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51.
Masayuki Yamada Sugako Aramaki Tomoo Hosoe Masahiko Kurosawa Isao Kijima-Suda Koichi Saito Hiroyuki Nakazawa 《Analytical sciences》2008,24(7):911-914
Fluoxymesterone, an anabolic steroid with the 17alpha-methyl,17beta-hydroxy group, has been developed as an oral formulation for therapeutic purposes. However, it is also used illegally in racehorses to enhance racing performance. In this study, we detected 9alpha-fluoro-17,17-dimethyl-18-norandrostane-4,13-dien-11beta-ol-3-one by gas chromatography/mass spectrometry (GC/MS), which has not been reported as a fluoxymesterone metabolite so far in horse. It was synthesized for use as a reference standard, and characterized on the basis of (1)H NMR and (13)C NMR spectra, as well as GC/MS EI mass spectra of TMS derivatives. It was excreted as the main metabolite in horse urine, and its reference standard could be synthesized easily. Therefore, this metabolite could be a useful target for a doping test of fluoxymesterone in racehorses. 相似文献
52.
53.
Kotaro Nagatani Yunosuke Hoshino Haruka Tezuka Masahisa Nakada 《Tetrahedron letters》2017,58(10):959-962
A synthetic pathway to the C-ring fragment of cotylenin A which emerged from our retrosynthetic analysis of cotylenin A is described. The catalytic asymmetric intramolecular cyclopropanation (CAIMCP) of the α-diazo-β-keto ester bearing 2,4,6-trimethylphenyl group as the ester part has been found to afford the crystalline product with high ee, which allowed to establish the approach to the C-ring fragment which required ten-pot operations. The developed approach would be beneficial to a large scale synthesis of the C-ring fragment for the total synthesis of cotylenin A. 相似文献
54.
Oriented films of cellulose prepared from algal cellulose were hydrothermally treated to convert them into highly crystalline cellulose Iβ. The lateral thermal expansion behavior of the prepared cellulose Iβ films was investigated using X-ray diffraction at temperatures from 20 to 300 °C. Cellulose Iβ was transformed into the high-temperature phase when the temperature was above 230 °C, allowing the lateral thermal expansion coefficient of cellulose Iβ and its high-temperature phase to be measured. For cellulose Iβ, the thermal expansion coefficients (TECs) of the a- and b-axes were αa = 9.8 × 10−5 °C−1 and αb = 1.2 × 10−5 °C−1, respectively. This anisotropic thermal expansion behavior in the lateral direction is ascribed to the crystal structure and to the hydrogen-bonding system of cellulose Iβ. For the high-temperature phase, the anisotropy was more conspicuous, and the TECs of the a- and b-axes were αa = 19.8 × 10−5 °C−1 and αb = −1.6 × 10−5 °C−1, respectively. Synchrotron X-ray fiber diffraction diagrams of the high-temperature phase were also recorded at 250 °C. The cellulose high-temperature phase is composed of a two-chain monoclinic unit cell, a = 0.819 nm, b = 0.818 nm, c (fiber repeat) = 1.037 nm, and γ = 96.4°, with space group = P21. The volume of this cell is 4.6% larger than that of cellulose Iβ at 30 °C. 相似文献
55.
A method in which antibodies are produced by using an immunogen heterogeneously conjugated with two or more kinds of haptens having unlike chemical structures against a same carrier protein was offered as an efficient approach for development of antibody to low molecular compounds. To appreciate the potentiality of the approach, 17β-estradiol (E2) and testosterone were selected as model compounds. The I50 values of antiserum developed were 6 and 8 μg L−1 with the detection limits of 0.02 and 0.15 μg L−1 for E2 and testosterone, respectively. Antiserum owned an interesting characteristic that it was possible to independently analyze E2 and testosterone without mutual interference by making proper use of coating antigens. When using β-estradiol 17-hemisuccuinate (EH) conjugated with bovine serum albumin (BSA) as a coating antigen, the enzyme-linked immunosorbent assay (ELISA) was very selective to E2 and some estrogen analogues. Therefore, if testosterone coexisted in the ELISA for E2 detection, it showed no interference with it. From these findings, it was suggested that the verified method was an efficient and rational approach in development of polyclonal antibody to low molecular compounds. 相似文献
56.
Nakazawa M. Okamoto S. Omiya T. Kasai K. Yoshida M. 《Photonics Technology Letters, IEEE》2010,22(3):185-187
57.
Field profiles, equivalent isotropic radiated power (EIRP), beamwidth, and sidelobe levels of a quasi-optical power-combining grid amplifier structure are obtained using a whole-field electromagnetic analysis of a finite structure. This is efficiently obtained using a mixed spectral- and spatial-domain method-of-moments technique. It is seen that edge effects can have a significant effect on system performance 相似文献
58.
Yusuke Iwasaki Masato Goto Keisuke Mochizuki Emi Terayama Rie Ito Koichi Saito Norihiro Sugino Tsunehisa Makino Hiroyuki Nakazawa 《Biomedical chromatography : BMC》2011,25(4):503-510
A selective and sensitive HILIC‐MS/MS method for the simultaneous quantification of nicotine and its metabolites in human maternal and cord sera was developed and validated. After solid‐phase extraction, LC separation was achieved on a hydrophilic interaction chromatography. The validated method is capable of selective identification as well as accurate and sensitive quantification. Analyte recovery ranged from 86.2 to 107.7% and intra‐ and inter‐day assay precision were less than 15% relative standard deviation. This sensitive HILIC‐MS/MS method can be used to determine nicotine and its metabolic profile in smokers. This validated method is useful for the determination of nicotine and its metabolites in human serum in future studies of the effects of nicotine exposure on neonatal outcome. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
59.
60.
The microstructure of Cu interconnections fabricated by high-pressure annealing was evaluated using a field emission scanning
electron microscope/electron backscatter diffraction pattern (FE-SEM/EBSP) technique, and the results are compared with as-deposited
and normally annealed Cu films. The results show some grains extending from the bulk field to the via regions in the case
of the high-pressure annealed Cu films. The existence of via holes was also observed, in which all grains were (111) oriented.
This indicates that the high-pressure annealing process enables the Cu that in-fills the via holes to develop into favorable
microstructures, i.e., single-crystal and with (111) orientation. 相似文献