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71.
Takahashi K Kinugasa S Senda M Kimizuka K Fukushima K Matsumoto T Shibata Y Christensen J 《Journal of chromatography. A》2008,1193(1-2):151-155
A corona-charged aerosol detector (CAD) was developed to improve the sensitivity, reproducibility and quantitativeness of detection as compared to evaporative light-scattering detector (ELSD) for liquid chromatography. Our laboratory used the corona CAD as a detector for supercritical fluid chromatography (SFC) and evaluated its performance compared to the ELSD by using a certified reference material of poly(ethylene glycol) (PEG) and a well-defined equimass mixture of uniform PEG oligomers. The corona CAD was able to detect a 10 times more dilute solution of uniform oligomers compared to the ELSD. Although the original data of molecular mass by ELSD was 4.6% smaller than the certified value of PEG 1000, molecular mass distribution obtained by corona CAD was virtually almost the same as the certified value without any calibrations. 相似文献
72.
3-Succinylaconitine was conjugated with bovine serum albumin (BSA) for use as an immunogen for the preparation of a monoclonal antibody (MAb) against aconitine (Aco). Splenocytes from mice immunized with the Aco-BSA conjugate were fused with an aminopterin-sensitive mouse myeloma cell line, P3-X63-Ag8-653, and a hybridoma secreting a MAb against Aco was successfully obtained. The MAb cross-reacted with mesaconitine, hypaconitine and jesaconitine, which are Aco-type alkaloids, but not with any other compounds examined. The full measurement range of an enzyme-linked immunosorbent assay (ELISA) developed using the new MAb extended from 100 ng mL−1 to 1.5 μg mL−1 of Aco. The concentrations of Aco-type alkaloids in various Aconiti radixes assayed using the new ELISA method showed good agreement with previous reports. 相似文献
73.
Determination and purification of sesamin and sesamolin in sesame seed oil unsaponified matter using reversed‐phase liquid chromatography coupled with photodiode array and tandem mass spectrometry and high‐speed countercurrent chromatography 下载免费PDF全文
Miki Takahashi Yuzo Nishizaki Naoki Sugimoto Hiroaki Takeuchi Kazuya Nakagawa Hiroshi Akiyama Kyoko Sato Koichi Inoue 《Journal of separation science》2016,39(20):3898-3905
In Asian countries, sesame seed oil unsaponified matter is used as a natural food additive due to its associated antioxidant effects. We determined and purified the primary lignans sesamin and sesamolin in sesame seed oil unsaponified matter using reversed‐phase liquid chromatography coupled with photodiode array and tandem mass spectrometry and high‐speed countercurrent chromatography. Calibration curves showed good correlation coefficients (r2 > 0.999, range 0.08 and/or 0.15 to 5 μg/mL) with a limit of detection (at 290 nm) of 0.02 μg/mL for sesamin and 0.04 μg/mL for sesamolin. Sesame seed oil unsaponified matter contained 2.82% sesamin and 2.54% sesamolin, respectively. Direct qualitative analysis of sesamin and sesamolin was achieved using quadrupole mass spectrometry with positive‐mode electrospray ionization. Pure (>99%) sesamin and sesamolin standards were obtained using high‐speed countercurrent chromatographic purification (hexane/ethyl acetate/methanol/water; 7:3:7:3). An effective method for determining and purifying sesamin and sesamolin from sesame seed oil unsaponified matter was developed by combining these separation techniques for standardized food additives. 相似文献
74.
75.
Kikkawa Y Koyama E Tsuzuki S Fujiwara K Miyake K Tokuhisa H Kanesato M 《Chemical communications (Cambridge, England)》2007,(13):1343-1345
Scanning tunneling microscopy (STM) observations reveal that bipyridine derivatives which exhibit various two-dimensional structures due to the odd-even chain length effect are converged into a lamellar structure upon metal coordination. 相似文献
76.
Ito A Okamura TA Yamamoto H Ueyama N Yamaguchi M Kuyama H Ando E Tsunasawa S Ake K Masui R Kuramitsu S Nakazawa T Norioka S 《Rapid communications in mass spectrometry : RCM》2007,21(16):2647-2653
Use of a bis(terpyridine)ruthenium(II) derivative as an N-terminal labeling reagent resulted in the simultaneous detection and individual determination of all the N-terminal fragments of the proteins in a mixture without requiring any separation. All of the N-termini of the guanidinated proteins were labeled selectively by the ruthenium complex (-CO-labeling). After chymotryptic digestion, the fragments were analyzed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and post-source decay (PSD). The -CO moiety exclusively enhanced N-terminal fragment ions in mass spectra and enabled easy N-terminal sequencing. In a mixture containing three different proteins (lysozyme, ubiquitin, and insulin), all of the N-terminal fragment ions labeled with the ruthenium complex were found to produce uniformly intense peaks without the detection of the other unlabeled fragments. The N-terminal sequences of these ions were determined individually by PSD analysis. Application to unknown proteins from Thermus thermophilus HB8 with two-dimensional electrophoretic separation resulted in the successful determination of the N-terminal sequence and easy identification of the target protein. 相似文献
77.
Uekusa Y Sugimoto N Sato K Yun YS Kunugi A Yamazaki T Tanamoto K 《Chemical & pharmaceutical bulletin》2007,55(11):1643-1646
A novel crocetin glycosyl ester, neocrocin A (2), was isolated from gardenia yellow. The structure of 2 was elucidated as that of an all-trans-crocetin beta-D-gentiobiosyl beta-D-glucopyranosyl-(1-->6)-D-2-deoxy-glucopyranos-2-yl diester based on chemical and spectral data. The findings provide evidence that the binding system of crocetin glycosides is not limited to the anomeric position. 相似文献
78.
Ito H Miyake M Nishitani E Miyashita K Yoshimura M Yoshida T Takasaki M Konoshima T Kozuka M Hatano T 《Chemical & pharmaceutical bulletin》2007,55(3):492-494
A new complex tannin, cowaniin (1) was isolated from the leaves and stems of Cowania mexicana (Rosaceae), and its structure was characterized as novel C-glucosidic tannin dimer linked through (+)-catechin on the basis of spectral and chemical evidence. The inhibitory effect on activation of the Epstein-Barr virus early antigen was assessed for cowaniin. Six known polyphenols and related compounds, including a nitrile glucoside, purshianin, were also characterized. 相似文献
79.
Formation of fractal porous silica by hydrolysis of TEOS in a bicontinuous microemulsion 总被引:1,自引:0,他引:1
Kyoko Aikawa Katsumi Kaneko Takamitsu Tamura Masako Fujitsu Kazuo Ohbu 《Colloids and surfaces. A, Physicochemical and engineering aspects》1999,150(1-3):95-104
Mesoporous silica particles have been prepared by hydrolysis of TEOS (Si(OC2H5)4) in bicontinuous microemulsions containing polyoxyethylene (POE) dodecylether, isooctane and water. TEOS was dissolved in a continuous water phase and hydrolyzed by the dispersed water at around the phase inversion temperature (60°C). Undulating solid materials with layered mesostructures were produced from middle-phase microemulsions in the three phase region (o/w=0.2–0.7). On the other hand, the solids obtained from the lower aqueous phase in the three phase region were found to have a heterogeneous disordered structure. Measurements of the fractal dimensions were performed in the macropore region using a box-counting method for the outline of the SEM texture. We found that the macropore size distribution in the particles prepared from the middle-phase microemulsion follows the fractal rule with a dimension of 1.7. From the results of nitrogen adsorption/desorption curves on the silica, a steep increase in the adsorption amounts was observed at a relative pressure below 0.2, and adsorption/desorption hysteresis was also observed at a relative pressure between 0.3 and 0.5. These studies suggest that the silica synthesized in the bicontinuous microemulsion mesostructure has a very broad size range from micro to macropores with a fractal distribution. 相似文献
80.
Susumu Kuwabata Hidemasa Tomiyori Shingo Masui Hiroshi Yoneyama 《Macromolecular Symposia》2000,156(1):213-222
Composite of polypyrrole and crystalline V2O5 powder was prepared by chemical oxidation of pyrrole with use of V2O5 powder itself as an oxidizing agent. The V2O5 content was changed from 0 to 94 wt% by changing the amount of V2O5 dispersed in the preparation bath. The pellet electrodes could be prepared by pressing the composite powder alone even if amount of polypyrrole in the composite was only 6 wt%. The resulting pellet electrode exhibited good charge‐discharge performance as a positive electrode of Li rechargeable battery in an electrolyte solution as well as in a quasi‐solid cell fabricated by using a gel electrolyte sheet of poly(methyl methacrylate). 相似文献