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1.
Han X Wang C He L Beesley TE Armstrong DW 《Analytical and bioanalytical chemistry》2007,387(8):2681-2697
A new synthetic polymeric chiral stationary phase for liquid chromatography was prepared via free-radical-initiated polymerization
of trans-9,10-dihydro-9,10-ethanoanthracene-(11S,12S)-11,12-dicarboxylic acid bis-4-vinylphenylamide. The new polymeric chiral stationary phase (CSP) showed enantioselectivity
for many chiral compounds in multiple mobile phases. High stability and sample capacities were observed on this polymeric
chiral stationary phase. Mobile phase components and additives affected chiral separation greatly. This new synthetic chiral
stationary phase is complementary to two other related commercially available CSPs: the P-CAP and P-CAP-DP columns. Interactions
between the chiral stationary phase and analytes that lead to retention and chiral recognition include hydrogen bonding, dipolar,
and π–π interactions. Repulsive (steric) interactions also contribute to chiral recognition.
Figure LC chromatograms showing the analytical (blue) and preparative (red) separations of N-(3,5-dinitrobenzoylleucine) enantiomers on a new synthetic polymeric chiral stationary phase 相似文献
2.
Webb A 《Analytical and bioanalytical chemistry》2007,388(3):525-528
Figure Schematic diagram of a typical arrangement used for hyphenating chemical microseparations (e.g. capillary HPLC, CE, or CEC)
with microcoil NMR detection 相似文献
3.
Ma X Zhu T Xu H Li G Zheng J Liu A Zhang J Du H 《Analytical and bioanalytical chemistry》2008,390(4):1133-1137
A chemical prototype sensor was constructed based on nanofiber-structured TiO2 and highly sensitive quartz resonators. The gas-sensing behavior of this new sensor to selected simulant warfare agents was
investigated at room temperature. Results showed rapid response and good reversibility of this sensor when used with high-purity
nitrogen. This provides a simple approach to preparation of materials needed as chemical sensors for selected organic volatiles
or warfare agents.
Figure Sensing behavior of TiO2 nanofiber sensor to chemical vapors 相似文献
4.
We have developed an iterative procedure for predicting the retention times of polycyclic aromatic hydrocarbons (PAHs) and
n-alkanes during separations by temperature-programmed gas chromatography. The procedure is based on estimates of two thermodynamic
properties for each analyte (the differences in enthalpy and entropy associated with movements between the stationary and
mobile phases) derived from data acquired experimentally in separations under isothermal conditions at temperatures spanning
the range covered by the temperature programs in ten-degree increments. The columns used for this purpose were capillary columns
containing polydimethylsiloxane-based stationary phases with three degrees of phenyl substitution (0%, 5%, and 50%). Predicted
values were mostly within 1% of experimentally determined values, implying that the method is stable and precise.
Figure Predicted values were mostly within 1 % of experimentally determined values, thus implying that the method is stable and precise 相似文献
5.
Klejdus B Vacek J Benesová L Kopecký J Lapcík O Kubán V 《Analytical and bioanalytical chemistry》2007,389(7-8):2277-2285
A rapid-resolution HPLC/UV-VIS DAD separation method (which takes <1 min) for the determination and identification of genistin,
genistein, daidzein, daidzin, glycitin, glycitein, ononin, formononetin, sissotrin and biochanin A in fmol quantities in submicroliter
sample volumes was optimized. A linear gradient elution (0 min 22% B, 1.0 min 80% B, 1.4 min 100% B, 1.8 min 22% B) using
a mobile phase containing 0.2 % (v/v) acetic acid (solvent A) and methanol (solvent B) was applied on a Zorbax SB C18 column (1.8 μm particle size) at 80 °C. The method was verified using samples of bits of soy and methanolic extracts from
Trifolium pratense, Iresine herbstii and Ononis spinosa plants. Pseudobaptigenin glucoside, irilone, prunetin, texasin, tlatlancuayin and other isoflavones, in addition to aglycones
of isoflavones and their β-glucosides and malonyl and acetyl derivatives, were identified by UV-VIS DAD and electrospray mass
spectrometric (ESI-MS) detection in the extracts.
Figure Rapid resolution HPLC for determination and identification of isoflavones in soy preparations and plant extracts 相似文献
6.
The integration of a range of technologies including microfluidics, surface-enhanced Raman scattering and confocal microspectroscopy
has been successfully used to characterize in situ single living CHO (Chinese hamster ovary) cells with a high degree of spatial (in three dimensions) and temporal (1 s per spectrum) resolution. Following the introduction of a continuous flow of ionomycin, the real time spectral response
from the cell was monitored during the agonist-evoked Ca2+ flux process. The methodology described has the potential to be used for the study of the cellular dynamics of a range of
signalling processes.
Figure Spectral mapping of a single CHO cell 相似文献
7.
The derivatization of cysteine-containing peptides with benzoquinone compounds is rapid, quantitative and specific in acidic
media. The conversion of cysteines into hydrophobic benzoquinone-adducted residues in peptides is used here to alter the chromatographic
properties of cysteinyl peptides during liquid chromatography separation. The benzoquinone derivatization is shown to allow
the accurate selection of cysteine-containing peptides of bovine serum albumin tryptic digest by diagonal reversed-phase chromatography,
which consists of one primary and a series of secondary identical liquid chromatographic separations, before and after a cysteinyl-targeted
modification of the peptides by benzoquinone compounds.
Figure Diagonal chromatographic selection of cysteinyl peptides modified with benzoquinones
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
8.
Various toxicological and metabolic interactions have been reported to exist between arsenic and selenium. In the present
study, synthetic seleno-arsenic compounds, potentially suitable for probing metabolic interactions between these two elements,
were prepared and tentatively characterized by using high-performance liquid chromatography (HPLC)–electrospray tandem mass
spectrometry and HPLC–inductively coupled plasma mass spectrometry. In analogy to the recently identified thio-arsenic species,
which can be prepared from their corresponding oxo-arsenic species via reaction with H2S, the seleno-arsenic compounds were also derived from oxo-arsenic compounds via reaction with H2Se.
Figure H2Se bubbled into solutions containing oxo‐arsenosugars converts them into their seleno‐arsenosugar analogues. 相似文献
9.
An impurity-profiling method for 3,4-methylenedioxymethamphetamine (MDMA) is presented. The impurities of interest were extracted
by solid-phase extraction (SPE) on Bakerbond C18 spe columns from a weakly alkaline solution (pH 8.5). Development of the extraction conditions covered selection of the buffer
for dissolution of the sample and the volume of the eluent used to elute the impurities. An important part of the studies
was to optimise the separation conditions, and the simplex method was used for this purpose. Cluster analysis was applied
for comparison of samples and its grouping. The developed method was based on the areas of 33 selected peaks corresponding
to MDMA impurities. All examined samples were correctly classified into clusters corresponding to the synthetic route.
相似文献
10.
Lee JO So HM Jeon EK Chang H Won K Kim YH 《Analytical and bioanalytical chemistry》2008,390(4):1023-1032
Recent advances in nanotechnology have enabled the development of nanoscale sensors that outperform conventional biosensors.
This review summarizes the nanoscale biosensors that use aptamers as molecular recognition elements. The advantages of aptamers
over antibodies as sensors are highlighted. These advantages are especially apparent with electrical sensors such as electrochemical
sensors or those using field-effect transistors.
Figure Feeling proteins with aptamer-functionalized carbon nanotubes 相似文献
11.
Acetone plays an important role in the chemistry of both the atmosphere and the ocean, due to its potential effect on the
tropospheric HOx (= HO + HO2) budget, as well as its environmental and health effects. We discuss the development of a mobile, sensitive, selective, economical
and facile method for the determination of acetone in seawater. The method consists of derivatizing acetone to its pentafluorobenzyl
oxime using 1,2,3,4,5-pentafluorobenzylhydroxylamine (PFBHA), followed by solid-phase microextraction (SPME) and analysis
by gas chromatography/mass spectrometry (GC/MS). A detection limit of 3.0 nM was achieved. The buffering capacity of seawater
imposes challenges in using the method’s optimum pH (3.7) on seawater samples, requiring calibration standards to be made
in buffered salt water and the acidification of seawater samples and standards prior to extraction. We employed the technique
for analysis of selected surface seawater samples taken on the Nordic seas during the ARK-XX/1 cruise (R.V. Polarstern). An upper limit of 5.5–9.6 nM was observed for acetone in these waters, the first acetone measurements reported for far
North Atlantic and Arctic waters.
Simplified schematic of transformations of organic compounds at the atmosphere–ocean interface 相似文献
12.
Herschbach H Hosomizu K Hahn U Leize E Van Dorsselaer A Imahori H Nierengarten JF 《Analytical and bioanalytical chemistry》2006,386(1):46-51
The electrospray mass spectrometric characterization of neutral dendrons with a carboxylic acid function or a t-butyl ester moiety at the central point and up to eight peripheral C60 subunits has been performed and is described in detail. Molecules bearing a carboxylic acid group at the center turned out
to be preferentially ionized by deprotonation, whereas those with a t-butyl ester head group were ionized by reduction of the C60 units in the infusion capillary of the electrospray source.
Electronic supplementary material Supplementary material is available for this article at and is accessible for authorized users. 相似文献
13.
Lisowski W Keim EG Kaszkur Z van den Berg AH Smithers MA 《Analytical and bioanalytical chemistry》2007,389(5):1489-1498
Using a combination of scanning electron microscopy, transmission electron microscopy (TEM), X-ray diffraction and X-ray photoelectron
spectroscopy (XPS), we made a comparative study of the high-temperature annealing impact on thin titanium deuteride (TiD
y
) films covered by an ultrathin Pd layer, and on Ti/Pd bilayer films. The bilayer films were prepared under ultrahigh vacuum
conditions and were in situ annealed using the same annealing procedure. It was found that the surface and the bulk morphology
of both films undergo different annealing-induced transformations, leading to an extensive intermixing between the Ti and
Pd layers and the formation of a new PdTi2 bimetallic phase. Energy-filtered TEM imaging and energy-dispersive X-ray spectrometry analysis, as well as XPS depth profiling
all provided evidence of a different distribution of Pd and Ti in the annealed TiD
y
/Pd film compared with the annealed Ti/Pd film. Our results show that thermal decomposition of TiD
y
, as a consequence of annealing the TiD
y
/Pd film, modifies the intermixing process, thereby promoting Ti diffusion into the Pd-rich top layer of the TiD
y
film and thus providing a more likely path for the formation of the PdTi2 phase than in an annealed Ti/Pd film.
Figure Figure Microstructural and chemical characterisation of thin TiDy/Pd film after annealing 相似文献
14.
András Gergely Péter Horváth György Szász Gábor Veress 《Analytical and bioanalytical chemistry》2009,394(8):2105-2109
A three-step gradient reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for the separation
of dehydroepiandrosterone (DHEA), its sulfate ester (DHEA-S), its three C7-oxidized metabolites (7αOH-DHEA, 7βOH-DHEA, 7-keto-DHEA),
and its biosynthetic congeners (androstenedione, testosterone, estradiol, pregnenolone). This new method allows the quantitative
characterization of DHEA metabolism and biosynthetic transformation under given physiological, pathological, or therapeutically
influenced circumstances. Tetrahydrofuran probably acts as a proton acceptor coadsorbent, while isopropanol behaves as a proton
donor during the separation of testosterone, estradiol, and the stereoisomers of 7-OH-DHEA.
Figure Optimized gradient RP-HPLC results in full separation of DHEA from its biosynthetic congeners and metabolites 相似文献
15.
16.
17.
Pérez Pavón JL García Pinto C Guerrero Peña A Moreno Cordero B 《Analytical and bioanalytical chemistry》2008,391(2):599-607
In the present work we report the results obtained with a methodology based on direct coupling of a headspace generator to
a mass spectrometer for the identification of different types of petroleum crudes in polluted soils. With no prior treatment,
the samples are subjected to the headspace generation process and the volatiles generated are introduced directly into the
mass spectrometer, thereby obtaining a fingerprint of volatiles in the sample analysed. The mass spectrum corresponding to
the mass/charge ratios (m/z) contains the information related to the composition of the headspace and is used as the analytical signal for the characterization
of the samples. The signals obtained for the different samples were treated by chemometric techniques to obtain the desired
information. The main advantage of the proposed methodology is that no prior chromatographic separation and no sample manipulation
are required. The method is rapid, simple and, in view of the results, highly promising for the implementation of a new approach
for oil spill identification in soils.
Figure PCA score plots illustrate clear discrimination of types of crude oil in polluted soil samples (e.g. results are shown for
vertisol) 相似文献
18.
Henchoz Y Schappler J Geiser L Prat J Carrupt PA Veuthey JL 《Analytical and bioanalytical chemistry》2007,389(6):1869-1878
A rapid and universal capillary zone electrophoresis (CZE) method was developed to determine the dissociation constants (pK
a) of the 20 standard proteogenic amino acids. Since some amino acids are poorly detected by UV, capacitively coupled contactless
conductivity detection (C4D) was used as an additional detection mode. The C4D coupling proved to be very successful on a conventional CE-UV instrument, neither inducing supplementary analyses nor instrument
modification. In order to reduce the analysis time for pK
a determination, two strategies were applied: (i) a short-end injection to reduce the effective length, and (ii) a dynamic
coating procedure to generate a large electroosmotic flow (EOF), even at pH values as low as 1.5. As a result, the analysis
time per amino acid was less than 2 h, using 22 optimized buffers covering a pH range from 1.5 to 12.0 at a constant ionic
strength of 50 mM. pK
a values were calculated using an appropriate mathematical model describing the relationship between effective mobility and
pH. The obtained pK
a values were in accordance with the literature.
Figure
a UV (1) and C4D (2) detectors placed on-line on the CE capillary. b Curve of effective mobility as a function of pH for histidine 相似文献
19.
Ortner K Sivanandam VN Buchberger W Müller N 《Analytical and bioanalytical chemistry》2007,388(1):173-177
Enzymatically cleaved glycans from sub-milligram quantities of erythropoietin (EPO) and ovalbumin have been analyzed, without
further purification, by two-dimensional diffusion-ordered nuclear magnetic resonance spectroscopy. At NMR sample concentrations
below 50 μmol L−1 the major components of the oligosaccharide fractions could be distinguished by their anomeric proton chemical shift and
their size-dependent diffusion coefficients.
Figure
1H NMR diffusion decay curves of anomeric protons in the EPO glycan fraction 相似文献
20.
Surmeian A Diplasu C Groza A Ganciu M Belenguer P Tempez A Chapon P 《Analytical and bioanalytical chemistry》2007,388(8):1625-1629
A high-current pulsed hollow cathode discharge was used to study the role of atomic and ionic metastables involved in ionization
plasma processes. We observed the enhancement of the spectral emission lines of noble gas ions in the afterglow. A study of
the processes that involve atomic and ionic metastables is of great interest since it should lead to a better understanding
of and enhanced control over the ionization mechanisms crucial to analytical glow discharge mass spectrometry (GDMS) analysis.
Figure Time profile of Ti, Ti+, and Ne+ spectral lines 相似文献