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Plasma lipid analysis by hydrophilic interaction liquid chromatography coupled with electrospray ionization tandem mass spectrometry 下载免费PDF全文
Kazuhiro Sonomura Shinobu Kudoh Taka‐Aki Sato Fumihiko Matsuda 《Journal of separation science》2015,38(12):2033-2037
A novel method for the analysis of endogenous lipids and related compounds was developed employing hydrophilic interaction liquid chromatography with electrospray ionization tandem mass spectrometry. A hydrophilic interaction liquid chromatography with carbamoyl stationary phase achieved clear separation of phosphatidylcholine, lysophosphatidylcholine, sphingomyelin, ceramide, and mono‐hexsosyl ceramide groups with good peak area repeatability (RSD% < 10) and linearity (R2 > 0.99). The established method was applied to human plasma assays and a total of 117 endogenous lipids were successfully detected and reproducibly identified. In addition, we investigated the simultaneous detection of small polar metabolites such as amino and organic acids co‐existing in the same biological samples processed in a single analytical run with lipids. Our results show that hydrophilic interaction liquid chromatography is a useful tool for human plasma lipidome analysis and offers more comprehensive metabolome coverage. 相似文献
135.
Recyclable Ligands for the Non‐Enzymatic Dynamic Kinetic Resolution of Challenging α‐Amino Acids 下载免费PDF全文
Yong Nian Dr. Jiang Wang Dr. Shengbin Zhou Shuni Wang Dr. Hiroki Moriwaki Dr. Aki Kawashima Prof. Dr. Vadim A. Soloshonok Prof. Dr. Hong Liu 《Angewandte Chemie (International ed. in English)》2015,54(44):12918-12922
Structurally simple and inexpensive chiral tridentate ligands were employed for substantially advancing the purely chemical dynamic kinetic resolution (DKR) of unprotected racemic tailor‐made α‐amino acids (TM‐α‐AAs), enabling the first DKR of TM‐α‐AAs bearing tertiary alkyl chains as well as multiple unprotected functional groups. Owing to the operationally convenient conditions, virtually complete stereoselectivity, and full recyclability of the source of chirality, this method should find wide applications for the preparation of TM‐α‐AAs, especially on large scale. 相似文献
136.
Mizukoshi Y Makise Y Shuto T Hu J Tominaga A Shironita S Tanabe S 《Ultrasonics sonochemistry》2007,14(3):387-392
Sonochemically prepared Pt, Au and Pd nanoparticles were successfully immobilized onto TiO2 with the assistance of prolonged sonication. Their photocatalytic activities were evaluated in H2 production from aqueous ethanol solutions. Beside the sonochemical method, the conventional impregnation method was also employed to prepare photocatalysts. The sonochemically prepared catalysts showed higher activities than did the conventional ones. Their photocatalytic activities depended on the work functions and the dimensions of supported noble metal nanoparticles. Smaller Pt nanoparticles effectively restricted recombination of electrons and holes and provided H2 at a higher rate. 相似文献
137.
Condensation reaction of gem-dimethyldipyrrylmethane-5,5′-dicarbinol and 4,4′-dimethyl-3,3′-di-iso-butyl-2,2′-bipyrrole under the catalysis by trifluoroacetic acid gave a hexapyrrolic macrocycle 6 in 15% yield after DDQ oxidation. X-ray crystallography of 6 shows that three parts of highly planar dipyrrylmethene unit are assembled by two sp3 hybridized gem-dimethyl carbon bridges and one direct linking at the pyrrole α-positions, leading to C2 molecular symmetry. The complexation of 6 with (S)-(+)- and (R)-(−)-mandelic acid induced a CD Cotton effect at 461 and 650 nm. 相似文献
138.
A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of toxic element concentrations (arsenic, barium, cobalt, copper, lead, nickel, strontium, vanadium and zinc) in ash samples was developed. All the measurements were performed in robust plasma conditions which were tested by measuring the Mg(II) 280.270 nm/Mg(I) 285.213 nm line intensity ratios. The highest line intensity ratios were observed when a nebulizer gas flow of 0.6 L min−1, auxiliary gas flow of 0.2 L min−1 and plasma power of 1400 W were used for radially viewed plasma. The analysis of SRM 1633b showed that the ultrasound-assisted method developed is highly comparable with the microwave digestion method standardized by the United States Environmental Protection Agency (EPA-3052). The ultrasound-assisted digestion with a digestion solution of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 81%. One exception is arsenic which resulted in recoveries of about 60% only; however, it could be digested with good recovery (>90%) using a digestion solution of 5 mL of water and 5 mL of aqua regia. The major advantage of the ultrasound-assisted digestion over microwave digestion is the high treatment rate (30 samples simultaneously with a sonication time of 18 min). 相似文献
139.
Mellein BR Aki SN Ladewski RL Brennecke JF 《The journal of physical chemistry. B》2007,111(1):131-138
Room-temperature ionic liquids (ILs) have potential for many different applications, including catalysis and synthesis. Organics are often present during IL applications; therefore, a more fundamental understanding of the interactions between IL and organics is necessary. A systematic study of the effects of organic cosolvents, cations, and anions on the solvent strength of IL/organic mixtures will allow for a greater understanding and potential for tuning of ILs for specific purposes. Solvent strength is commonly quantified using spectroscopic probes. We report the solvent strength of IL/organic mixtures using Reichardt's dyes 30 and 33, Kamlet-Taft parameters, and phenol blue. The results show that the polarity of ILs is largely unaffected by the organic cosolvent; that is, the probes are preferentially solvated by the ILs. However, more specific solvation forces, such as hydrogen bonding, can be influenced indirectly by the strength of the anion/cation interaction, giving counterintuitive results. 相似文献
140.
A multiple-site competitive model has been developed to evaluate quantitatively the equilibrium competition of drugs that bind to multiple classes of binding sites on human serum albumin (HSA). The equations, which are based on the multiple-class binding site model, assume that competition exists at individual sites, that the binding parameters for drug or drug competitor pertain to individual sites, and also that the binding parameters for drug or competitor at any given site are independent of drug or competitor bound at other sites. For the drug-competitor pairs, ethacrynic acid (EA) -caproic acid (C6), -lauric acid (C12), and -palmitic acid (C16), the reaction heat of EA binding to HSA was measured in the absence and the presence of fatty acids at the molar ratio of 3:1 with HSA at pH 7.4 and 37°C by isothermal titration microcalorimetry. The calorimetric titration data induced by the presence of fatty acids were directly compaired to the computer simulation curves by the corresponding multiple-site competititve models, which were precedently calculated from binding parameters of EA and fatty acids. In the case of EA-C12 or -C16 competitive binding, EA binding at the first and the second classes of binding sites on HSA were instantaneously inhibited by C12 or C16, resulting that the binding constant of the first class of binding sites of EA were decreased and that the second class of binding sites on HSA entirely disappeared. In the competition between EA and C6, the first class of binding sites of EA was diminished by C6, resulting in the decrease of the binding constants and the number of binding sites in the first class of EA, whereas, the second class of binding sites was unaffected. The multiple-site competitive model assuming site-site competition could be directly comparable to the calorimetric data and be suitable to account for the competitive processes for drugs bound to the multiple-class of binding sites on HSA.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献