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1.
Application of surface chemical analysis tools for characterization of nanoparticles 总被引:1,自引:1,他引:0
D. R. Baer D. J. Gaspar P. Nachimuthu S. D. Techane D. G. Castner 《Analytical and bioanalytical chemistry》2010,396(3):983-1002
The important role that surface chemical analysis methods can and should play in the characterization of nanoparticles is
described. The types of information that can be obtained from analysis of nanoparticles using Auger electron spectroscopy
(AES), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary-ion mass spectrometry (TOF-SIMS), low-energy ion scattering
(LEIS), and scanning-probe microscopy (SPM), including scanning tunneling microscopy (STM) and atomic force microscopy (AFM),
are briefly summarized. Examples describing the characterization of engineered nanoparticles are provided. Specific analysis
considerations and issues associated with using surface-analysis methods for the characterization of nanoparticles are discussed
and summarized, with the impact that shape instability, environmentally induced changes, deliberate and accidental coating,
etc., have on nanoparticle properties.
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2.
The element sulfur is almost omnipresent in all natural proteomes and plays a key role in protein quantification. Incorporated
in the amino acids cysteine and methionine, it has been served as target for many protein-labeling reactions in classic quantitative
proteomic approaches based on electrospray or MALDI mass spectrometry. This critical review discusses the potential and limitations
of sulfur isotope dilution analysis (IDA) by inductively coupled plasma—mass spectrometry (ICP-MS) for absolute protein quantification.
The development of this approach was made possible due to the improved sensitivity and accuracy of sulfur isotope ratio measurement
by ICP-MS in recent years. The unique feature of ICP-MS, compound-independent ionization, enables compound (species)-unspecific
sulfur IDA. This has the main advantage that only one generic sulfur standard (i.e., one isotopically labeled sulfur spike)
is required to quantify each peptide or protein in a sample provided that they are completely separated in chromatography
or electrophoresis and that their identities are known. The principles of this approach are illustrated with selected examples
from the literature. The discussion includes also related fields of P/S and metal/S ratio measurements for the determination
of phosphorylation degrees of proteins and stoichiometries in metalloproteins, respectively. Emerging new areas and future
trends such as protein derivatization with metal tags for improved sensitivity of protein detection in ICP-MS are discussed.
Figure The key role of sulfur in protein quantification 相似文献
3.
Rosenberg E 《Analytical and bioanalytical chemistry》2008,391(1):33-57
This review discusses the characterisation of natural organic dyestuffs of historical interest by liquid chromatography–mass
spectrometry. The structures of the most important natural organic dyestuffs traditionally used are presented and discussed
from the perspective of their analytical chemical determination. The practical aspects of the determination of this inhomogeneous
range of compounds with different structures, such as anthraquinones, flavonoids, indigoids or tannins, are discussed with
their implications for sample preparation, liquid chromatographic separation and mass spectrometric detection. The particular
focus of this review is the discussion of the mass spectral fragmentation patterns of the different classes of natural organic
dyestuffs, which in the ideal case allow the identification of the dyestuff actually used, and thereby provide a key to the
better characterisation and understanding of historical objects dyed with natural organic dyestuffs.
Figure LC-MS allows characterisation of natural dyestuff constituents: the MS spectrum of alizarin is superimposed over a photo of
a textile coloured using this red dye 相似文献
4.
Bo Yan Zheng-Jiang Zhu Oscar R. Miranda Apiwat Chompoosor Vincent M. Rotello Richard W. Vachet 《Analytical and bioanalytical chemistry》2010,396(3):1025-1035
Monolayer-protected gold nanoparticles (AuNPs) feature unique surface properties that enable numerous applications. Thus,
there is a need for simple, rapid, and accurate methods to confirm the surface structures of these materials. Here, we describe
how laser desorption/ionization mass spectrometry (LDI-MS) can be used to characterize AuNPs with neutral, positively, and
negatively charged surface functional groups. LDI readily desorbs and ionizes the gold-bound ligands to produce both free
thiols and disulfide ions in pure and complex samples. We also find that LDI-MS can provide a semi-quantitative measure of
the ligand composition of mixed-monolayer AuNPs by monitoring mixed disulfide ions that are formed. Overall, the LDI-MS approach
requires very little sample, provides an accurate measure of the surface ligands, and can be used to monitor AuNPs in complex
mixtures.
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5.
Amino acids are important targets for metabolic profiling. For decades, amino acid analysis has been accomplished by either
cation-exchange or reversed-phase liquid chromatography coupled to UV absorbance or fluorescence detection of pre-column or
post-column-derivatized amino acids. Recent years have seen great progress in the development of direct-infusion or hyphenated
mass spectrometry in the analysis of free amino acids in physiological fluids, because mass spectrometry not only matches
optical detection in sensitivity, but also offers superior selectivity. The advent of cryo-probes has also brought NMR spectroscopy
within the detection limits required for the analysis of free amino acids. But there is still room for further improvement,
including expansion of the analyte spectrum, reduction of sample preparation and analysis time, automation, and synthesis
of affordable isotope standards.
Figure Fully automated gas chromatography-mass spectrometry analysis of amino acids. 相似文献
6.
Christopher T. Kingston Yadienka Martínez-Rubí Jingwen Guan Michael Barnes Christine Scriver Ralph E. Sturgeon Benoit Simard 《Analytical and bioanalytical chemistry》2010,396(3):1037-1044
We have successfully applied coupled thermogravimetry, mass spectrometry, and infrared spectroscopy to the quantification
of surface functional groups on single-walled carbon nanotubes. A high-purity single-walled carbon nanotube sample was subjected
to a rapid functionalization reaction that attached butyric acid moieties to the nanotube sidewalls. This sample was then
subjected to thermal analysis under inert desorption conditions. Resultant infrared and mass spectrometric data were easily
utilized to identify the desorption of the butyric acid groups across a narrow temperature range and we were able to calculate
the degree of substitution of the attached acid groups within the nanotube backbone as 1.7 carbon atoms per hundred, in very
good agreement with independent analytical measurements made by inductively coupled plasma optical emission spectrometry (ICP-OES).
The thermal analysis technique was also able to discern the presence of secondary functional moieties on the nanotube samples
that were not accessible by ICP-OES. This work demonstrates the potential of this technique for assessing the presence of
multiple and diverse functional addends on the nanotube sidewalls, beyond just the principal groups targeted by the specific
functionalization reaction.
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7.
Rodríguez-Fariñas N Gomez-Gomez MM Camara-Rica C 《Analytical and bioanalytical chemistry》2008,390(1):29-35
Oral administration of sodium tungstate is an effective treatment for type 1 and 2 diabetes in animal models; it does not
incur significant side effects, and it may constitute an alternative to insulin. However, the mechanism by which tungstate
exerts its observed metabolic effects in vivo is still not completely understood. In this work, serum-containing proteins
which bind tungstate have been characterized. Size exclusion chromatography (SEC) coupled to inductively coupled plasma mass
spectrometry (ICP-MS) with a Phenomenex Bio-Sep-S 2000 column and 20 mM HEPES and 150 mM NaCl at pH 7.4 as the mobile phase
was chosen as the most appropriate methodology to screen for tungsten–protein complexes. When human serum was incubated with
tungstate, three analytical peaks were observed, one related to tungstate–albumin binding, one to free tungstate, and one
to an unknown protein binding (MW higher than 300 kDa). Matrix-assisted laser desorption ionization time-of-flight (MALDI-TOF)
mass spectrometric analysis of the tungsten-containing fractions collected from SEC–ICP-MS chromatograms, after desalting
and preconcentration processes, confirmed the association of tungstate with albumin and the other unknown protein.
Figure SEC-ICP-MS // MALDI-TOF 相似文献
8.
Nora Graf Thomas Gross Thomas Wirth Wilfried Weigel Wolfgang E. S. Unger 《Analytical and bioanalytical chemistry》2009,393(8):1907-1912
The chemical composition of the functional surfaces of substrates used for microarrays is one of the important parameters
that determine the quality of a microarray experiment. In addition to the commonly used contact angle measurements to determine
the wettability of functionalized supports, X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry
(ToF-SIMS) are more specific methods to elucidate details about the chemical surface constitution. XPS yields information
about the atomic composition of the surface, whereas from ToF-SIMS, information on the molecular species on the surface can
be concluded. Applied on printed DNA microarrays, both techniques provide impressive chemical images down to the micrometer
scale and can be utilized for label-free spot detection and characterization. Detailed information about the chemical constitution
of single spots of microarrays can be obtained by high-resolution XPS imaging.
Figure Eye-catching image for the graphical online abstract 相似文献
9.
Harir M Frommberger M Gaspar A Martens D Kettrup A El Azzouzi M Schmitt-Kopplin P 《Analytical and bioanalytical chemistry》2007,389(5):1459-1467
The photodecomposition of imazamox, a herbicide of the imidazolinone family, was investigated in pure water. The main photoproducts
from the photolysis were followed over time by liquid chromatography mass spectrometry and structures were proposed from exact
mass determinations obtained by electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry. The method
comprised exact mass determination with better than 0.2 ppm mass accuracy and a corresponding structural visualization taking
care of respective isotopes with an adapted van Krevelen diagram that enabled a systematic approach to the characterisation
of the elementary composition of each photoproduct. By taking advantage of the high resolving power of FT-ICR MS to make precise
formula assignments, the derived 2D van Krevelen diagram (O/C; H/C; m/z) enabled one to structurally differentiate the formed photoproducts and to propose a degradation pathway for imazamox.
Figure Overview of applied method to analyse the photolysis process of imazamox herbicide 相似文献
10.
Hirner AV 《Analytical and bioanalytical chemistry》2006,385(3):555-567
The analytical methodology for speciation of metals and metalloids associated with alkyl groups and biomacromolecules is critically reviewed. Alkylated metals and metalloids are not only known to be produced by microbial methylation within most anaerobic compartments in the environment, but also in the course of enzymatic transformations during human metabolism. Because of the toxicological relevance of these compounds present in trace to ultratrace concentrations, firm species identification and exact quantification are essential. While many instrumental techniques coupling chromatography (GC, HPLC, CE, GE) with plasma mass spectrometry (ICP-MS) are available for quantification, methods used for structural identification often suffer from inadequate sensitivity (EI-MS, ESI-MS, MALDI-MS, FT-ICRMS). Other problems encountered are sample derivatisation artefacts, lack of suitable standards for quantification, lack of equilibrium between spikes and sample, and the integrity of metal–protein association during separation, in particular during SDS-PAGE. Selected application examples with respect to mercury and arsenic speciation will be discussed critically.
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11.
Veronica M. T. Lattanzio Michele Solfrizzo Angelo Visconti 《Analytical and bioanalytical chemistry》2009,395(5):1325-1334
The selective enzymatic deacetylation of T-2 toxin to give HT-2 toxin has been investigated in aqueous crude extracts of different
cereals and exploited to develop an analytical method for the determination of the sum of T-2 and HT-2 toxins. The method
has been validated for the analysis of total T-2 and HT-2 toxins in maize, wheat, and oats, showing recoveries from 72 to
97% for maize, from 67 to 84% for wheat, and from 61% to 87% for oats, at spiking levels of 20–400 μg/kg, with relative standard
deviation lower than 10%. Liquid chromatography-tandem mass spectrometry was used for quantitative toxin determination. The
potential biological role of this enzymatic conversion and its perspectives for application in the development of antibody-based
analytical techniques are discussed.
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12.
Heike Traub Markus W?lle Joachim Koch Ulrich Panne Ralf Matschat Heinrich Kipphardt Detlef Günther 《Analytical and bioanalytical chemistry》2009,395(5):1471-1480
Solution-doped metal powder pellets as well as aspirated liquids were used as calibration samples to analyze pure copper and
zinc certified reference materials (CRMs) by femtosecond laser ablation ICP-MS. It was demonstrated that calibration by copper
pellets resulted in relative deviations up to 20%, whereas fs-LA-ICP-MS among copper-based CRMs led to inaccuracies in the
same range unless nominal mass fractions were chosen to be <3 mg/kg. Calibration by zinc pellets generally provided better
accuracy. Depending on the analyte considered, deviations below 10% were obtained even for mass fractions close to the limit
of quantification. Our data, therefore, indicate solution-doped metal powder pellets to be suitable as calibration samples
for fs-LA-ICP-MS of metals. Furthermore, the utilization of liquid standards for calibration was found to result in stronger
deviations of up to 50% for both copper and zinc samples which, in addition, turned out to be dependent on the plasma conditions.
相似文献
13.
Liming Wang Yu-Feng Li Liangjun Zhou Ying Liu Li Meng Ke Zhang Xiaochun Wu Lili Zhang Bai Li Chunying Chen 《Analytical and bioanalytical chemistry》2010,396(3):1105-1114
Integrated analytical techniques were used to study the tissue distribution and structural information of gold nanorods (Au
NRs) in Sprague-Dawley rats through tail intravenous injection. Before in vivo experiments were conducted, careful characterization
of Au NRs was performed. The zeta potential proved that adsorption of bovine serum albumin on Au NRs turned the surface charges
from positive to negative as in an in vitro simulation. The biodistribution of Au NRs was investigated quantitatively by inductively
coupled plasma mass spectrometry at different time points after injection. As target tissues, both liver and spleen were chosen
to further demonstrate the intracellular localization of Au NRs by the combination of transmission electron microscopy and
energy-dispersive X-ray spectroscopy. Moreover, synchrotron-radiation-based X-ray absorption spectroscopy was employed and
it was observed that long-term retention of Au NRs in liver and spleen did not induce obvious changes in the oxidation states
of gold. Therefore, the present systematic method can provide important information about the fates of Au NRs in vivo and
can also be extended to study the biological effects of other metallic nanomaterials in the future.
相似文献
14.
Christian Zwiener Thomas Glauner Jochen Sturm Michael W?rner Fritz H. Frimmel 《Analytical and bioanalytical chemistry》2009,395(6):1885-1892
Potentiostatic-controlled electrochemical reduction of iomeprol was used to deiodinate iomeprol (IMP), a representative of
the iodinated X-ray contrast media. The reduction process was followed by product analysis with liquid chromatography-electrospray
ionization-tandem mass spectrometry and ion chromatography-inductively coupled plasma-mass spectrometry. The identification
is mainly based on the interpretation of the mass fragmentation. The product analysis showed a rather selective deiodination
process with the successive occurrence of IMP-I, IMP-2I, IMP-3I, and a transformation product (TP), respectively. The TP was
formed from IMP-3I by a further cleavage of an amide bond and release of a (C = O)CHOH group from the side chain of IMP. The
iodine mass balance on the basis of IMP and iodide showed a gap of about 26% at the beginning of the electrolysis process
which could be completely closed by taking the intermediates IMP-I and IMP-2I into consideration. This means that the major
intermediates and the TPs were considered and that the reduction process is a rather selective one to remove organically bound
iodine from X-ray contrast media. An attractive application area would be the electrochemical deiodination of X-ray contrast
media in urine of patients or hospital effluents.
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15.
Popot MA Woolfitt AR Garcia P Tabet JC 《Analytical and bioanalytical chemistry》2008,390(7):1843-1852
The insulin-like-growth factor (IGF-I) peptide is considered to be the main indirect marker for growth hormone administration
(GH) in a horse. Further to a previous investigation on measurement of IGF-I in plasma samples by mass spectrometry, this
study focuses on quantitative and qualitative analysis of intact IGF-I in horse plasma. First, protein-transposing software
has been developed for IGF-I to facilitate its quantification by HPLC–electrospray–ion-trap mass spectrometry. Second, product-ion
scan experiments on IGF-I have been conducted on standard samples, non-fortified equine plasma samples, fortified plasma samples,
and equine GH post-administration samples. This “top-down” approach method enables characterisation of fragment ions corresponding
to the carboxy terminal end, which can be useful for the confirmation of the presence of IGF-I in plasma samples.
Figure Structure of IGF-I and amino acid sequences of IGF-I and R3 IGF-I. Deconvolution mass spectra of the IGF-I and R3 IGF-I mixture 相似文献
16.
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
17.
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
18.
Determination of antimicrobial residues and metabolites in the aquatic environment by liquid chromatography tandem mass spectrometry 总被引:2,自引:0,他引:2
Antimicrobials are used in large quantities in human and veterinary medicine. Their environmental occurrence is of particular
concern due to the potential spread and maintenance of bacterial resistance. After intake by the organisms, the unchanged
drug and its metabolized forms are excreted and enter wastewater treatment plants where they are mostly incompletely eliminated,
and are therefore eventually released into the aquatic environment. The reliable detection of several antimicrobials in different
environmental aqueous compartments is the result of great improvements achieved in analytical chemistry. This article provides
an overview of the more outstanding analytical methods based on liquid chromatography tandem mass spectrometry, developed
and applied to determine antimicrobial residues and metabolites present in surface, waste, and ground waters.
相似文献
19.
Sara Wallin Anna Pettersson Henric Östmark Alison Hobro 《Analytical and bioanalytical chemistry》2009,395(2):259-274
A review of standoff detection technologies for explosives has been made. The review is focused on trace detection methods
(methods aiming to detect traces from handling explosives or the vapours surrounding an explosive charge due to the vapour
pressure of the explosive) rather than bulk detection methods (methods aiming to detect the bulk explosive charge). The requirements
for standoff detection technologies are discussed. The technologies discussed are mostly laser-based trace detection technologies,
such as laser-induced-breakdown spectroscopy, Raman spectroscopy, laser-induced-fluorescence spectroscopy and IR spectroscopy
but the bulk detection technologies millimetre wave imaging and terahertz spectroscopy are also discussed as a complement
to the laser-based methods. The review includes novel techniques, not yet tested in realistic environments, more mature technologies
which have been tested outdoors in realistic environments as well as the most mature millimetre wave imaging technique.
Figure Standoff detection and identification is one of the most wanted capabilities 相似文献
20.
Tuulia Hyötyläinen 《Analytical and bioanalytical chemistry》2009,394(3):743-758
Sample preparation before chromatographic separation is the most time-consuming and error-prone part of the analytical procedure.
Therefore, selecting and optimizing an appropriate sample preparation scheme is a key factor in the final success of the analysis,
and the judicious choice of an appropriate procedure greatly influences the reliability and accuracy of a given analysis.
The main objective of this review is to critically evaluate the applicability, disadvantages, and advantages of various sample
preparation techniques. Particular emphasis is placed on extraction techniques suitable for both liquid and solid samples.
Figure Miniaturised extraction techniques allow sensitive analysis of also small sample volumes. 相似文献