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201.
Analysis of scopolamine and its eighteen metabolites in rat urine by liquid chromatography-tandem mass spectrometry 总被引:1,自引:0,他引:1
A rapid and sensitive method is described for the determination of scopolamine and its metabolites in rat urine by combining liquid chromatography and tandem mass spectrometry (LC–MS/MS). Various extraction techniques (free fraction, acid hydrolyses and enzyme hydrolyses) and their comparison were carried out for investigation of the metabolism of scopolamine. After extraction procedure, the pretreated samples were injected into a reversed-phase C18 column with mobile phase of methanol/ ammonium acetate (2 mM, adjusted to pH 3.5 with formic acid) (70:30, v/v) and detected by an on-line MS/MS system. Identification and structural elucidation of the metabolites were performed by comparing their changes in molecular masses (ΔM), retention-times and full scan MSn spectra with those of the parent drug. The results revealed that at least 18 metabolites (norscopine, scopine, tropic acid, aponorscopolamine, aposcopolamine, norscopolamine, hydroxyscopolamine, hydroxyscopolamine N-oxide, p-hydroxy-m-methoxyscopolamine, trihydroxyscopolamine, dihydroxy-methoxyscopolamine, hydroxyl-dimethoxyscopolamine, glucuronide conjugates and sulfate conjugates of norscopolamine, hydroxyscopolamine and the parent drug) and the parent drug existed in urine after ingesting 55 mg/kg scopolamine to healthy rats. Hydroxyscopolamine, p-hydroxy-m-methoxyscopolamine and the parent drug were detected in rat urine for up 106 h after ingestion of scopolamine. 相似文献
202.
A method of determination of adsorbed and absorbed hydrogen on palladium catalysts with carbon carriers is suggested and verified. The method allows Had and Hab to be determined with an accuracy of about 10% using catalysts containing at least 5% Pd.
- . . . 10% , , - , 5% Pd.相似文献
203.
The interaction of oxygen with preadsorbed hydrogen on thermally activated magnesium oxide has been studied by temperature-programmed desorption (TPD) method. It was found that oxygen at 450 K reacts with preadsorbed hydrogen and the resulting hydroxylation suppresses the adsorptive capacity of magnesia with respect to oxygen.
. , 450 K , .相似文献
204.
Purification of astilbin and isoastilbin in the extract of smilax glabra rhizome by high-speed counter-current chromatography 总被引:2,自引:0,他引:2
Purification of astilbin from the rhizome extract of Smilax glabra was conducted using a high-speed counter-current chromatograph equipped with a 700 mL column. In a single operation, 1.5 g of crude sample was separated to yield 105 mg of component astilbin and 48 mg of isoastilbin while the upper phase of the two-phase solvent system composed of n-hexane-n-butanol-water (1:1:2, v/v/v) was used for stationary phase. The chemical structures of the two flavonoid glycosides were confirmed by electrospray ionization ion trap multiple mass spectrometry and nuclear magnetic resonance experiments. 相似文献
205.
The detection of point and other simple mutations in DNA is important for cancer research and diagnosis and other biological studies. Capillary electrophoresis has been successfully used for separating DNA fragments. However, a low-viscosity polymer sieving buffer for DNA separation with on-line coating has never been reported. In this paper, a new method using capillary electrophoresis with on-line coating and laser-induced fluorescence detection (CE-LIF) for screening for point or simple DNA mutations has been demonstrated. The method uses an on-line dynamic coating technique that increases capillary lifetime and analysis reproducibility, and employs a low-viscosity polymer solution, which allows the user to rinse the capillary rapidly and refill with polymer solution easily. Experiments proved that the additives in the separation buffer for on-line capillary coating do not affect the separation efficiency of the running buffer, and do not interfere with the formation of hydrogen-bonded network between boric acid, mannitol and hydroxypropylmethylcellulose polymers. The stability of the dynamically coated capillary was quantitatively studied; the capillary lifetime was increased 6- to 7-fold compared with that of permanently coated CE columns. Standard DNA fragments containing mutations, with sizes of 209, 219, and 338 bps, were successfully separated and detected with this system, after the mutated DNA fragments were cleaved by CEL-I endonuclease. The technique is very sensitive for the size-separation of low-range, middle-range, and high-range DNA fragments. Results were compared with the HPLC methods developed by Transgenomic, Inc. and were in good agreement. The method should be applicable to mutation detection for all relevant biological and clinical studies. The factors influencing separations and the stability of dynamic capillary coatings are also discussed in the paper. 相似文献
206.
Ping Yang Wei Zhang Yukou Du Xiaomei Wang 《Journal of molecular catalysis. A, Chemical》2006,260(1-2):4-10
Platinum nanoparticle core-polyaryl ether trisacetic acid ammonium chloride dendrimer shell nanocomposites (Pt@Gn-NACl) were prepared and used as catalysts for hydrogenation of nitrobenzenes to anilines with molecular hydrogen under mild conditions. The as-prepared nanoparticles have mean particle size from 2.0 to 5.5 nm, depending on the molar ratio of the metal and the dendrimer. The Pt nanoparticles demonstrate near-monodisperse when the molar ratio of Pt and G3-NACl is below 30. The interaction among three carboxyl groups terminated at the dendron and the metallic core keeps the Pt nanoparticles from agglomerating. The colloidal solution of Pt nanoparticles stabilized by the dendrimer, in which the molar ratio of Pt/G3-NACl was less than 60, is stable without precipitation for several weeks. The dendrons attach to the metal core radially, and a substantial fraction of the surface of the metal nanoparticle is unpassivated and available for catalytic reactions. Turnover frequencies for the hydrogenation of nitrobenzenes to anilines change from 353 to 49 h−1 depending on the dendrimer generation and substrates. The dendrimer catalysts are stable during the catalytic hydrogenation process and can be recovered by centrifugation and reused. The results suggest the effectiveness of polyaryl ether trisacetic acid ammonium chloride dendrimer as a stabilizer for the preparation of Pt nanoparticle catalysts. 相似文献
207.
Adam D. Martin Jonathan P. Wojciechowski Eric Y. Du Aditya Rawal Holly Stefen Carol G. Au Liming Hou Charles G. Cranfield Thomas Fath Lars M. Ittner Pall Thordarson 《Chemical science》2020,11(5):1375
Peptide-based nanofibres are a versatile class of tunable materials with applications in optoelectronics, sensing and tissue engineering. However, the understanding of the nanofibre surface at the molecular level is limited. Here, a series of homologous dilysine–diphenylalnine tetrapeptides were synthesised and shown to self-assemble into water-soluble nanofibres. Despite the peptide nanofibres displaying similar morphologies, as evaluated through atomic force microscopy and neutron scattering, significant differences were observed in their ability to support sensitive primary neurons. Contact angle and labelling experiments revealed that differential presentation of lysine moieties at the fibre surface did not affect neuronal viability; however the mobility of phenylalanine residues at the nanofibre surface, elucidated through solid- and gel-state NMR studies and confirmed through tethered bilayer lipid membrane experiments, was found to be the determining factor in governing the suitability of a given peptide as a scaffold for primary neurons. This work offers new insights into characterising and controlling the nanofibre surface at the molecular level.The mobility of hydrophobic moieties at a peptide nanofibre surface determines its suitability as a scaffold for sensitive primary cells. 相似文献
208.
Dai JC Wu XT Fu ZY Cui CP Hu SM Du WX Wu LM Zhang HH Sun RQ 《Inorganic chemistry》2002,41(6):1391-1396
Three novel complexes, Cd3tma2*13H2O (1), Cd3tma2*dabco*2H2O (2), and Cd3Htma3*8H2O (3) (tma = trimesate), of cadmium(II)-trimesate coordination polymers are obtained from hydrothermal reaction. 1 (C18H32O25Cd3) crystallizes in the monoclinic C2/c space group [a = 18.985(2) A, b = 7.3872(6) A, c = 20.432(2) A, = 97.1660(10), and Z = 4]. 2 (C24H22N2O14Cd3) crystallizes in the monoclinic P2(1)/c space group [a = 10.1323(2) A, b = 19.5669(5) A, c = 13.15880(10) A, = 108.9810(10), and Z = 4]. 3 (C27H28O26Cd3) belongs to the trigonal P31c space group [a = 15.7547(3) A, b = 15.7547(3) A, c = 7.93160(10) A, and Z = 2]. The Cd(II) centers in the three complexes are bridged by tma ligands in the coordination fashion of unidentate, bridging unidentate, bidentate, chelating bis-bidentate, chelating/bridging bis-bidentate, or chelating/bridging bidentate to form the T-shaped molecular bilayer motif for 1, chicken-wire-like motif for 2, and honeycomb-like porous structure for 3, respectively, in which the T-shaped molecular bilayer motif and chicken-wire-like motif are further interlinked in interdigitating or alternating fashion to construct the different coordination architectures. These three complexes exhibit strong fluorescent emission bands at 355 nm (lambda(ex) = 220 nm) for 1, 437 nm (lambda(ex) = 365 nm) for 2, and 353 nm (lambda(ex) = 218 nm) for 3 in the solid state at room temperature. 相似文献
209.
A novel approach to the detection of estriol using a flow injection system coupled to enhanced chemiluminescent immunoassay
was developed based on noncompetitive immunoassay formats. A conjugated estriol-ovalbumin immobilized immunoaffinity column
was inserted into the flow system to trap the unbound horseradish peroxidase (HRP)-labeled antibody after an off-line incubation
of estriol and HRP-labeled anti-estriol antibody. The trapped enzyme conjugate was detected by the injection of chemiluminescent
substrates to produce enhanced chemiluminescence. The linear range for the determination of estriol is 10.0 to 400 ng · mL−1 with a correlation coefficient of 0.996 and a detection limit of 5.0 ng · mL−1. The total time for sampling and chemiluminescent detection of one sample is 400 seconds after 30 min of pre-incubation.
The results for pregnancy serum samples obtained by this method are in good agreement with those obtained using ELISA. 相似文献
210.
Nebojša Banjac Gordana Ušćumlić Nataša Valentić Dušan Mijin 《Journal of solution chemistry》2007,36(7):869-878
Absorption spectra of eight 3-substituted-5,5-diphenylhydantoins have been recorded in fourteen solvents in the range 200–400 nm.
The effect of solvent dipolarity/polarizability and solvent/solute hydrogen bonding interactions are analyzed by means of
the linear solvation energy relationship (LSER) concept proposed by Kamlet and Taft. The lipophilic activity of the investigated
hydantoins was estimated by the calculation of log 10
P values with the Advanced Chemistry Development Software. The calculated values of log 10
P were correlated with the ratio of the contributions of specific solvent interactions, and, by employing the linear dependence
thus obtained, the pharmacological activity of the studied hydantoin derivatives is discussed. 相似文献