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991.
992.
Lipid profiling of human plasma from peritoneal dialysis patients using an improved 2D (NP/RP) LC-QToF MS method 总被引:1,自引:0,他引:1
Min Li Baosheng Feng Yuan Liang Wei Zhang Yu Bai Wen Tang Tao Wang Huwei Liu 《Analytical and bioanalytical chemistry》2013,405(21):6629-6638
An improved online two-dimensional liquid chromatography-quadrupole time-of-flight mass spectrometry (2D LC-QToF MS) system was developed for the lipid profiling of human plasma, in which different lipid classes were separated by the first dimensional normal-phase (NP) LC and different lipid molecular species were separated by the second dimensional reversed-phase (RP) LC. This 2D LC-QToF MS system was built based on a ten-port, two-position valve as the interface, the conditions of which had been optimized and discussed in detail. As two loops were used to trap and transfer the first dimensional elute to the second dimension separately, this new interface suppressed the sample band broadening in the first dimensional column, increased the recovery and repeatability of 2D LC interface, and offered the possibility for the realization of not-stop-flow NP/RP 2D LC system. Finally, 190 endogenous lipid species out of 10 lipid classes were determined within a single run from the plasma of peritoneal patients. This method was also applied to identify the difference in lipid profile between plasma from peritoneal dialysis patients with bad volume status and peritoneal dialysis patients with good volume status. The discovery of 30 potential biomarkers would be helpful to the malnutrition, inflammation, and atherosclerosis syndrome investigation. 相似文献
993.
994.
Wenxue Li Jun Wen Jingyu He Di Cao Fanlu Sun Jinying Li Guorong Fan 《Journal of separation science》2013,36(19):3184-3190
A simple, rapid, high‐throughput, and highly sensitive LC–MS/MS was developed to determine anisodamine in a small volume (50 μL) of beagle dog plasma using atropine sulfate as the internal standard. The analyte and internal standard were isolated from 50 μL plasma samples after a one‐step protein precipitation using Sirocco 96‐well protein precipitation filtration plates. The separation was accomplished on a Hanbon Hedera CN column (100 × 4.6 mm, 5 μm) and the run time was 4 min. A Micromass Quatro Ultima mass spectrometer equipped with an ESI source was operated in the multiple reaction monitoring mode with the precursor‐to‐product ion transitions m/z 306.0→140.0 (anisodamine) and 290.0→123.9 (atropine) used for quantitation. The method was sensitive with a low LOQ of 0.05 ng/mL, and good linearity in the range 0.05–50 ng/mL for anisodamine (r2 ≥ 0.995). All the validation data, such as accuracy, intra‐ and interrun precision, were within the required limits. The method was successfully applied to the pharmacokinetic study of anisodamine hydrochloride injection in beagle dogs. 相似文献
995.
A variety of related impurities, including starting materials, process impurities, and degradation products, can be detected in propofol. In this article, a sensitive and selective GC‐MS/MS method using pulsed splitless injection technique for the determination of 11 main related impurities in propofol in one chromatogram is investigated. This method is extensively validated for its linearity, recovery, precision, LOD, and LOQ, and is able to detect trace‐level related impurities (LOD = 0.2–5.6 μg/g) in propofol bulk drug. Stressed tests proposed that oxidative degradation, photolytic degradation, and heat are the main causes for the formation of degradation products in propofol. 相似文献
996.
The selenium derivatization of nucleic acids and nucleic acid-protein complexes has provided a powerful tool to solve phase problem in X-ray crystallography.Selenium atoms in the nucleotides can serve as fine scattering centers in crystal diffraction.Towards the synthesis of multiple selenium atom-containing nucleotides,which offers strong phasing power to facilitate crystal structure determination,we report here the synthesis of the thymidine analogue containing two Se atoms in one nucleobase.The novel Se-containing nucleoside and oligonucleotide DNAs were synthesized and found with the red-shifted UV spectrum and yellow color.Their unique properties are useful in phase determination,nucleic acid-based detection as well as spectroscopic studies of nucleic acids and nucleic acid-protein complexes. 相似文献
997.
Transthyretin (TTR), a plasma protein with a tetramer structure, could form amyloid fibril associated with several human diseases through the dissociation of tetramer and the misfolding of monomer. These amyloidogenesis can be inhibited by small molecules which bind to the central channel of TTR. A number of small molecules like 2-arylbenzoxazoles (ABZ) analogues are proposed as promising therapeutic strategy to treat amyloidosis. In this work, comparative molecular field analysis (CoMFA) and comparative molecular similarity indices analysis (CoMSIA) three-dimensional quantitative structure-activity relationship (3D-QSAR) and docking studies were performed on series of 2-arylbenzoxazoles (ABZ) and linker-Y analogues to investigate the inhibitory activities of TTR amyloidogenesis at atomic level. Significant correlation coefficients for ABZ series (CoMFA, r 2 = 0.877, q 2 = 0.431; CoMSIA, r 2 = 0.836, q 2 = 0.447) and those for linker-Y series (CoMFA, r 2 = 0.828, q 2 = 0.522; CoMSIA, r 2 = 0.800, q 2 = 0.493) were obtained, and the generated models were validated using test sets. In addition, docking studies on 6 compounds binding to TTR were performed to analyze the forward or reverse binding mode and interactions between molecules and TTR. These results from 3D-QSAR and docking studies have great significance for designing novel TTR amyloidogenesis inhibitors in the future. 相似文献
998.
Catalytic wet air oxidation process, enable to eliminate organic pollutants with non toxic by-product formation, was investigated in micellar system under room condition. Degradation of a series of aromatic compounds, including aromatic hydrocarbons, benzyl alcohol, benzaldehyde, benzoic acid, and some N-containing compounds was carried out based on molybdovanadophosphoric polyoxometalates [(C16H33)N(CH3)3]3+x PV x Mo12?x O40 (x = 1, 2, 3) catalysts and surfactants. Outstanding results (60–96 % degradation efficiencies) were achieved for most of the tested substrates. And the POM micellar catalysts have an excellent stability and can be used as heterogeneous catalysts for about six times. 相似文献
999.
1000.