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791.
Summary Several -cyclodextrin (CD)-bonded stationary phases for high performance liquid chromatography (HPLC) were prepared, based on silica beads coated with a poly(alkylamine), [poly(ethyleneimine)(PEI)]. In order to obtain stationary phases with a high content of CD and maximum accessibility of the CD cavity, the functionalization was carried out after the coating, using the mono-tosyl derivative of CD as the intermediate. The ability of these supports to separate ortho, meta and para isomers of some disubstituted benzene derivatives was examined. The contribution of the amino groups of the polymer and of the CD cavity to the separation process is discussed. The resolution is mainly based on the difference in the stability of the complexes of the various isomers with CD. The influence of the amount of CD on the height of the theoretical plate is also studied. 相似文献
792.
793.
Effects of metal surfaces, such as aluminium, silver and gold, on the melting behavior and thermal polymerization of long-chain diynoic acids having a diacetylene group at different positions were investigated by thermal analyses using DSC, TG and other methods. The surface effects of metals were significant in the order of Ag, Al and Au. These effects are attributable to the anchoring of carboxyl group on the surface by chemisorption, which leads to unfavorable condition for polymerization of heptadeca-2,4-diynoic acid. In the case of tricosa-10,12-diynoic acid, containing a flexible methylene chain, inserted between COOH and C≡C?C≡C groups, the anchoring of COOH on the metal surface causes rather favorable effect on the polymerization. 相似文献
794.
Meso- and dl-1,2-diarylethylenediamines (14 species) were evaluated for pre-column fluorescence derivatization reagents in the high-performance liquid chromatographic determination of catecholamines (norepinephrine, epinephrine and dopamine) in human urine and plasma. Of the compounds, meso-1,2-bis(4-methoxyphenyl)ethylenediamine was most preferable for all the catecholamines in terms of sensitivity and selectivity. The detection limit for each catecholamine is approximately 0.5 fmol in a 50-microliters injection volume. 相似文献
795.
L. Bapat G. N. Natu G. Y. Rohokale 《Journal of Radioanalytical and Nuclear Chemistry》1992,165(2):127-136
-Irradiated KCl, KBr and KI are dissolved separately in the emulsion of water and aniline. Halogens as radiolytic products are extracted in aniline forming stable halogen-aniline complexes. Hole species from V2 and V3 centers and free halogens trapped in crystalline salts are solvated first in water phase during dissolution and immediately form complexes with aniline. A typical vibrational structure of absorption bands around 300 nm is observed. The yields of halogens and thereby complexes are found to depend upon the concentration of F and hole centers and the mesh of the salt. 相似文献
796.
Generation of chromioenamines by reduction of O-acetyloximes with chromium(II) and their application
Chromioenamines can be generated by treatment of O-acetyloximes with chromium(II) via two steps of one-electron reduction and successive isomerization, and the species react with aldehydes to give gamma-amino alcohols after reduction with LiAlH4. 相似文献
797.
Y. Oura S. Enomoto H. Nakahara H. Matsue C. Yonezawa 《Journal of Radioanalytical and Nuclear Chemistry》2000,244(2):311-315
Prompt -ray analysis with the internal monostandard method was used to organs taken from rats. After B or Cd was administered, the B/H and Cd/H contents ratios were determined in the brain, kidney, and liver to study their distribution and metabolism. Boron was distributed in all organs but metabolized quickly. Cd was slowly accumulated in the liver and kidneys during the 65 hours studied but no Cd was detected in the brain. 相似文献
798.
E Ohshima T Kumazawa H Takizawa H Harakawa H Sato H Obase Y Oiji A Ishii H Ishii K Ohmori 《Chemical & pharmaceutical bulletin》1991,39(10):2724-2728
A new series of 11-substituted 6,11-dihydrodibenz[b,e]oxepin derivatives was synthesized and evaluated for antiallergic activity. Convenient methods for the preparation of sulfides from alcohols were developed. Structure-activity relationships are described. Compound 7, 11-[2-(dimethylamin)ethyl]thio-6,11-dihydrodibenz[b,e] oxepin-2-carboxylic acid hydrochloride, was the most potent in the rat passive cutaneous anaphylaxis test (ED50 = 0.92 mg/kg p.o.). It had a potent inhibitory effect on anaphylactic bronchoconstriction in guinea pigs (ED50 = 0.029 mg/kg p.o.) and H1 receptor antagonistic effect (Ki = 14 nM) with few central nervous system side effects. Additionally, an antagonistic effect against prostaglandin D2-induced contraction of isolated guinea pig trachea (pA2 = 5.73) was an attractive mechanism of action of the new antiallergic agent. Compound 7 was selected for further evaluation as KW-4994. 相似文献
799.
Isomers of O-alpha-D-glucopyranosyl-(1----6)-O-beta-D-glucopyranosyl- (1----6)-N-[L-aspart-1-oyl-(L-proline)-4-oyl]-alpha-D-glucopyranos ylamine have been prepared, as models for a derivative possibly present in the glomerular basement membrane of rats, by condensation of the corresponding dipeptide derivative (5) with triglycosylamine (4) in the presence of O,O-diethylcyanophosphonate, followed by deprotection of the trisaccharide-dipeptide derivative. During the deprotection process, cis- and trans-isomers containing proline were separated by silica gel column chromatography and also reversed-phase high performance liquid chromatography. 相似文献
800.
Y. L. Tong 《Annals of the Institute of Statistical Mathematics》1987,39(1):289-297
Summary This paper concerns interval estimation of the critical value θ which satisfies
under the general linear model,Y
i
=μ(x
i
)+ε
i
(i=1,2,···), where
for
and the functional forms off
j
′
s are known. From an asymptotic expansion it is shown that, under reasonable conditions, the limiting distribution of
is normal. Thus in the large-sample case a confidence interval for θ can be obtained. Such a result is useful when one is
interested in carrying out a retrospective analysis rather than designing the experiment (as in the Kiefer-Wolfowitz procedure).
In Section 3 a sequential procedure is considered for confidence intervals with fixed width 2d. It is shown that, for a given stopping variableN,
is also asymptotically normal asd→0. Thus the coverage probability converges to 1−α (preassigned) asd→0. An example of application in estimating the phase parameter in circadian rhythms is given for the purpose of illustration.
Research partially supported by the NSF Grant DMS-8502346. 相似文献