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21.
W. Y. Choy S. C. F. Au-Yeung S. Y. Fan W. L. A. K. Chiu C. S. Cockram 《Analytical and bioanalytical chemistry》1998,361(5):500-503
Glucose in 5% D2O/95% H2O solution was successfully determined quantitatively by measurements of the 1H NMR peak height (intensity) of the single peaks at δ(1H) = 5.22 and 4.64 ppm corresponding to the α-D and the β-D-glucose spectrum, respectively. The single peaks were obtained from decoupling of the high field part of the AX spectrum of the α-D- or the β-D-glucose by incorporation of time shared homonuclear decoupling in the WATR-CPMG method (WATR-HDCPMG) without re-attenuation of the water peak. The method was applied to the determination of total glucose in blood plasma from human subjects undergoing oral glucose tolerance test (OGTT) in the teaching hospital. The results compared favorably with those obtained from the standard glucose oxidase method obtained in a hospital pathology laboratory. The accuracy of the results obtained using the WATR-HDCPMG method was within 3.5% of the glucose oxidation method. 相似文献
22.
Aqueous two-phase extraction as an effective tool for isolation of geniposide from gardenia fruit 总被引:5,自引:0,他引:5
Natural products are normally obtained by organic solvent extraction and many subsequent chromatographic separations. Compounds of interest are often isolated with very low yield and limited purity. An aqueous two-phase extraction process combined with a simple ethanol treatment, for removing excess inorganic salt, has been developed for preparation of geniposide from gardenia. The system was comprised of PE62, a random copolymer composed of 20% ethylene oxide and 80% propylene oxide, KH2PO4 and ethanol. To find optimal conditions, the partition behavior of geniposide under an aqueous two-phase system was investigated. Various factors were considered, including the concentration of salt, the concentration of polymer, the sample loading, and the addition of ethanol. The experimental results demonstrated that increasing salt concentration or decreasing PE62 concentration results in enhancement of the geniposide partition in the salt-rich phase. The addition of ethanol and higher sample loading also promoted the partition efficiency of geniposide. Based on this study, an optimized system containing 5% PE62, 7.5% KH2PO4, and 10% ethanol was tested on a large-scale extraction. A 39.0-g aliquot of final product (in powder form) with 77% purity of geniposide can be effectively extracted from 500 g of gardenia fruit. This process is proved to be useful for industrial application of geniposide preparation. 相似文献
23.
In this study, porous glass fiber membranes were coated with monophenyl trimethoxysilane (MPh) and then sulphonated by chlorosulphonic acid to prepare the cation-exchange membranes with sulphonic acid groups. Different MPh-coating times were tested and the properties of the resulting membranes such as contact angle, FTIR spectrum, conductivity, and ion-exchange capacity were measured. It was found that the optimal MPh-coating time was 60 min and the related ion-exchange capacity was 49.5 μequiv./disc. The modified membrane under the optimal MPh-coating condition was adopted for lysozyme isolation. The results were compared with those for the commercial cation-exchange membrane with sulphonic acid groups (ICE 450 unsupported membrane). Although the prepared membrane exhibited less adsorption capacity than ICE 450 unsupported membrane in the batch lysozyme adsorption experiment, it showed lower non-specific binding ratio under higher salt concentration. In the flow process isolating lysozyme from hen egg albumen, the purification effectiveness obtained using the prepared cation-exchange membrane was superior to the ICE 450 unsupported membrane. 相似文献
24.
Huang HS Chiou JF Chiu HF Hwang JM Lin PY Tao CW Yeh PF Jeng WR 《Chemical & pharmaceutical bulletin》2002,50(11):1491-1494
The synthesis of a series of anthraquinone moieties bearing symmetrical sulfur-linked substituents in the 1 and 5 positions is described. These compounds were evaluated for their ability to inhibit the growth of suspended rat glioma C6 cells and human hepatoma G2 cells, respectively. In addition, the redox property of the compounds was determined based on the inhibition of lipid peroxidation in model membranes. Compounds 2a and 2h in this series compared favorably and exhibited the most potent cytotoxicity (0.02, 0.05 microM) against C6 cells in the XTT colorimetric assay. As far as redox properties are concerned, all bis-thio-anthraquinones show potential lipid peroxidation in model membranes very close to that of mitoxantrone (MX), and 2a, 2d, 2e, 2i, 2j, and 2k have more potential than that of MX. The lack of cytotoxicity of compound 2i cannot be related to lipid peroxidation, but the steric and electronic properties of the side-chain substituent maybe impair effective recognition of the cleavable complex. In contrast to MX, 2a and 2h are cytotoxic in rat glioma C6 cells and do not enhance lipid peroxidation in model membranes. 相似文献
25.
Electrogenerated chemiluminescence (ECL) of six new ethyne-based acridine derivatives (1-6) has been studied. The new acridine derivatives were synthesized by cross-coupling of 9-chloroacridine and corresponding donor-substituted phenylethynes under modified Sonogashira conditions. The donor groups were varied in the order of increasing steric hindrance and donor strength at the donor site. The solution phase photophysical properties and ECL of these compounds were studied comparatively in acetonitrile solvent. The UV-Visible spectra of compounds 1-5 exhibit closely the same maxima. Density functional theory (DFT) has been invoked to analyze and understand the unexpected UV-Visible absorption behavior. Compounds with weak electron donors produce excimer ECL irrespective of steric hindrance at the donor site, while the compound with a stronger donor gives rise to ECL that is blue-shifted with respect to its photoluminescence spectrum. All except one of these compounds also exhibit solid state fluorescence which may be useful for solid state devices such as organic light emitting diodes (OLEDs) and as laser dyes. The observed properties are discussed with reference to the structure of the compounds synthesized. 相似文献
26.
A trinuclear heterobimetallic Ru(II)/Pt(II) complex, cis-{Ru(phen)2[CN-Pt(DMSO)Cl2]2} (phen = 1,10-phenanthroline), is able to function as a "switch-on" luminescent chemodosimeter for sulfhydryl-containing amino acids and peptides via specific binding of the amino acids/peptides with the Pt(II) centers and the subsequent cleavage of the Ru(II)-Pt(II) cyano-bridge. 相似文献
27.
S. C. F. Au-Yeung S. Y. Fan J. C. Yu W. L. A. K. Chiu 《Fresenius' Journal of Analytical Chemistry》1998,361(2):210-213
A novel analytical approach is described that combines the preconcentration power of solvent extraction with the resolution
and sensitivity of a 500 MHz 1H NMR spectroscopic detection method for the quantitative determination of metals. Co(II), Cr(VI), Ni(II) and Pb(II) in water
are extracted into chloroform as dithiocarbamate complexes. By decoupling the protons and employing a solvent-induced shift
method, the 1H NMR spectrum containing the dithiocarbamate complexes of Co(II), Cr(VI), Ni(II) and Pb(II) is fully resolved at CDCl3/ C6D6 below 40%/60%. The detection limits for Co(II), Cr(VI), Ni(II) and Pb(II) are estimated to be 0.12, 0.073, 0.11 and 0.27
μg/mL, respectively, in the sample solution.
Received: 31 July 1997 / Revised: 24 October 1997 / Accepted: 31 October 1997 相似文献
28.
Tam Nga Chiu Fletcher Stephen P. Vogels Christopher M. Westcott Stephen A. Decken Andreas 《Transition Metal Chemistry》2003,28(1):103-109
Dioxomolybdenum(VI) complexes derived from ethyl maltol (2-ethyl-3-hydroxy-4-pyrone) and 1-alkyl-2-ethyl-3-hydroxy-4-pyridin-4(1H)-ones have been prepared and characterized using physical methods including 1H- and 13C-n.m.r. spectroscopy, i.r., elemental analysis, and X-ray diffraction for the pyrone and 3-methylpyridine pyridinone derivatives. The octahedral complexes have the general formula cis-MoO2L2 where L = the deprotonated pyrone or pyridinone ligand. 相似文献
29.
A series of lithium europium double tungsto-molybdate phosphors LiEu(WO4)2−x(MoO4)x (x=0, 0.4, 0.8, 1.2, 1.6, 2.0) have been synthesized by solid-state reactions and their crystal structure, optical and luminescent properties were studied. As the molybdate content increases, the intensity of the 5D0→7F2 emission of Eu3+ activated at wavelength of 396 nm was found to increase and reach a maximum when the relative ratio of Mo/W is 2:0. These changes were found to be accompanied with the changes in the spectral feature, which can be attributed to the crystal field splitting of the 5D0→7F2 transition. As the molybdate content increases the emission intensity of the 615 nm peak also increases. The intense red-emission of the tungstomolybdate phosphors under near-UV excitation suggests them to be potential candidate for white light generation by using near-UV LEDs. In this study the effect of chemical compositions and crystal structure on the photoluminescent properties of LiEu(WO4)2−x(MoO4)x is investigated and discussed. 相似文献
30.
Three novel triosmium complexes with unusual coordination characteristics are reported. Treatment of the hydridotriosmium cluster (mu-H)2Os3(CO)10 with CNNPPh3 in CH2Cl2 gave complexes (mu-H)Os3(CO)(10)(mu2-eta2-C(H)NNPPh3) (1) and (mu-H)Os3(CO)10(mu2-eta1-CHPPh3) (2). Complex 1 represents the first example of the existence of a coordinated phosphinazine ligand. An in-situ 1H NMR study showed that the reaction of (mu-H)2Os3(CO)10 with CNNPPh3 produced complex 1 as the initial product in 100% conversion. The latter is not stable in solution and slowly eliminates nitrogen to form an unusual ylide complex 2 in quantitative yield. The thermolysis of 2 in refluxing toluene afforded (mu-H)3Os3(CO)9(mu3-eta1-CCO2CH2Ph) (3) as a colorless compound. Complexes 1-3 were characterized by spectroscopic methods and single-crystal X-ray diffraction analysis. The interesting feature of structure 3 is the presence of a mu3-alkylidyne ligand where the symmetrically triply bridged CCO2CH2Ph fragment lies perpendicular to and above the triosmium triangle. 相似文献