学进展》2005,5(4):16-18
目的:探讨应用ZME-Ⅱ型大功率治疗机的微波热靶点效应治疗肿瘤的临床疗效及作用机理。方法:应用微波仪体表照射患者肿瘤部位及转移淋巴结及体腔内加温治疗(用于宫颈癌等,将辐射器探入阴道内,直接接触肿瘤)。输出功率100W,治疗温度42℃-45℃,间隔72小时热疗一次,6次为一疗程,一般热疗2-3疗程。结果:52例患者中,肿瘤消失8例,疗效显著20例,好转19例,无效5例。总有效率90.38%。结论:临床疗效证明,热疗是一种比较理想的辅助手段,为我们进一步开展热化疗的临床实验提供了理论基础和指导。同时为进一步开展热化疗多靶点效应治疗肿瘤提供了广阔的应用前景。 相似文献
8.
Degradation of hyaluronan by ultrasonication in comparison to microwave and conventional heating 总被引:2,自引:0,他引:2
Evenia Dímalov Vladimír Velebný Vlasta Sasinkov Zdenka Hromdkov Anna Ebringerov 《Carbohydrate polymers》2005,61(4):420-426
Hyaluronan (hyaluronic acid, HA) was depolymerised by ultrasonication (US), microwave irradiation (MW) and conventional heating (CH), and the effect of pH and oxidants was investigated. The degradation was followed by viscometry and size exclusion chromatography coupled with low-angle light scattering. The results demonstrated that depolymerisation of HA by US leveled off to a limiting molecular mass, and the degradation was significantly enhanced by acidic and alkaline pH only in the presence of oxidants. In contrast to US, the course of depolymerisation by MW was strongly pH-dependent, and the degradation rate increased with decreasing pH. The expected enhancement of depolymerisation by MW in comparison to CH was marked only at very short heating time at pH <4. The NMR and FTIR spectral analyses indicated that HA in the whole Mw-range studied retained almost the backbone of the parent polysaccharide independently on the degradation method used. At harsh degradation conditions (long-term treatments, particularly at acidic pH or alkaline pH and in presence of oxidants) the depolymerisation was accompanied by destruction of both constituent sugar residues and formation of unsaturated structures detectable by UV-absorption at 230–240 and 260–270 nm. US-assisted oxidative degradation under mild reaction conditions was shown to be the most appropriate procedure to reduce the molecular mass of HA to 100 kDa without significant chemical modification of the polysaccharide. 相似文献
9.
Emily House Anthony Polwart Philippa Darbre Lester Barr George Metaxas Christopher Exley 《Journal of trace elements in medicine and biology》2013,27(4):257-266
The aetiology of breast cancer is multifactorial. While there are known genetic predispositions to the disease it is probable that environmental factors are also involved. Recent research has demonstrated a regionally specific distribution of aluminium in breast tissue mastectomies while other work has suggested mechanisms whereby breast tissue aluminium might contribute towards the aetiology of breast cancer. We have looked to develop microwave digestion combined with a new form of graphite furnace atomic absorption spectrometry as a precise, accurate and reproducible method for the measurement of aluminium in breast tissue biopsies. We have used this method to test the thesis that there is a regional distribution of aluminium across the breast in women with breast cancer. Microwave digestion of whole breast tissue samples resulted in clear homogenous digests perfectly suitable for the determination of aluminium by graphite furnace atomic absorption spectrometry. The instrument detection limit for the method was 0.48 μg/L. Method blanks were used to estimate background levels of contamination of 14.80 μg/L. The mean concentration of aluminium across all tissues was 0.39 μg Al/g tissue dry wt. There were no statistically significant regionally specific differences in the content of aluminium. We have developed a robust method for the precise and accurate measurement of aluminium in human breast tissue. There are very few such data currently available in the scientific literature and they will add substantially to our understanding of any putative role of aluminium in breast cancer. While we did not observe any statistically significant differences in aluminium content across the breast it has to be emphasised that herein we measured whole breast tissue and not defatted tissue where such a distribution was previously noted. We are very confident that the method developed herein could now be used to provide accurate and reproducible data on the aluminium content in defatted tissue and oil from such tissues and thereby contribute towards our knowledge on aluminium and any role in breast cancer. 相似文献
10.
Derek D. Lovingood Jeffrey R. Owens Michael Seeber Konstantin G. Kornev Igor Luzinov 《Journal of visualized experiments : JoVE》2013,(82)
Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan δ solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials'' morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by Stöber''s methods, which have smooth surfaces. 相似文献