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101.
Kanda M Sasamoto T Takeba K Hayashi H Kusano T Matsushima Y Nakajima T Kanai S Takano I 《Journal of AOAC International》2011,94(3):878-885
A new, rapid, and efficient method for determining the fumagillin residues in honey was developed. The samples extracted were analyzed using LC/MS/MS. Chromatographic separation of fumagillin was performed in gradient mode on a C8 column (100 x 2.0 mm, 5 microm) at 40 degrees C. The mobile phase consisted of a mixture of 2 mM ammonium formate-0.01% formic acid solution and methanol; the flow rate was set to 0.2 mL/min. Under these conditions, it was possible to measure fumagillin and its isomers as a single peak. The sample preparation procedure used is based on the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, which is fast (approximately 30 min) and uses less organic solvent. The fumagillin was extracted with acetonitrile containing 0.1% formic acid, then purified using a solid-phase extraction method with an Oasis mixed-mode weak anion-exchange cartridge. The overall recovery of fumagillin ranged from 88.1 to 99.4%; the intra- and interassay CVs were <4.5% and <4.9%, respectively. The LOQ was 0.1 microg/kg. LC/MS/MS coupled with the QuEChERS method showed strong potential as a method for determining fumagillin residues in honey. 相似文献
102.
Miyagawa T Nagai K Yamada A Sugihara Y Fukuda T Fukuda T Uchida R Tomoda H Omura S Nagamitsu T 《Organic letters》2011,13(5):1158-1161
The first total synthesis of citridone A has been achieved through regioselective intramolecular iodocyclization and regio- and stereoselective Pd(0)-catalyzed coupling as key reactions. 相似文献
103.
Futaba DN Yamada T Kobashi K Yumura M Hata K 《Journal of the American Chemical Society》2011,133(15):5716-5719
The layer number is of great importance for nanocarbon materials, such as carbon nanotubes (CNTs) and graphene. While simple optical methods exist to evaluate few-layer graphene, equivalent analysis for CNTs is limited to transmission electron microscopy. We present a simple macroscopic method based on the (002) X-ray diffraction peak to evaluate the average wall number of CNTs in the range from single- to few-walled. The key was the finding that the (002) peak could be decomposed into two basic components: the intertube structure (outer-wall contacts) and the intratube structure (concentric shells). Decomposition of the peaks revealed a linear relationship between the average wall number and the ratio of the intertube and intratube contributions to the (002) peak. Good agreement with CNTs having average wall numbers ranging from 1 to ~5 demonstrated this as a macroscopic method for average wall number analysis. 相似文献
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Chiharu Hidaka Eri Yamagishi Takeo Takizawa 《Journal of Physics and Chemistry of Solids》2005,66(11):2058-2060
The single crystal of CaGa2S4:Eu is expected as a useful laser material with a high quantum efficiency of light emission. However, as far as our knowledge is concerned, the systematic study of the mixed compounds of Ca(1−x)EuxGa2S4 as a function of x has not been reported up to now. Here, we have first constructed the phase diagram of the CaGa2S4 and EuGa2S4 pseudo binary system, and show that it forms the solid solution. Then we have grown single crystals of these compounds. The maximum photoluminescence efficiency is achieved at x=0.25. From the three peak energies observed in the photoluminescence excitation (PLE) and absorption spectra, the 5d excited states are suggested to consist of three levels arising from the multiplets of Eu2+ ions. 相似文献
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Geoffrey B Edwards Kaoru Yamanouchi Kozo Kuchitsu Masaaki Sugie Harutoshi Takeo Chi Matsumura Keiichiro Ogawa Yoshito Takeuchi 《Journal of Molecular Spectroscopy》1985,111(2):301-319
The microwave spectrum of 1-pyrroline has been measured from 8 to 48 GHz. The transitions have been assigned to those of the ground state and the four lowest excited states of the ring-puckering vibration of monomer, which is a five-membered ring molecule with one CN double bond. The trimer, which exists in the liquid phase, has not been detected in the gas phase. The geometrical structure of the monomer has been estimated by an ab initio calculation and the trimer by a molecular mechanics calculation. The former is consistent with the experimental rotational constants. A gas-phase infrared spectrum has also been measured, and the ring-puckering potential has been determined by an analysis of the combination bands of the ring-puckering mode and the ring-stretching modes. The potential is described using a puckering coordinate, z, as V(z) = az2 + bz4, where and ; these values are intermediate of the corresponding values for cyclopentene and 1-pyrazoline. The nuclear quadrupole coupling constants, χaa = ?4.39(10), χbb = 1.04(10), and χcc = 3.35(10) MHz, have been determined by an analysis of well-resolved hyperfine splittings. These constants have been reproduced by an ab initio calculation with a 4-31G(N1) basis set. 相似文献
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