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121.
Dianjie Ma Yasuaki Okamoto Takahiro Kumamaru Etsuro Iwamoto 《Analytica chimica acta》1999,390(1-3):201-206
Tungsten-coated non-pyrolytic graphite (NPG), pyrolytic graphite (PG) and pyrolytic L'vov platform graphite (PPG) tubes were prepared, and their analytical performances were compared. The coating process simply involved injecting 100 μl of a sodium tungstate solution (0.01 mol l−1) into each graphite tube, followed by heating according to a temperature programme similar to an atomisation cycle for the determination of gallium. This procedure for coating was repeated at least 12, 25, and 7 times towards NPG, PG, and PPG tubes, respectively. Among these tubes, the tungsten-coated PPG tube showed excellent performance for the determination of gallium. By combined use of a chemical modifier such as aluminium(III) or nickel(II) a detection limit (3σ) of 6 pg and sensitivity (1% absorption) of 3–4 pg were achieved. The practical potential of the proposed technique was demonstrated for the determination of gallium in several samples of alloys and fresh water. 相似文献
122.
Kaname Takagi Tomoji Aotsuka And Hikari Morita Yoshihisa Okamoto 《Journal of heterocyclic chemistry》1986,23(5):1443-1449
Reactions of 4-ethoxycarbonylamino-1H-1,5-benzodiazepine-3-carbonitrile (2) with aliphatic primary amines gave 1-substituted 4-(2-aminoanilino)pyrimidin-2(1H)-one-5-carbonitriles 3. Analogous reactions of 2 with aromatic primary amines afforded 2-(2′-anilino-1′-cyanovinyl)benzimidazoles 5 and 6. Upon treatment with triethylamine, 3 underwent intramolecular cyclization to give 3-substituted 5-aminopyrimidino[4,5-b]-[1,5]benzodiazepin-2(3H,11H)-ones 8 . Heating of 3 with p-toluenesulfonic acid in ethanol gave 2-substituted pyrimidino[1,6-a]benzimidazol-1(2H)one-4-carbonitriles 9 . Reactions of 2 with hydrazines were also described. Mechanistic pathways are proposed to account for the products. 相似文献
123.
High-performance liquid chromatography of coenzyme Q-related compounds and its application to biological materials 总被引:1,自引:0,他引:1
T Okamoto K Fukui M Nakamoto T Kishi T Okishio T Yamagami N Kanamori H Kishi E Hiraoka 《Journal of chromatography. A》1985,342(1):35-46
A convenient and precise method for the separation and determination of coenzyme Q (CoQ)-related compounds (CoQ homologues, plastoquinone-9, ubichromenol-9, etc.) was developed using high-performance liquid chromatography (HPLC). All compounds tested were separated using a reverse-phase column with a suitable mobile phase and detected at a wavelength of 275 nm. CoQ extracts in plasma and erythrocytes were purified by thin-layer chromatography prior to HPLC analysis, but such purification was not necessary when determining CoQ in urine and tissues. Hydroquinone forms of CoQ existing in animal tissues were oxidized to the corresponding quinone forms with potassium hexacyanoferrate(III). This HPLC method was applied satisfactorily to the determination of the contents of CoQ homologues in human and animal samples. CoQ10 was the only homologue detected in human samples, and CoQ8, CoQ9 and CoQ10 were native homologues of CoQ in rat tissues. Ubichromenol-9 and plastoquinone-9 were not detected in these samples. 相似文献
124.
Yoshihisa Kurasawa Yoshihisa Okamoto Atsushi Takada 《Journal of heterocyclic chemistry》1985,22(3):935-936
Novel compounds 8-(quinoxalin-2-yl)-1,2,4-triazolo[3,4-f][1,2,4]triazines 3a,b were obtained by a new annulation method in the 1,2,4-triazine synthesis. 相似文献
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128.
A carbon-paste chemically modified with glucose oxidase and a ferrocene-containing siloxane polymer was further modified by coating the electrode surface with a poly(ester-sulfonic acid) cation-exchanger, Eastman AQ-29D. The polymer is obtained as a homogeneous aqueous dispersion at pH 5–6; when dried, the polymer coating is not water-soluble. The coating was shown not to be detrimental to the enzyme activity but to prevent electrochemically active anionic interferents such as ascorbate and urate from reaching the electrode surface. The polymer coating also prevented glucose oxidase from leaking out of the carbon paste into the contacting solution and protected the electrode surface from fouling agents present in urine and bovine serum albumin. Uncoated electrodes lost some 10-2-15% of their original response to glucose after storage in buffer for three weeks whereas the response of the coated electrodes remained constant. Calibration curves for glucose were strictly linear up to about 5 mM for uncoated and up to 20 mM for coated electrodes. The response current to glucose was not decreased after coating. 相似文献
129.
A microanalytical method for the determination of traces of natural brassinosteroids as their dansylaminophenylboronates by liquid chromatography with fluorimetric detection is described. The boronates are easily prepared by the reaction of brassinosteroids with dansylaminophenylboronic acid (DABA), which was newly synthesized as a precolumn fluorogenic reagent for brassinosteroids. The potential of the method is demonstrated by the separation of a standard brassinosteroid mixture and the analysis of a biologically active fraction sample obtained from an extract of Zea mays L. pollen. The detection limit of the DABA derivative was found to be 25 pg for brassinolide, which is superior to that of the phenanthreneboronate derivative. 相似文献
130.
Upon UV irradiation in methanol, triphenyl phosphate ( 1a ) gave biphenylyl phenyl phosphate ( 2a ) as the main product, whereas the addition of water to the solution caused an increase of the yield of biphenyl ( 3a ). These products were formed through a singlet excited state and an intramolecular excimer, respectively. © 1996 John Wiley & Sons, Inc. 相似文献