948 resultados para Chromatographic columns
Resumo:
Through leaching experiments and simulated rainfall experiments, characteristics of vertical leaching of exogenous rare earth elements (REEs) and phosphorus (P) and their losses with surface runoff during simulated rainfall in different types of soils (terra nera soil, cinnamon soil, red soil, loess soil, and purple soil) were investigated. Results of the leaching experiments showed that vertical transports of REEs and P were relatively low, with transport depths less than 6 cm. The vertical leaching rates of REEs and P in the different soils followed the order of purple soil > terra nera soil > red soil > cinnamon soil > loess soil. Results of the simulated rainfall experiments (83 mm h(-1)) revealed that more than 92% of REEs and P transported with soil particles in runoff. The loss rates of REEs and P in surface runoff in the different soil types were in the order of loess soil > terra nera soil > cinnamon soil > red soil > purple soil. The total amounts of losses of REEs and P in runoff were significantly correlated.
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A facile, mild and rapid solid phase synthetic route free of column chromatographic purification to the synthesis of soluble monodisperse long-chain oligo(1,4-phenyleneethynylene)s is presented.
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A method of capillary HPLC-high-resolution MS was developed for the trace analysis of ATP, GTP, dATP and dGTP Dimethylhexylamine (DMHA) was used as ion-pairing agent for the HPLC retention and separation of the nucleotides and positive ion electrospray time-of-flight MS was used for the detection. The application of capillary HPLC allowed minimal usage of DMHA while providing excellent peak retention and resolution, which significantly reduced the ion suppression in electrospray ionization-MS analysis and thus increased the sensitivity. Adduct ions of nucleotides and DMHA were used as quantitative ions in order to achieve the best sensitivity. DMHA concentration at 5 mM in the aqueous mobile phase at pH 7 was found to be the optimal conditions for the C Is capillary column. The method was applied to determine ATP level in cultured C6 glioma cells that were treated with toxic concentrations of Zn. The results showed that the cellular ATP level decreased from 2.7 pmol/cell (<10% cell death) in average control cell samples to 0.36 pmol/cell as the concentration of Zn increased to 120 mg/l (>35% cell death) in culture medium.
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Quantitative structure-retention relationship(QSRR) was studied for amines to gas-liquid chromatography on three stationary phases of different polarities with the topological indices A(m) (A(m1), A(m2), A(m3)) and gravitational index GI. The algorithm of "Leaps and Bounds" was performed for selection of the variables. And the multi-regression and the quasi-Newton neural networks were employed for the calculation with better results.
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Reverse phase high performance liquid chromatography (HPLC) was used to separate and quantify aromatic diester-diacids isomers which arise from the opening selectivity of anhydride rings towards methanol. C-13 NMR spectroscopy was a supplementary tool to characterize the isomer structure. It was found that a meta-position attack is slightly preferred in pyromellitic dianhydride (PMDA), while the preferred position of an attack in bridged dianhydrides is determined by the chemical nature (donors or accepters) of the bridged group. The stronger its electron-withdrawing abilities, the lower the probability of a meta-position attack.
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A modified method for dispersing platinum particles on a glassy carbon (GC) electrode was investigated. The ultramicro Pt particle-modified electrode obtained exhibited high catalytic stability and activity towards the oxidation of some halide ions (Br-, I-) and inorganic sulfur species (S2O32-, SO32- and SCN-). These anions were separated and detected by using ion chromatography and electrochemical detection via this novel dispersed Pt particles-GC working electrode. The detection limits were 20 ng/ml for Br-, 1.0 ng/ml for I-, 10 ng/ml for SO32- and 4.0 ng/ml for SCN-. This method was employed for the analysis of industrial and environmental waste waters.
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This approach is undertaken to examine the correlation ability of the general a(N)-index (GAI) to predict chromatographic behavior. The test is performed on various types of organophosphorus compounds. The results demonstrate that the GAI possesses a good correlation with chromatographic properties.
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A sensitive and efficient method for simultaneous determination of glutamic acid (Glu), gamma-amino-butyric acid (GABA), dopamine (DA), 5-hydroxytryptamine (5-HT) and 5-hydroxyindole acetic acid (5-HIAA) in rat endbrains was developed by high-performance liquid chromatography (HPLC) with fluorescence detection and on-line mass spectrometric identification following derivatization with 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC). Different parameters which influenced derivatization and separation were optimized. The complete separation of five neurotransmitter (NT) derivatives was performed on a reversed-phase Hypersil BDS-C-18 column with a gradient elution. The rapid structure identification of five neurotransmitter derivatives was carried out by on-line mass spectrometry with electrospray ionization (ESI) source in positive ion mode, and the BCEOC-labeled derivatives were characterized by easy-to-interpret mass spectra. Stability of derivatives, repeatability, precision and accuracy were evaluated and the results were excellent for efficient HPLC analysis. The quantitative linear range of five neurotransmitters were 2.441-2 x 10(4) nM, and limits of detection were in the range of 0.398-1.258 nM (S/N = 3:1). The changes of their concentrations in endbrains of three rat groups were also studied using this HPLC fluorescence detection method. The results indicated that exhausting exercise could obviously influence the concentrations of neurotransmitters in rat endbrains. The established method exhibited excellent validity, high sensitivity and convenience, and provided a new technique for simultaneous analysis of monoamine and amino acid neurotransmitters in rat brain. (C) 2008 Elsevier B.V. All rights reserved.
Resumo:
Capillary gas chromatographic enantiomer separation of some polar compounds, including alpha-phenylethylamine, styrene oxide, pyrethroid insecticides and other carboxylates, was investigated on modified cyclodextrin (CD) chiral stationary phases. The chiral stationary phases studied included permethylated beta-CD (PMBCD), heptakis (2,6-di-O-butyl-3-O-butyryl)-beta-CD (DBBBCD), heptakis (2,6-di-O-nonyl-3-O-trifluoroacetyl)-beta-CD (DNTBCD), the mixture of PMBCD and DBBBCD, and the mixture of PMBCD and DNTBCD. On the mixed chiral stationary phases containing the mixtures of derivatized cyclodextrins, enantiomer separation was improved significantly for some compounds as compared to the single cyclodextrin derivative chiral stationary phases, and synergistic effects were observed for some compounds on the mixed cyclodextrin derivative chiral stationary phases.