排序方式: 共有102条查询结果,搜索用时 15 毫秒
41.
Yamashita K Okuyama M Nakagawa R Honma S Satoh F Morimoto R Ito S Takahashi M Numazawa M 《Journal of chromatography. A》2008,1200(2):114-121
A highly sensitive quantification method of aldosterone by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) was investigated in a positive mode using recently developed picolinyl derivatization. Aldosterone was smoothly and quantitatively converted to the ethyl ether-picolinyl derivative by treatment with HCl-ethanol followed by the esterification with picolinic acid in the presence of 2-methyl-6-nitrobenzoic anhydride and 4-dimethylaminopyridine. The positive ion-ESI mass spectrum of the ethyl ether-picolinyl derivative was characterized by an appearance of protonated molecule ([M+H](+)) as a base peak. The ethyl ether-picolinyl derivatization gave a successful result in a separation of aldosterone from corticosterone, dehydrocorticosterone and cortexolone, and also provided an approximately 10-fold higher ESI response in the positive-LC-ESI-MS/MS (selected reaction monitoring; SRM) when compared to that of underivatized molecule (negative mode). The limit of quantification of aldosterone by SRM using ethyl ether-picolinyl derivatization (m/z 494-->m/z 448) was 1 pg/0.2 ml serum with accuracy and precision of 92.6% and 5.6%, respectively. 相似文献
42.
Kuniaki Tatsuta Takahiro Yamaguchi Yusuke Tsuda Yumiko Yamaguchi Nobutaka Hattori Hiroshi Nagai Seijiro Hosokawa 《Tetrahedron letters》2007,48(24):4187-4190
The first total synthesis and structural determination of YCM1008A, a Ca2+ signaling inhibitor, have been achieved. The N-methoxy pyrano-pyridone moiety was synthesized by successive O- and N-conjugate additions with diketoamide 15. The absolute structure was determined to be (2R,3R,4S,8′R)-configuration. 相似文献
43.
Diffusions of Cu(2+) and Fe(3+) in gelatin generate a moving blue band. It is formed by a diffusion of Cu(2+) and a phase separation of gelatin with diffusing Fe(3+). The diffusing Fe(3+) forms Fe(OH)(3) colloids and gathers gelatin molecules from the surroundings. The diffusion of gelatin molecules generates the concentration gradient, resulting in a gel/sol transition in the dilute phase. In the region where the concentration of Fe(3+) is high enough, the gel remains hard, while a sol phase appears under the hard gel. The absorption spectrum of Cu(2+) depends on the concentration ratio of Cu(2+) to gelatin. As a consequence, we can see a blue band in the restricted region between the diffusing front of Cu(2+) and the phase separation front. The movement of the blue band is caused by a coupling of a simple diffusion and the phase separation. 相似文献
44.
A nickel-catalyzed [4+1] cycloaddition of enones with methylenecyclopropanes leading to dihydrofurans was developed. The reaction outcome is attributed to the transformation of methlenecyclopropane, which is incorporated into a five-membered ring as a one-carbon fragment. 相似文献
45.
Cationic iron(III) porphyrin was found to be an efficient catalyst for the highly chemoselective hetero-Diels-Alder-type reaction of aldehydes with 1,3-dienes. The catalyzed process did not require the use of electron-deficient aldehydes such as glyoxylic acid derivatives or activated electron-rich 1,3-dienes such as Danishefsky's diene and Rawal's diene. The high functional group tolerance and robustness of the catalyst were demonstrated. Further, the potential utility of the catalyst was demonstrated by performing the cycloaddition in the presence of water and by carrying out cycloaddition of an unactivated ketone such as cyclohexanone with a diene. 相似文献
46.
Cycloisomerization of 1,6-enynes to five- or six-membered ring systems is successfully carried out in the presence of a cationic manganese(III) catalyst. The use of a structurally rigid tetradentate porphyrin as the equatorial ligand and a weakly coordinating axial ligand is the key to bringing out the catalytic reactivity of manganese for the reaction. The axial ligand of the catalyst has a marked effect on the product and selectively aids the formation of five- or six-membered cyclic products. 相似文献
47.
Seijiro Shioi Akiyoshi Shimamoto Yuki Nakagami Lexin Qin Mototsugu Shimokawa Shinya Oda 《Electrophoresis》2021,42(12-13):1323-1332
Despite being commonplace, polymerase chain reactions (PCRs) still contain many unknown aspects. One example is microsatellite PCR, which is now widely used for various purposes from ecology to cancer medicine. Since this category of repetitive DNA sequences induces polymerase slippage not only in vivo but also in vitro, microsatellite PCR products comprise a complex combination of DNA fragments with various lengths and have, therefore, been empirically interpreted. The primary obstacle for understanding microsatellite PCR was the intrinsic inaccuracy in sizing of DNA fragments in capillary electrophoresis (CE), which, however, has been overcome by elucidating intrinsic sizing errors in each fragment length range. Secondly, the slippage properties of the thermostable polymerases were first clarified in detail using primer extension assays. Furthermore, using the obtained slippage parameters and our original program, we have first reconstructed microsatellite PCR in silico. The entire processes of complex microsatellite PCR have, thus, been more clearly understood. 相似文献
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49.
Secondary alcohols were converted into the corresponding ketones by methyl acrylate and rhodium catalyst efficiently under microwave irradiation. Treatment of primary alcohols with the same condition resulted in the recovery of the starting materials. Primary alcohols were converted into aldehydes by hydrogen transfer reaction using methyl vinyl ketone and ruthenium catalyst under microwave irradiation. 相似文献
50.
[reaction: see text] Decarboxylation of free carboxylic acid was performed by Pd/C catalyst under hydrothermal water (250 degrees C/4 MPa). Under the hydrothermal conditions of deuterium oxide, decarbonylative deuteration was observed to give fully deuterated hydrocarbons from carboxylic acids or aldehydes. 相似文献