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81.
Performance of the apparatus was evaluated in terms of stationary phase retention, partition efficiency and sample loading capacity. Preliminary studies with short coils revealed high retention of the stationary phase under a proper combination of the head-tail elution and planetary motion. Preparative capability of the apparatus was successfully demonstrated on efficient multigram separations of 2,4-dinitrophenyl amino acids, indole auxins, and bacitracin in a pair of large multilayer coils with a total capacity of 1.5 l. 相似文献
82.
Y Ito 《Journal of chromatography. A》1984,301(2):387-403
Extensive studies have been performed on hydrodynamic distribution of two immiscible solvent phases in helical and spiral columns by means of coil planet centrifugation. Under the Scheme IV [see Fig. 1 in Y. Ito, J. Chromatogr., 301 (1984) 377] planetary motion, the two phases display unilateral distribution in the coil, i.e., one phase travels toward the head and the other phase toward the tail. This hydrodynamic trend is sensitively affected by various factors such as physical properties of the solvent system, helical diameter of the column, revolutional radius, etc. Phase distribution diagrams obtained from a set of conventional two-phase solvent systems under various experimental conditions provide extremely useful information for both basic hydrodynamic studies and practical application in high-speed counter-current chromatography. 相似文献
83.
Fuyuki Ito Nobuaki Tanaka Akio Katsuki Akikazu Kakehi Tsuneo Fujii 《Research on Chemical Intermediates》2004,30(3):331-336
Three types of flavylium salts (FVs, yellow, green and red) have been synthesized and the colors depended on recrystallization conditions. The existence of these color states was confirmed by diffuse reflectance spectra. The spectra were almost the same as the absorption spectra in ethanol solution. The molecular state of FVs in crystals will be the same as that in solutions. The crystal colors of the FVs are controlled by the recrystallization conditions. 相似文献
84.
E Makino N Iwasaki N Yagi T Ohashi H Kato Y Ito H Azuma 《Chemical & pharmaceutical bulletin》1990,38(1):201-207
Various pyrazine derivatives were synthesized and their antiallergic activity was examined. The inhibitory activity on allergic histamine release of the compounds bearing a 5-tetrazolyl group was more potent than that of the corresponding carboxyl derivatives. The introduction of -CONH- or -NHCO- between the pyrazine ring and the 5-tetrazolyl group as a spacer greatly enhanced the activity. N-(1H-Tetrazol-5-yl)-2-pyrazinecarboxamide (I-3) was estimated to exhibit nearly the same potency as disodium cromoglycate (DSCG). The structure-activity relationship among various derivatives modified by introducing some substituents onto the 3-, 5- or 6-position of the pyrazine ring of I-3 was investigated. The activity remained unchanged or was reduced when such substituents as methyl, chloro, methoxy, methylamino and dimethylamino were introduced at the 3- or 5-position. In contrast, 6-substitution with various alkylamino groups more or less increased the activity. Among them, the 6-dimethylamino (I-17c) and 6-(1-pyrrolidinyl) (I-34) derivative were proved to be most potent. The IC50 values (concentration which produces 50% inhibition of the allergic histamine release) of I-17c and I-34 were determined to be 4.7 x 10(-10) and 4.6 x 10(-10) M, respectively. These two compounds produced a potent inhibitory activity on passive cutaneous anaphylaxis (PCA) in rat, not only by the intravenous route (ED50 = 0.0096 mg/kg for both compounds) but also by the oral route (ED50 = 0.19 and 0.18 mg/kg, respectively). On the other hand, when the pyrazine ring of some representative compounds was replaced with a pyridine ring, the inhibitory activity on histamine release was significantly reduced. 相似文献
85.
Abstract —5-Bromouridine (BrUd) photochemically reacted with l -tryptophan (trp) only in aqueous frozen solution giving rise to 2-[1,2,3,4-tetrahydro-1-(β-d -ribofuranosyl)-2,4-dioxo-5-pyrimidinyl]-l -tryptophan ( 1a ). Under similar conditions irradiation of 5-bromouracil (BrU) and trp gave the corresponding coupled product 2. Addition of acetone, potassium carbonate or sodium chloride to the frozen system completely inhibited the photocoupling reaction. These photocoupling reactions are suggested to proceed via mixed aggregate formation between trp and BrUd (or BrU) in frozen aqueous solution. Stacking interactions in these aggregates are characterized by an efficient quenching of trp fluorescence by BrUd. Under the same conditions other amino acids such as phenylalanine, tyrosine, histidine and lysine did not react with BrUd, indicating that the photocoupling of BrUd (or BrU) is specific for trp. 相似文献
86.
Hiroshi Ito Vladimir Marousek Conrad Schuerch 《Journal of polymer science. Part A, Polymer chemistry》1979,17(5):1299-1307
1,6-Anhydro-2,3,4-tri-O-(p-methylbenzyl)-ß-D -galactopyranose (TXGal,M1) has been copolymerized with 1,6-anhydro-2,3,4-tri-O-benzyl-ß-D -mannopyranose (TBMan,M2), the products characterized by NMR, specific rotation, and viscosity, and the reactivity ratios calculated. The reactivity ratios r1 = 0.37 ± 0.15 and r2 = 38 ± 4 indicate that the anhydromannose derivative is about 100 times as reactive as that of anhydrogalactose. A comparison of glucose, mannose, and galactose copolymerizations suggests that the reactivity differences of the three propagating cations are comparatively small and the reactivity differences of the monomers large. This result is consistent with a mechanism proposed earlier. Methyl substitution on the aromatic rings of the p-xylyl groups inhibits the initiation process significantly relative to benzyl, but propagation only slightly. 相似文献
87.
Yoshimoto S Honda Y Murata Y Murata M Komatsu K Ito O Itaya K 《The journal of physical chemistry. B》2005,109(18):8547-8550
Adlayers of ZnOEP were prepared on reconstructed Au(100)-(hex) and unreconstructed Au(100)-(1 x 1) surfaces by immersing into a benzene solution containing ZnOEP molecules, and the adlayer structures were characterized by scanning tunneling microscopy (STM). A hexagonally arranged ZnOEP array was formed on an Au(100)-(hex) surface, whereas a rectangularly arranged ZnOEP array was found on an Au(100)-(1 x 1) surface. The adlayer structure of ZnOEP was dependent upon the underlying Au atomic arrangements. Furthermore, an investigation of the spuramolecular assembly for these modified surfaces was carried out by using an open-cage C(60) derivative (opened C(60)). A supramolecular assembled adlayer with a 1:1 composition of opened C(60)/ZnOEP was formed on Au(100)-(hex), whereas aggregates of opened C(60) were found on the ZnOEP-modified Au(100)-(1 x 1) surface. Electrochemical responses of opened C(60) were significantly influenced by underlying ZnOEP arrays. This finding suggests that precise control of underlying ZnOEP adlayers with the Au atomic structure is important to recognize the opened C(60) on them. 相似文献
88.
S Sakurai K Mitani S Hashimoto K Morikawa S Yasuda E Koshinaka H Kato Y Ito 《Chemical & pharmaceutical bulletin》1992,40(6):1443-1451
To find a novel alpha-blocker with high alpha-blocking selectivity against dopamine D2-receptor affinity, we performed structural modification of the alkylene chains and the substituents on two benzene rings of 2-alkoxy-5-[(phenoxyalkylamino)alkyl]benzenesulfonamide derivatives. The modification of the alkylene chain between the amino moiety in the center of the molecule and the benzene ring (ring A) was found to be the most significant. 5-[2-[[2-(5-Fluoro-2-methoxyphenoxy)ethyl]amino]propyl]-2- methoxybenzenesulfonamide (II-4), which possesses 1-methylethyl as the alkylene chain, exhibited high alpha-blocking selectivity as well as potent alpha-blocking activity. 相似文献
89.
Compact Dry TC qualifies as a rapid method kit for determining aerobic colony counts in foods. The plates are presterilized and contain culture medium and a cold-soluble gelling agent. The medium is rehydrated by inoculating 1 mL diluted sample into the center of the self-diffusible medium and allowing the solution to diffuse by capillary action. The plates can then be incubated and the colonies counted without any additional steps. The Compact Dry TC method was validated with 5 different raw meats. The performance tests were conducted at 35 degrees and 30 degrees C. In all required performance studies, no apparent differences were observed between the Compact Dry TC method and the Standard Pour Plate method (AOAC Official Method 966.23) for the detection level of aerobic microorganisms. For the accuracy claim (n = 60), a correlation factor of r2(35) = 0.9977 (35 degrees C) and r2(30) = 0.9932 (30 degrees C) could be assigned, as stated in the application for "Performance Tested Method." Quality consistency and storage robustness studies, showed no significant variations in plate count results with different production lots or plates of diverse storage age. 相似文献
90.
Separation and purification of isoflavones from a crude soybean extract by high-speed counter-current chromatography 总被引:8,自引:0,他引:8
A set of isoflavones with a broad range of polarity including daidzin, glycitin, genistin, acetyldaidzin, glycitein, acetylgenistin and daidzein was separated from a crude soybean extract by high-speed counter-current chromatography using a two-step operation. Three solvent systems were used: chloroform-methanol-water (4:3:2, v/v); chloroform-methanol-n-butanol-water (4:3:0.5:2, v/v); and methyl tert.-butyl ether-tetrahydrofuran-0.5% aqueous trifluoroacetic acid (2:2:0.15:4, v/v). The first solvent system was used for separating less polar isoflavones and the second for more polar isoflavones by eluting the lower organic phase. Genistin and glycitin, which were only partially resolved in the chloroform system, were separated by the third solvent system. Each isolated component showed 98-99% purity as determined by high-performance liquid chromatography analysis. Their structures were identified by LC-MS. 相似文献