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51.
52.
ω-Tetrahydropyran-2-ylsulfanylalkylmagnesium chlorides are prepared as Grignard reagents containing protected mercaptoalkyl chains, which are useful for the direct introduction of ω-mercaptoalkyl chains to electrophiles. In order to prove the usefulness of these reagents, they were reacted with buckminsterfullerene (C60) to give 1-(ω-mercaptoalkyl)-1,2-dihydrobuck minsterfullerenes after the deprotection of THP group with TFA. 相似文献
53.
An analytical method has been developed for determination of dextromethorphan (DMP) and dextrorphan (DRP) in human hair by gas chromatography–mass spectrometry (GC–MS). Hair samples (30 mg) were washed with distilled water and acetone and cut into small fragments (<1 mm) before extraction with methanol. The extracts were evaporated to dryness and then derivatized by use of BSTFA containing 1% TMCS, for preparation of the trimethylsilyl (TMS) derivative of DRP. The extract (1 μL) was then injected into the GC–MS. Recoveries of DMP and DRP at 7.0 and 22.5 ng mg?1 were in the range 90.6–97.2% with intra-assay and inter-assay precision of less than 5.7% and 4.7%, respectively. LOD and LOQ were, respectively, 0.67 and 2.13 ng mg?1 for DMP and 0.14 and 0.47 ng mg?1 for DRP. The responses were linear with correlation coefficients (r > 0.9995) for the drugs studied. The applicability of the method was proven by analysis of authentic hair samples. 相似文献
54.
Jeong Gwi-Taek Park Don-Hee Hwang Baik Park Kyungmoon Kim Si-Wouk Woo Je-Chang 《Applied biochemistry and biotechnology》2002,98(1-9):1115-1127
The growth properties of Panax ginseng hairy roots transformed by Agrobacterium rhizogenes were compared between flask and aerated column or stirred bioreactor. In flask cultures, sucrose, initially 30 g/L, was nearly
exhausted after 45 d of culture. The pH of the medium dropped from 5.5 to 4.96 after 10 d, but afterward it gradually increased
to 6.4. After 45 d, hairy roots grew about 16-folds. The growth rate of hairy roots in air-bubble column or stirred bioreactor
cultures was 1.13 (1.11) to 1.23 (1.20) g fresh wt (dry wt)/(g of cells·d), respectively. For both bioreactors, growth was
about three times as high as in the flask cultivation. 相似文献
55.
56.
A simple method has been developed for the simultaneous determination of N-butylscopolamine bromide and oxazepam in pharmaceutical formulations using first-order digital derivative spectrophotometry. Acetonitrile was selected as the solvent in which both compounds showed well-defined bands. Both analytes showed good stability in this solvent when solutions of the analytes were exposed to light and temperatures between 20 degrees and 80 degrees C. The simultaneous determination of both drugs was performed by the zero-crossing method at 226.0 and 257.0 nm for N-butylscopolamine and oxazepam, respectively. The linear range of determination was found to be 2.5 x 10(-7) to 8.0 x 10(-5) mol/L for N-butylscopolamine and 7.1 x 10(-8) to 8.0 x 10(-5) mol/L for oxazepam. A very good level of repeatability (relative standard deviation) of 0.2% was observed for N-butylscopolamine and oxazepam. The ingredients commonly found in pharmaceutical formulations do not interfere. The proposed method was applied to the determination of these drugs in pharmaceutical formulations (capsules). 相似文献
57.
Ronaldo Santos da Silva Maria Inês Basso Bernardi Antonio Carlos Hernandes 《Journal of Sol-Gel Science and Technology》2007,42(2):173-179
In this work, we have studied the influence of the pH on the synthesis and structural properties of the Ba0.77Ca0.23TiO3 nanopowders synthesized by a modified polymeric precursor method, in order to achieve non-agglomerated powders. Synthesis,
morphology, thermal reactions, crystallite and average particle size of the synthesized powders were investigated through
thermal analysis (DTA/TG), X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM) and Infrared spectroscopy.
In summary, Ba0.77Ca0.23TiO3 nanopowders were synthesized for the first time at a relative low temperature (500 °C). It was also found that the alkalinity
and acidity of the solution presented a great influence on the powder properties. The best results were obtained from solutions
with pH = 8.5 and 11 whose nanopowders presented weakly agglomerate, with homogeneous particle size and a narrow size distribution
(30–40 nm). This behavior could be explained based on the FT-IR results in which it was possible to see the increased of the
chelation in higher pHs. 相似文献
58.
Microwave synthesis,characterization and catalytic properties of titanium-incorporated ZSM-5 zeolite
Taihuan Jin Young Kyu Hwang Do-Young Hong Sung Hwa Jhung Jin-Soo Hwang San-Eon Park Young Ho Kim Jong-San Chang 《Research on Chemical Intermediates》2007,33(6):501-512
Titanium-incorporated ZSM-5 zeolites (Si/Al = 50–200 and Si/Ti = 70) were successfully synthesized in a one-step sol-gel process
under microwave irradiation. The characteristics of Ti-ZSM-5 zeolites were investigated using X-ray power diffraction, UV/Vis-DRS,
FT-IR spectroscopy and solid-state 27Al-NMR to monitor the physico-chemical properties. Simultaneously, the acidic properties were characterized by the NH3-TPD profile. The characterization results revealed that the Ti4+ and Al3+ ions were well incorporated into the framework of Ti-ZSM-5 zeolite. The prepared zeolite was moderately active but selective
in the dehydration of methanol to dimethyl ether. 相似文献
59.
Heo YS Ryu JM Park SM Park JH Lee HC Hwang KY Kim J 《Experimental & molecular medicine》2002,34(3):211-223
Protein-tyrosine phosphatases (PTPs) constitute a family of receptor-like, and cytoplasmic enzymes, which catalyze the dephosphorylation of phosphotyrosine residues in a variety of receptors and signaling molecules. Together with protein tyrosine kinases (PTKs), PTPs are critically involved in regulating many cellular signaling processes. In this study, diverse compounds were screened for PTP inhibition and selectively screened for inhibitors with the end product inhibition properties. Among phosphate analogues and their derivatives for PTP inhibition, Keggin compounds phosphomolybdate (PM) and phosphotungstate (PT) strongly inhibited both PTP-1B and SHP-1, with K(i) values of 0.06-1.2 micromM in the presence of EDTA. Unlike the vanadium compounds, inhibition potencies of PM and PT were not significantly affected by EDTA. PM and PT were potent, competitive inhibitors for PTPs, but relatively poor inhibitors of Ser/Thr phosphatase. Interestingly, PM and PT did not inhibit alkaline phosphatase at all. The crystal structure of PTP-1B in complex with PM, at 2.0 A resolution, reveals that MoO(3), derived from PM by hydrolysis, binds at the active site. The molybdenium atom of the inhibitor is coordinated with six ligands: three oxo-ligands, two apical water molecules and a S atom of the catalytic cysteine residue. In support of the crystallographic finding, we observed that molybdenium oxides (MoO(3), MoO(2), and MoO(2)Cl(2)) inhibited PTP-1B with IC(50) in the range 5-15 micromM. 相似文献
60.
Visible light active platinum-ion-doped TiO2 photocatalyst 总被引:6,自引:0,他引:6
Platinum-ion-doped TiO2 (Pt(ion)-TiO2) was synthesized by a sol-gel method, and its visible light photocatalytic activities were successfully demonstrated for the oxidative and reductive degradation of chlorinated organic compounds. Pt(ion)-TiO2 exhibited a yellow-brown color, and its band gap was lower than that of undoped TiO2 by about 0.2 eV. The flat band potential of Pt(ion)-TiO2 was positively shifted by 50 mV compared with that of undoped TiO2. X-ray absorption spectroscopy and X-ray photoelectron spectroscopy analyses showed that the Pt ions substituted in the TiO2 lattice were present mainly in the Pt(IV) state with some Pt(II) on the sample surface. Pt(ion)-TiO2 exhibited higher photocatalytic activities than undoped TiO2 under UV irradiation as well. The visible light activity of Pt(ion)-TiO2 was strongly affected by the calcination temperature and the concentration of Pt ion dopant, which were optimal at 673 K and 0.5 atom %, respectively. Under visible irradiation, Pt(ion)-TiO2 degraded dichloroacetate and 4-chlorophenol through an oxidative path and trichloroacetate via a reductive path. The activity of Pt(ion)-TiO2 was not reduced when used repeatedly under visible light. However, visible-light-illuminated Pt(ion)-TiO2 could not degrade substrates such as tetramethylammonium and trichloroethylene, which are degraded with UV-illuminated TiO2. The characteristics and reactivities of Pt(ion)-TiO2 as a new visible light photocatalyst were investigated in various ways and discussed in detail. 相似文献