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91.
Characterization of clarithromycin polymorph was performed by solid-state cross polarization and magic angle spinning (CP/MAS) 13C-NMR spectroscopy. Two polymorphs, form II and form I, of clarithromycins indicated characteristic resonances of C1 carbonyl carbon at 176.2 and 175.2 ppm, respectively. Since each peak of C1 carbon was well separated in the spectrum of the two polymorphs, we performed quantitative analysis of the polymorphic fraction from the peak area of these peaks. The peak area of form I was found to linearly increase with an increase of its content, with a correlation coefficient of above 0.99. Solid-state NMR was found to be a useful technique to determine the characteristics of the polymorphic forms. 相似文献
92.
93.
Synthesis and characterization of 6-O-acyl-2-O-alpha-D-glucopyranosyl-L-ascorbic acids with a branched-acyl chain 总被引:3,自引:0,他引:3
We previously reported the chemical synthesis of a series of novel monoacylated vitamin C derivatives, 6-O-acyl-2-O-alpha-D-glucopyranosyl-L-ascorbic acids (6-Acyl-AA-2G) possessing a straight-acyl chain of varying length from C(4) to C(18), as effective skin antioxidants. In this paper, we describe branched type of 6-Acyl-AA-2G derivatives (6-bAcyl-AA-2G) synthesized by use of a 2-branched-chain fatty acid anhydride as an acyl donor. The stability of 6-bAcyl-AA-2G in neutral solution was much higher than that of 6-Acyl-AA-2G, while they were susceptible to enzymatic hydrolysis for exerting vitamin C effect. These branched derivatives as well as 6-Acyl-AA-2G increased the radical scavenging activity against 1, 1-diphenyl-2-picrylhydrazyl and the lipophilicity in octanol/water-partitioning systems with increasing length of their acyl group. In addition, the 6-bAcyl-AA-2G derivative with an acyl chain of C(12), 6-bDode-AA-2G had the excellent solubility to various solvents, suggesting easy handling in cosmetic use. These characteristics of 6-bAcyl-AA-2G may be available for skin care application as an effective antioxidant. 相似文献
94.
Keishi Nishio Yuichi Watanabe Toshio Tsuchiya 《Journal of Sol-Gel Science and Technology》2003,26(1-3):245-250
In this study, we prepared Sr
x
Ba1 – x
Nb2O6 (x = 0.3, 0.5 and 0.7) thin film on 0.75 wt% La doped SrTiO3 (100) and (110) single crystal substrates. A homogeneous coating solution was prepared with Sr and Ba acetates and Nb(OEt)5 as raw materials, and acetic acid and diethlene glycol monomethyl ether as solvents. The substrates were coated with the solution by spin coating method. As-coated thin films were heated from 973 to 1273 K in air. The grains of the thin film on La doped SrTiO3 (100) were pillar shaped and arranged in right angle to each other. On the other hand, the grains of these thin films on La doped SrTiO3 were pillar shape and arranged in one direction. The crystallographic relationship of the thin film between Sr
x
Ba1 – x
Nb2O6 and substrate that the 130 and 310 direction of the thin film on the substrate were oriented with c-axis in parallel to the substrate surface. On the other hand, (hk0) phase diffractions of Sr
x
Ba1 – x
Nb2O6 thin film on the substrate (110) were investigated in the XRD theta-2theta measurement. It is expected that the Sr
x
Ba1 – x
Nb2O6 (x = 0.3, 0.5 and 0.7) were highly oriented or epitaxial growing on La doped SrTiO3 (110) single crystal substrate. 相似文献
95.
Itoh S Kawasaki N Hashii N Harazono A Matsuishi Y Hayakawa T Kawanishi T 《Journal of chromatography. A》2006,1103(2):296-306
We have previously described the site-specific glycosylation analysis of rat brain Thy-1 by LC/multistage tandem mass spectrometry (MS(n)) using proteinase-digested Thy-1. In the present study, detailed structures of oligosaccharides released from Thy-1 were elucidated by mass spectrometric oligosaccharide profiling using LC/MS with a graphitized carbon column (GCC-LC/MS). First, using model oligosaccharides, we improved the oligosaccharide profiling by ion trap mass spectrometry (IT-MS) coupled with Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS). Sequential scanning of a full MS(1) scan with FT-ICR-MS followed by data-dependent MS(n) with IT-MS in positive ion mode, and a subsequent full MS(1) scan with FT-ICR-MS followed by data-dependent MS(n) with IT-MS in negative ion mode enabled the monosaccharide composition analysis as well as profiling and sequencing of both neutral and acidic oligosaccharides in a single analysis. The improved oligosaccharide profiling was applied to elucidation of N-linked oligosaccharides from Thy-1 isolated by sodium dodecyl sulfate-polyacrylamide gel electrophoresis. It was demonstrated that Thy-1 possesses a significant variety of N-linked oligosaccharides, including Lewis a/x, Lewis b/y, and disialylated structure as a partial structure. Our method could be applicable to analysis of a small abundance of glycoproteins, and could become a powerful tool for glycoproteomics. 相似文献
96.
A novel flow-injection system is proposed for the rapid measurement of the fish freshness indices K1 and K2: K1=[([HxR+[Hx])×100/([IMP]+[HxR]+[Hx])] and K2=[[Hx]×100/([HxR]+[Hx])], where [IMP], [HxR] and [Hx] are inosine-5′-monophosphate, inosine and hypoxanthine concentrations, respectively. For the estimation of index K1, 5′-nucleotidase immobilized reactor and nucleoside phosphorylase (NP)/xanthine oxidase (XO) coimmobilized reactor were incorporated in series in the flow-injection line made up by a 16-way switching valve with two sample loops. For the estimation of index K2, NP and XO immobilized reactors were also incorporated in the similar flow-line. Two sample portions passed through the flow-line with different residence times so that two peaks were obtained. The first and second peaks obtained in the K1-determining system corresponded to the total of HxR and Hx and the total of Hx, HxR and IMP, respectively. Similarly, the first and second peaks obtained in the K2-determining system corresponded to Hx and the total of Hx and HxR, respectively. Therefore, the indices K1 and K2 can be estimated by where i1 and i2 present the peak current of the first and second peaks, respectively, and f the ratio of the peak currents of the first and second peaks for a Hx standard solution. A sea bream was selected as a model fish and it was stored at 4 °C after death. A good correlation was found between the index K1 and the storage time over a period of 400 h, with a correlation coefficient of 0.992, but no correlation between the index K2 and the storage time. The measurements could be performed at a rate of 22 samples per hour with satisfactory precision (0.6–1.2% R.S.D.), without calibration for each species, accurate weighing of fish meat and any interferences in fish meat. 相似文献
97.
Chiral beta-amino esters are synthesized in one-pot from three components, amines, aldehydes, and ethyl bromoacetate, under the rhodium-catalyzed Reformatsky-type reaction condition, where complete diastereoselection is achieved in the nucleophilic addition step of ethyl bromoacetate to the imines prepared in 相似文献
98.
Synthesis of 3,3′-(1,6-hexanediyl)bis-pyrimidine derivatives and 3,4-dithia[6.6](1.3)pyrimidinophane
Toshio Kinoshita Shirou Odawara Keiko Fukumura Sunao Furukawa 《Journal of heterocyclic chemistry》1985,22(6):1573-1576
Several 3,3′-(1,6-hexanediyl)bis[6-methyl-2,4(1H,3H)-pyrimidinedione] derivatives ( 4a, 4b , and 4c ) were synthesized from 1,6-(hexanediyl)bis[6-methyl-2H-1,3-oxazine-2,4(3H)-dione] (3) . Compound 4c was converted to 6, which reacted with thiourea giving thiuronium salt 7 . 3,3′-(1,6-Hexanediyl)bis [1-(2-mercaptoethyl)-6-methyl-2,4(1H,3H)-pyrimidinedione] (9) was obtained by the hydrolysis of 7 , and then 9 was oxidized to 12,22-dimethyl-3,4-dithia[6.6] (1.3)-1,2,3,4-tetrahydro-2,4-dioxopyrimidinophane (10) . 相似文献
99.
Kinoshita M Murakami E Oda Y Funakubo T Kawakami D Kakehi K Kawasaki N Morimoto K Hayakawa T 《Journal of chromatography. A》2000,890(2):261-271
Frontal affinity chromatography is a method for quantitative analysis of biomolecular interactions. We reinforced it by incorporating various merits of a contemporary liquid chromatography system. As a model study, the interaction between an immobilized Caenorhabditis elegans galectin (LEC-6) and fluorescently labeled oligosaccharides (pyridylaminated sugars) was analyzed. LEC-6 was coupled to N-hydroxysuccinimide-activated Sepharose 4 Fast Flow (100 μm diameter), and packed into a miniature column (e.g., 10×4.0 mm, 0.126 ml). Twelve pyridylaminated oligosaccharides were applied to the column through a 2-ml sample loop, and their elution patterns were monitored by fluorescence. The volume of the elution front (V) determined graphically for each sample was compared with that obtained in the presence of an excess amount of hapten saccharide, lactose (V0); and the dissociation constant, Kd, was calculated according to the literature [K. Kasai, Y. Oda, M. Nishikawa, S. Ishii, J. Chromatogr. 376 (1986) 33]. This system also proved to be useful for an inverse confirmation; that is, application of galectins to an immobilized glycan column (in the present case, asialofetuin was immobilized on Sepharose 4 Fast Flow), and the elution profiles were monitored by fluorescence based on tryptophan. The relative affinity of various galectins for asialofetuin could be easily compared in terms of the extent of retardation. The newly constructed system proved to be extremely versatile. It enabled rapid (analysis time 12 min/cycle) and sensitive (20 nM for pyridylaminated derivatives, and 1 μg/ml for protein) analyses of lectin–carbohydrate interactions. It should become a powerful tool for elucidation of biomolecular interactions, in particular for functional analysis of a large number of proteins that should be the essential issues of post-genome projects. 相似文献
100.
Perovskite-type barium lithium fluoride (BaLiF3) was synthesized by pyrolysis of metal trifluoroacetates. The reaction temperature necessary for producing a single-phase material was found to be 600°C, which was lower than that for a conventional solid-state reaction or a melting method. Eu-doped BaLiF3 was also prepared and characterized to examine the suitability of trifluoroacetates for precursors in synthesizing homogeneous complex metal fluoride materials. It was demonstrated that trivalent Eu3+, which was used as acetate for a starting material, was reduced to divalent Eu2+ in the pyrolysis process of BaLiF3, as indicated by a broad blue emission due to an allowed 4f65d→4f7 transition at 408 nm with a ultraviolet excitation at 254 nm. The concentration quenching of the blue emission occurred at 5 at% of Eu in BaLiF3, indicating that Eu was homogeneously dispersed in the BaLiF3 host lattice. Mechanisms of the formation and reduction process of BaLiF3 were discussed based on pertinent chemical reactions. 相似文献