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Design and development of a two‐dimensional system based on hydrophilic and reversed‐phase liquid chromatography with on‐line sample treatment for the simultaneous separation of excreted xenobiotics and endogenous metabolites in urine
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Diego García‐Gómez Encarnación Rodríguez‐Gonzalo Rita Carabias‐Martínez 《Biomedical chromatography : BMC》2015,29(8):1190-1196
In the present work we describe a two‐dimensional liquid chromatographic system (2D‐LC) with detection by mass spectrometry (MS) for the simultaneous separation of endogenous metabolites of clinical interest and excreted xenobiotics deriving from exposure to toxic compounds. The 2D‐LC system involves two orthogonal chromatographic modes, hydrophilic interaction liquid chromatography (HILIC) to separate polar endogenous metabolites and reversed‐phase (RP) chromatography to separate excreted xenobiotics of low and intermediate polarity. Additionally, the present proposal has the novelty of incorporating an on‐line sample treatment based on the use of restricted access materials (RAMs), which permits the direct injection of urine samples into the system. The work is focused on the instrumental coupling, studying all possible options and attempting to circumvent the problems of solvent incompatibility between the RAM device and the two chromatographic columns, HILIC and RP. The instrumental configuration developed, RAM‐HILIC‐RPLC‐MS/MS, allows the simultaneous assessment of urinary metabolites of clinical interest and excreted compounds derived from exposure to toxic agents with minimal sample manipulation. Thus, it may be of interest in areas such as occupational and environmental toxicology in order to explore the possible relationship between the two types of compounds. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
95.
The use of soft X-rays in a neutrahzer represents an alternative technique that could replace conventional radioactive sources.In this study,we evaluated the charging characteristics of a soft X-ray aerosol neutralize!".In addition,the results from the evaluation of the soft X-ray charger were compared with results obtained using a neutralizer incorporating an 241Am radioactive source.The tandem differential mobility analyzer technique was used previously to determine the size-dependent positive,negative,and neutral charge fractions of a soft X-ray neutralizer.This technique was used to show that the neutral fractions obtained using the soft X-ray charger agreed well with the predictions of bipolar diffusion charging theory,and that the soft X-ray charger could be used as a neutralizer for a scanning mobility particle sizer system. 相似文献
96.
Dmitrievskii A. A. Zhigachev A. O. Zhigacheva D. G. Rodaev V. V. 《Technical Physics》2020,65(12):2016-2025
Technical Physics - The influence of SiO2 impurity (with a concentration varying from 0 to 10 mol %) on the stability of tetragonal ZrO2 (t-ZrO2) and on a set of micro- and macromechanical... 相似文献
97.
Russian Physics Journal - Using the potentials, generated by a tight binding approximation, the equilibrium atomic structure and the phonon spectra of Cr and Ni thin films (one monolayer) deposited... 相似文献
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Solid‐state 31P NMR investigation on the status of guanine nucleotides in paclitaxel‐stabilized microtubules
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Ga Hyang Lee Su Young Oh Kwon Joo Yeo Taslima Ferdous Meeyeon Cho Younkee Paik 《Magnetic resonance in chemistry : MRC》2015,53(5):330-336
Microtubule dynamics is a target for many chemotherapeutic drugs. In order to understand the biochemical effects of paclitaxel on the GTPase activity of tubulin, the status of guanine nucleotides in microtubules was investigated by 31P cross‐polarization magic angle spinning (CPMAS) NMR. Microtubules were freshly prepared in vitro in the presence of paclitaxel and then lyophilized in sucrose buffer for solid‐state NMR experiments. A 31P CPMAS NMR spectrum with the SNR of 25 was successfully acquired from the lyophilized microtubule sample. The broadness of the 31P spectral lines in the spectrum indicates that the molecular environments around the guanine nucleotides inside tubulin may not be as crystalline as reported by many diffraction studies. Deconvolution of the spectrum into four spectral components was carried out in comparison with the 31P NMR spectra obtained from five control samples. The spectral analysis suggested that about 13% of the nucleotides were present as GTP and 37% as GDP in the β‐tubulin (E‐site) of the microtubules. It was found that most of the GDPs were present as GDP‐Pi complex in the microtubules, which seems to be one of the effects of paclitaxel binding. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
100.
Yablokov M. Yu. Shchegolikhin A. N. Lebedev O. V. Goncharuk G. P. Ozerin A. N. 《Russian Chemical Bulletin》2021,70(9):1816-1821
Russian Chemical Bulletin - Gradient polymer composites were prepared by melt-mixing of carbon black and polypropylene in a compounder and subsequent hot pressing of pellets. The thermally treated... 相似文献