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排序方式: 共有1118条查询结果,搜索用时 15 毫秒
61.
Trifa M. Ahmed Christoffer Bergvall Magnus Åberg Roger Westerholm 《Analytical and bioanalytical chemistry》2015,407(2):427-438
The objective of this study was to develop a novel analytical chemistry method, comprised of a coupled high-performance liquid chromatography–gas chromatography/mass spectrometry system (LC–GC/MS) with low detection limits and high selectivity, for the identification and determination of oxygenated polycyclic aromatic hydrocarbons (OPAHs) and polycyclic aromatic hydrocarbons (PAHs) in urban air and diesel particulate matter. The linear range of the four OPAHs, which include 9,10-anthraquinone, 4H-cyclopenta[def]phenanthrene-4-one, benzanthrone, and 7,12-benz[a]anthraquinone, was 0.7 pg–43.3 ng with limits of detection (LODs) and limits of quantification (LOQs) on the order of 0.2–0.8 and 0.7–1.3 pg, respectively. The LODs in this study are generally lower than values reported in the literature, which can be explained by using large-volume injection. The recoveries of the OPAHs spiked onto glass fiber filters using two different pressurized liquid extraction (PLE) methods were in the ranges of 84–107 and 67–110 %, respectively. The analytical protocols were validated using the following National Institute of Standards and Technology standard reference materials: SRM 1649a (Urban Dust), SRM 1650b (Diesel Particulate Matter), and SRM 2975 (Diesel Particulate Matter, Industrial Forklift). The measured mass fractions of the OPAHs in the standard reference materials (SRMs) in this present study are higher than the values from the literature, except for benzanthrone in SRM 1649a (Urban Dust). In addition to the OPAHs, 44 PAHs could be detected and quantified from the same particulate extract used in this protocol. Using data from the literature and applying a two-sided t test at the 5 % level using Bonferroni correction, significant differences were found between the tested PLE methods for individual PAHs. However, the measured mass fractions of the PAHs were comparable, similar to, or higher than those previously reported in the literature. 相似文献
62.
Magnus Rogeberg Steven Ray WilsonTyge Greibrokk Elsa Lundanes 《Journal of chromatography. A》2010,1217(17):2782-2786
Porous layer open tubular (PLOT) polystyrene divinylbenzene columns have been used for separating intact proteins with gradient elution. The 10 μm I.D. × 3 m columns were easily coupled to standard liquid chromatography–mass spectrometry (LC–MS) instrumentation with commercially available fittings. Standard proteins separated on PLOT columns appeared as narrow and symmetrical peaks with good resolution. Average peak width increased linearly with gradient time (tG) from 0.14 to 0.33 min (tG 20 and 120 min, respectively) using a 3 m column. With shorter columns, peak widths were larger and increased more steeply with gradient time. Theoretical peak capacity (nc) increased with column length (tested up to 3 m). The nc increased with tG until a plateau was reached. The highest peak capacity achieved (nc = 185) was obtained with a 3 m column, where a plateau was reached with tG 90 min. The within- and between column retention time repeatabilities were below 0.6% and below 2.5% (relative standard deviation, RSD), respectively. The carry-over following injection of 0.5 ng per protein was less than 1.1%. The retention time dependence on column temperature was investigated in the range 20–50 °C. Proteins in a skimmed milk sample were separated using the method. 相似文献
63.
Gizelle Cristina Bedendo Isabel Cristina Sales Fontes Jardim Eduardo Carasek 《Journal of chromatography. A》2010,1217(42):6449-6454
A sensitive and precise analysis using hollow fiber renewal liquid membrane (HFRLM) extraction followed by high performance liquid chromatography–tandem mass spectrometry (LC–MS/MS) is described for determination of five sulfonamides in honey samples. In this procedure, the organic solvent introduced directly into the sample matrix extracts the sulfonamides and carries them over the polypropylene porous membrane. An organic solvent is immobilized inside the polypropylene porous membrane, leading to a homogeneous phase. The stripping phase at higher pH in the lumen of the membrane promotes the ionization of the target compounds releasing them to this phase. The most important parameters affecting the extraction efficiency were optimized by multivariable designs (pH and sample mass, pH and buffer for stripping phase, extraction temperature and time, type and volume of extractor solvent and use of salt to saturate the sample). Detection limits in the range of 5.1–27.4 μg kg−1 and linearity coefficient of correlation higher than 0.987 were obtained for the target analytes. The results obtained for the proposed method show that HFRLM–LC–MS/MS can be used for determination of the five sulfonamides studied in honey samples with excellent precision, accuracy, practicality and short analysis time. 相似文献
64.
Leonardo Maestri Teixeira Aaron Strickland Sonny S. Mark Magnus Bergkvist Yajaira Sierra‐Sastre Carl A. Batt 《Macromolecular bioscience》2010,10(2):147-155
S‐Layer proteins are an example of bionanostructures that can be exploited in nanofabrication. In addition to their ordered structure, the ability to self‐assembly is a key feature that makes them a promising technological tool. Here, in vitro self‐assembly kinetics of SpbA was investigated, and found that it occurs at a rate that is dependent on temperature, its concentration, and the concentration of calcium ions and sodium chloride. The activation enthalpy (120.81 kJ · mol?1) and entropy (129.34 J · mol?1 · K?1) obtained infers that the incorporation of monomers incurs in a net loss of hydrophobic surface. By understanding how the protein monomers drive the self‐assembly at different conditions, the rational optimization of this process was feasible.
65.
Magnus G. Johnston 《Journal of solid state chemistry》2004,177(11):4316-4324
Three new hydrated scandium selenites have been hydrothermally synthesized as single crystals and structurally and physically characterized. Sc2(SeO3)3·H2O crystallizes as a new structure type containing novel ScO7 pentagonal bipyramidal and ScO6+1 capped octahedral coordination polyhedra. Sc2(SeO3)3·3H2O contains typical ScO6 octahedra and is isostructural with its M2(SeO3)3·3H2O (M=Al, Cr, Fe, Ga) congeners. CsSc3(SeO3)4(HSeO3)2·2H2O contains near-regular ScO6 octahedra and has essentially the same structure as its indium-containing analogue. All three phases contain the expected pyramidal [SeO3]2- selenite groups. Crystal data: Sc2(SeO3)3·3H2O, Mr=524.85, trigonal, R3c (No. 161), , , , Z=6, R(F)=0.018, wR(F2)=0.036; Sc2(SeO3)3·H2O, Mr=488.82, orthorhombic, P212121 (No. 19), , , , , Z=4, R(F)=0.051, wR(F2)=0.086; CsSc3(SeO3)4(HSeO3)2·2H2O, Mr=1067.60, orthorhombic, Pnma (No. 62), , , , , Z=4, R(F)=0.035, wR(F2)=0.070. 相似文献
66.
Leiming Zhu Leonard Himmel Jean Michél Merkes Prof. Dr. Fabian Kiessling Prof. Dr. Magnus Rueping Dr. Srinivas Banala 《Chemistry (Weinheim an der Bergstrasse, Germany)》2020,26(19):4232-4235
Atropisomerism has been observed in a variety of biaryl compounds and meso-aryl substituted porphyrins. However, in porphyrins, this phenomenon had been shown only with o-substituted 6-membered aromatic groups at the meso-position. We show herein that a 5-membered heteroaromatic (N-mesyl-pyrrol-2-yl) group at the meso-position leads to atropisomerism. In addition, we report a ‘one-pot’ synthetic route for the synthesis of ‘all-pyrrolic’ porphyrin (APP) with several N-protection groups (Boc, Cbz, Ms and Ts). Among these groups, we found that only the Ms group gave four individually separable atropisomers of meso-tetra(N-Ms-pyrrol-2-yl) porphyrin. Furthermore, the reductive removal of Cbz- was achieved to obtain meso-tetra(pyrrol-2-yl) porphyrin. Thus, our synthetic procedure provides an easy access to a group of APPs and stable atropisomers, which is expected to expand the application of novel APP-based materials. 相似文献
67.
Samskog J Bergström SK Jönsson M Klett O Wetterhall M Markides KE 《Electrophoresis》2003,24(11):1723-1729
A method for coupling an electrophoretic driven separation to a liquid flow, using conventional fused-silica capillaries and a soft polymeric interface is presented. A novel design of the electrode providing high voltage to the electrophoretic separation was also developed. The electrode consisted of a conductive polyimide/graphite imbedded coating immobilized onto the capillary electrophoresis (CE) column inlet. This integrated electrode gave the same separation performance as a commonly used platinum electrode. The on-column electrode also showed good electrochemical stability in chronoamperometric experiments. In addition, with this electrode design, the electrode position relative to the inlet end of the CE column will always be constant and well defined. The on-line flow injection analysis (FIA)-CE system was used with electrospray ionization (ESI)-time of flight (TOF)-mass spectrometry detection. The preparation of the PDMS (poly(dimethylsiloxane)) interface for FIA-CE is described in detail and used for initial tests of the on-column polymer-imbedded graphite inlet electrode. In this interface, a pressure-driven liquid flow, a make up CE electrolyte and a CE column inlet meet in a two-level cross (95 microm ID) in the PDMS structure, enabling independent flow characterization. 相似文献
68.
Lemos Judith L. S. Fontes Maria C. de A. Pereira Nei 《Applied biochemistry and biotechnology》2001,91(1-9):681-689
The use of purified xylan as a substrate for bioconversion into xylanases increases the cost of enzyme production. Consequently,
there have been attempts to develop a bioprocess to produce such enzymes using different lignocellulosic residues. Filamentous
fungi have been widely used to produce hydrolytic enzymes for industrial applications, including xylanases, whose levels in
fungi are generally much higher than those in yeast and bacteria. Considering the industrial importance of xylanases, the
present study evaluated the use of milled sugarcane bagasse, without any pretreatment, as a carbon source. Also, the effect
of different nitrogen sources and the C∶N ratio on xylanase production by Aspergillus awamori were investigated, in experiments carried out in solid-state fermentation. High extracellular xylanolytic activity was observed
on cultivation of A. awamori on milled sugarcane bagasse and organic nitrogen sources (45 IU/mL for endoxylanase and 3.5 IU/mL for β-xylosidase). Endoxylanase
and β-xylosidase activities were higher when sodium nitrate was used as the nitrogen source, when compared with peptone, urea,
and ammonium sulfate at the optimized C∶N ratio of 10∶1. The use of yeast extract as a supplement to the these nitrogen sources
resulted in considerable improvementin the production of xylanases, showing the importance of this organic nitrogen source
on A. awamori metabolism. 相似文献
69.
Janina Sroka-Markovic Linda Johansson Magnus B. O. Andersson Ingrid Granelli 《Chromatographia》2012,75(7-8):329-336
Development of a reversed phase high performance liquid chromatographic method for determination of six related impurities in prilocaine substance is reported. The test of related impurities in European Pharmacopoeia (Ph. Eur.) cannot meet the demands with the chromatographic parameters given, therefore different types of chromatographic systems and eight columns have been evaluated in the present study. A new method with a Hypercarb column was developed and validated. This method fulfils the demands in the Ph. Eur., and the validation shows that the method is selective, reproducible, linear, accurate and robust with sufficient limits of detection (0.001–0.004% of 2.5?mg prilocaine mL?1) and quantification (0.002–0.009% of 2.5?mg prilocaine mL?1). 相似文献
70.