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101.
Sudarsanan Varaprath Mark Seaton Debra McNett Lin Cao Kathleen P. Plotzke 《International journal of environmental analytical chemistry》2013,93(3):203-219
Abstract A method was developed and validated to measure octamethylcyclotetrasiloxane (D4)? quantitatively by gas chromatography-mass spectrometry (GC-MS) at low level in extracts of several biological matrices that include plasma, liver, lung, feces and fat from rats. The key to the successful determination lay in the use of extracts dried with anhydrous magnesium sulfate. This was necessary in view of the propensity of the methyl siloxane based GC-stationary phase to generate D4 by its reaction with water present in the extracts. To enable quantiiation of D4 at parts per billion (μg/L) levels, the base ion m/z 281 resulting from the loss of a methyl group from the parent molecule was selected for monitoring by SIM mode in GC-MS. The recovery of D4 from any of the biological matrices was determined to be greater than 90% in three extractions. The D4 response for the standards in GC-MS was linear (R2 > 0.9900) and reproducible at concentrations ranging from 1—16,000 ng D4/g solvent. Precision was less than 5%. 相似文献
102.
Carmen Gal Remus Nutiu 《International journal of environmental analytical chemistry》2013,93(7):447-460
An extraction device has been investigated for the separation and preconcentration of a series of volatile organic compounds (CHCl3, CHCl2Br, CHClBr2 and CHBr3) in aqueous matrices. The device consisted of a microporous membrane system utilising a hollow fibre tube filled with organic solvent directly immersed into the sample solution. The hollow fibre containing 160 µL organic solvent was immersed in a glass vial with 10 mL capacity, and the extraction took place through diffusive transport between the aqueous sample and the small amount of solvent. For validation of the method, some operational conditions, such as extraction solvent, temperature, stirring rate and separation time, were optimised. Limit of detection was at low ppb levels, with GC-MS analysis under selected ion monitoring (SIM), whereas enrichment factors between 22 and 35 were obtained. Good reproducibility with RSDs between 7.2% and 9.8% and large linear dynamic ranges with R 2 between 0.996 and 0.998 were also achieved. In addition, the performance of the membrane assisted solvent extraction (MASE) system was compared with two existing configurations: a non-porous membrane separation device, as well as with a comparable microporous configuration. The comparison considered the extraction mechanism and the underlying transport processes. The application to real samples showed a good concordance with classical analytical methods. 相似文献
103.
Ionic liquids as stationary phases in gas chromatography: Determination of chlorobenzenes in soils 下载免费PDF全文
Rosa María González Paredes Carmelo García Pinto José Luis Pérez Pavón Bernardo Moreno Cordero 《Journal of separation science》2014,37(12):1448-1455
The present research focuses on the evaluation of different ionic liquid (IL) stationary phases in gas chromatography. The different IL columns were evaluated in terms of peak resolution (Rs) and peak symmetry for the separation of the chlorobenzenes. The determination of chlorobenzenes in soil samples by means of the optimal IL stationary phase (SLB‐IL82) is proposed as an application. Soil pretreatment was based on a simplified quick, easy, cheap, effective, rugged, and safe extraction procedure and a large injection volume via a programed temperature vaporizer working in solvent vent mode. The retention time of the chlorobenzenes increased as the polarity of the IL column decreased. SLB‐IL82 is the stationary phase that provides the best values as regards Rs and asymmetry factor. Soil sample blanks were spiked with the analytes before subjecting the sample to the extraction process. The existence of a matrix effect was checked and the analytical characteristics of the method were determined in a fortified garden soil sample. The method provided good linearity, good repeatability and reproducibility values, and the LODs were in the 0.1–4.7 μg/kg range. Two fortified soil samples were applied to validate the proposed methodology. 相似文献
104.
This brief review analyzes the parameters that can be used to guide the generation of hierarchic systems that include inorganic and/or biological nanoscale objects. Importance of interface effects and geometrical factors are underlined. The mutual influence between the substrate and the deposited material is an important factor to determine the most appropriate set of parameters for the synthesis of nanomaterials with desirable properties for industrial applications. 相似文献
105.
Zhentao Tang Fei Liu Fang Fang Xuelu Ding Qingrong Han Yuzhu Tan Cheng Peng 《Journal of separation science》2022,45(13):2273-2300
Mycotoxin contamination is a globally concerned problem for food and agricultural products since it may directly or indirectly induce severe threats to human health. Sensitive and selective screening is an efficient strategy to prevent or reduce human and animal exposure to mycotoxins. However, enormous challenges exist in the determination of mycotoxins, arising from complex sample matrices, trace-level analytes, and the co-occurrence of diverse mycotoxins. Appropriate sample preparation is essential to isolate, purify, and enrich mycotoxins from complicated matrices, thus decreasing sample matrix effects and lowering detection limits. With the cross-disciplinary development, new solid-phase extraction strategies have been exploited and integrated with nanotechnology to meet the challenges of mycotoxin analysis. This review summarizes the advance and progress of solid-phase extraction techniques as the methodological solutions for mycotoxin analysis. Emphases are paid on nanomaterials fabricated as trapping media of solid-phase extraction techniques, including carbonaceous nanoparticles, metal/metal oxide-based nanoparticles, and nanoporous materials. Advantages and limitations are discussed, along with the potential prospects. 相似文献
106.
We apply random matrix theory to compare correlation matrix estimators C obtained from emerging market data. The correlation matrices are constructed from 10 years of daily data for stocks listed on the Johannesburg stock exchange (JSE) from January 1993 to December 2002. We test the spectral properties of C against random matrix predictions and find some agreement between the distributions of eigenvalues, nearest neighbour spacings, distributions of eigenvector components and the inverse participation ratios for eigenvectors. We show that interpolating both missing data and illiquid trading days with a zero-order hold increases agreement with RMT predictions. For the more realistic estimation of correlations in an emerging market, we suggest a pairwise measured-data correlation matrix. For the data set used, this approach suggests greater temporal stability for the leading eigenvectors. An interpretation of eigenvectors in terms of trading strategies is given, as opposed to classification by economic sectors. 相似文献
107.
Ştefan Ţălu Sebastian Stach Joana Zaharieva Maria Milanova Dimitar Todorovsky Stefano Giovanzana 《International Journal of Polymer Analysis and Characterization》2014,19(5):404-421
The structural complexity of the 3-D surface of poly(methylmethacrylate) films with immobilized europium β-diketonates was studied by atomic force microscopy and fractal analysis. Fractal analysis of surface roughness revealed that the 3-D surface has fractal geometry at the nanometer scale. Poly(methylmethacrylate) (PMMA) as immobilization matrix is dense and uniform, and a tendency for formation of chain structures was observed. Fractal analysis can quantify key elements of 3-D surface roughness such as the fractal dimensions D f determined by the morphological envelopes method of the Eu(DBM)3 and Eu(DBM)3 · dpp nanostructures, which are not taken into account by traditional surface statistical parameters. 相似文献
108.
Polydimethylsiloxane: A General Matrix for High‐Performance Chromatographic NMR Spectroscopy 下载免费PDF全文
Dr. Shaohua Huang Dr. Jun Gao Rui Wu Prof. Dr. Shengying Li Prof. Dr. Zhengwu Bai 《Angewandte Chemie (International ed. in English)》2014,53(43):11592-11595
The detection and structural characterization of the components of a mixture is a challenging task. Therefore, the development of a facile and general method that enables both the separation and the structural characterization of the components is desired. Diffusion‐ordered NMR spectroscopy (DOSY) with the aid of a matrix is a promising tool for this purpose. However, because the currently existing matrices only separate limited components, the application of the DOSY technique is restricted. Herein we introduce a new versatile matrix, poly(dimethylsiloxane), which can fully separate many mixtures of different structural types by liquid‐state NMR spectroscopy. With poly(dimethylsiloxane), liquid‐state chromatographic NMR spectroscopy could become a general approach for the structural elucidation of mixtures of compounds. 相似文献
109.
Construction of 3D tissues by various types of cells with specific characteristics is an important and fundamental technology in tissue reconstruction medicine and animal‐free diagnosis system. To do so, an excellent extracellular matrix (ECM) is needed for encapsulation of cells and maintaining cell activity. Spontaneously forming hydrogel matrix is used by complexation between two water‐soluble polymers, 2‐methacryloyloxyethyl phosphorylcholine polymer bearing phenylboronic acid groups and poly(vinyl alcohol). Two cytokines for cell proliferation are immobilized in the hydrogel matrix to control the activities of the encapsulated cells. The cytokine‐immobilized hydrogel matrix can encapsulate both L929 fibroblasts and normal human dermal fibroblasts under mild condition. The physical properties of the hydrogel matrix can follow the proliferation process of the encapsulated cells. The encapsulated cells secrete ECM in the polymer hydrogel networks upon 3D culturing for 7 days. Consequently, the tissue‐mimicking ECM hybrid hydrogels are fabricated successfully. 相似文献
110.
Motivated by the theory of self‐duality that provides a variational formulation and resolution for non‐self‐adjoint partial differential equations (Ann. Inst. Henri Poincaré (C) Anal Non Linéaire 2007; 24 :171–205; Selfdual Partial Differential Systems and Their Variational Principles. Springer: New York, 2008), we propose new templates for solving large non‐symmetric linear systems. The method consists of combining a new scheme that simultaneously preconditions and symmetrizes the problem, with various well‐known iterative methods for solving linear and symmetric problems. The approach seems to be efficient when dealing with certain ill‐conditioned, and highly non‐symmetric systems. The numerical and theoretical results are provided to show the efficiency of our approach. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献