World Congress on Biosensors 2014

World Congress on Biosensors 2014
Biosensors 2014

Wednesday 19 September 2012

Just Published: Journal of Chromatography A


A new issue of this journal has just been published. To see abstracts of the papers it contains (with links through to the full papers) click here:
Journal of Chromatography A
Selected papers from the latest issue:

Mass spectrometry: Innovation and application. Part VII

19 September 2012, 08:44:59
Publication year: 2012
Source:Journal of Chromatography A, Volume 1259
M. Holčapek, P.J. Schoenmakers

Recent developments in liquid chromatography–mass spectrometry and related techniques

19 September 2012, 08:44:59
Publication year: 2012
Source:Journal of Chromatography A, Volume 1259
Michal Holčapek, Robert Jirásko, Miroslav Lísa
This review summarizes the state-of-art in liquid chromatography–mass spectrometry (LC–MS) and related techniques with the main focus on recent developments in the last decade. LC–MS records an enormous growth in recent years due to the application potential in analytical chemistry, biochemistry, pharmaceutical analysis, clinical analysis and many other fields, where the qualitative and quantitative characterization of complex organic, bioorganic and organometallic mixtures is needed. Beginners and moderately experienced LC–MS users may be confused by the number of different LC–MS systems on the market, therefore an actual overview of mass spectrometers designed for the LC–MS configuration and matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) from main manufacturers is compiled here together with an independent assessment of their advantages and limitations. Current trends in terms of mass analyzers, ionization techniques, fast LC–MS, LC–MALDI-MS, ion mobility spectrometry used in LC–MS, quantitation issues specific to MS and emerging mass spectrometric approaches complementary to LC–MS are discussed as well.

Highlights

► Comprehensive list of current LC–MS and MALDI-TOF instrumentation. ► Overview of current trends in LC–MS. ► MS approaches complementary to LC–MS.

Electrochemistry coupled to (liquid chromatography/) mass spectrometry—Current state and future perspectives

19 September 2012, 08:44:59
Publication year: 2012
Source:Journal of Chromatography A, Volume 1259
Sandra Jahn, Uwe Karst
The coupling of electrochemistry (EC) to different mass spectrometric (MS) techniques in off-line and especially in on-line approaches is a quickly growing research field in analytical chemistry with numerous distinct objectives. Depending on the analytical problem, a separation step can be further integrated according to the instrumental set-up and, most frequently, liquid chromatography (LC) is selected for this purpose. In this review, various scientific areas of application for this EC/(LC/)MS hybrid method are presented and discussed in detail. Therefore, one major division is made between those applications which are already successfully used on a large scale (current state), and those which have shown promising results for future utilization (future perspectives). The reader shall be provided with a thorough overview on the capabilities of the combination of EC/(LC/)MS and the drawbacks which result in further optimization and exploration of this technique. The major topics addressed in this review include the role of EC/(LC/)MS for drug metabolism studies, peptide, protein and DNA (deoxyribonucleic acid) research and quantification strategies. Promising future applications that are presented and evaluated comprise the fields of toxicology and forensics, targeted product synthesis and environmental analysis.

Highlights

► Electrochemistry/LC/MS is an emerging analytical technique. ► A major application is the simulation of the oxidative metabolism of drugs. ► Protein cleavage and chemical modification of biomacromolecules can be carried out. ► Various technical arrangements are applied.

Liquid chromatography–nuclear magnetic resonance coupling as alternative to liquid chromatography–mass spectrometry hyphenations: Curious option or powerful and complementary routine tool?

19 September 2012, 08:44:59
Publication year: 2012
Source:Journal of Chromatography A, Volume 1259
Sonja Sturm, Christoph Seger
Combining the most powerful separation techniques, i.e. liquid chromatography (LC) or capillary electrophoresis (CE) with a information rich detection system – the mass spectrometer or the nuclear magnetic resonance (NMR) spectrometer – has been pursued for more than three decades. This compilation shall provide an overview of the advantages and limitations of the LC–NMR hyphenation in the light of its most valued application–the unequivocal analyte identification. Especially the post LC trapping of analytes with an in-line solid phase extraction (SPE) device prior to transferring the analyte of interest to the NMR spectrometer (LC–SPE–NMR) proved to be a robust installation allowing a significant cut-down of the amount of analyte needed for the generation of high quality heteronuclear NMR shift correlation data. Different available technical realizations will be discussed and typical application examples from natural product research and from industrial settings will be given.

Highlights

► NMR spectroscopy is the major de novo structure elucidation method in liquid state. ► LC–NMR combines high resolution separation with unequivocal structure elucidation. ► The most advanced technical LC–NMR instrumentation is LC–SPE–NMR. ► Application fields range from pharmaceutical industry to phytochemistry.

Analysis of phospolipids and glycolipids by thin-layer chromatography–matrix-assisted laser desorption and ionization mass spectrometry

19 September 2012, 08:44:59
Publication year: 2012
Source:Journal of Chromatography A, Volume 1259
Beate Fuchs
Thin-layer chromatography–matrix-assisted laser desorption and ionization mass spectrometry (TLC–MALDI-MS) of organic extracts from biological samples allows untargeted analysis and structural characterization of phospholipids and glycolipids ionized from the near-surface region of a sample separated on a TLC-plate. In particular, MALDI-MS enables the sensitive detection of many analytes directly from the solid surface of an ordinary TLC-plate even without previous staining. It will be shown that the detailed fatty acyl composition of phospholipids can be determined solely by TLC–MALDI-MS without previous derivatization, enzymatic cleavage and/or reversed phase separation. MALDI-time-of-flight (TOF) MS is thus a powerful method in this field due to its high sensitivity, low extent of induced fragmentation and simple, user-friendly performance. This review summarizes the so far available knowledge about combined TLC–MALDI-MS for phospholipid and glycolipid characterization together with the technical workflow and a survey of applications. Finally a perspective on the future of TLC–MALDI-MS is given.

Highlights

► Certain lipid species are increasingly considered to be of therapeutic value. ► Separation is an important prerequisite for successful lipid analysis. ► As MALDI-MS makes use of a solid sample combined TLC–MALDI-MS seems straightforward. ► Useful TLC/MALDI-MS matrices and application methods are discussed. ► Phospholipids and glycolipids can be successfully analyzed by TLC/MALDI-MS.

Applications of liquid chromatography–mass spectrometry for food analysis

19 September 2012, 08:44:59
Publication year: 2012
Source:Journal of Chromatography A, Volume 1259
Vita Di Stefano, Giuseppe Avellone, David Bongiorno, Vincenzo Cunsolo, Vera Muccilli, Stefano Sforza, Arnaldo Dossena, László Drahos, Károly Vékey
HPLC–MS applications in the agrifood sector are among the fastest developing fields in science and industry. The present tutorial mini-review briefly describes this analytical methodology: HPLC, UHPLC, nano-HPLC on one hand, mass spectrometry (MS) and tandem mass spectrometry (MS/MS) on the other hand. Analytical results are grouped together based on the type of chemicals analyzed (lipids, carbohydrates, glycoproteins, vitamins, flavonoids, mycotoxins, pesticides, allergens and food additives). Results are also shown for various types of food (ham, cheese, milk, cereals, olive oil and wines). Although it is not an exhaustive list, it illustrates the main current directions of applications. Finally, one of the most important features, the characterization of food quality (including problems of authentication and adulteration) is discussed, together with a future outlook on future directions.

Highlights

► Food analysis using HPLC–MS. ► Analytical methodology of (tandem) mass spectrometry. ► LC–MS analysis of flavonoids, mycotoxins, pesticides and other components in food. ► LC–MS analysis of ham, cheese, milk, cereals, olive oil and wine.

Achievements and future trends in the analysis of emerging organic contaminants in environmental samples by mass spectrometry and bioanalytical techniques

19 September 2012, 08:44:59
Publication year: 2012
Source:Journal of Chromatography A, Volume 1259
Marinella Farré, Lina Kantiani, Mira Petrovic, Sandra Pérez, Damià Barceló
Several groups of organic compounds have emerged as particularly relevant as environmental pollutants. These compounds, including new brominated flame retardants, disinfection by-products, drugs of abuse and their metabolites, hormones and other endocrine disrupting compounds, nanomaterials, perfluoroalkyl substances, pharmaceuticals and siloxanes among others, constitute new risks for environmental and human health. In order to face up to these new risk challenges there is an increasing need to assess their occurrence and behaviour in the environment, as well as, that of their degradation products. Therefore, during recent years an important part of research has been focused on to the improvement of analytical schemes for complex matrices, in which the new tendencies in sample preparation (e.g. online clean up systems), the development of new materials and new mass spectrometry analysers have played an important role. This paper presents a general overview of new analytical trends and potentials in trace analysis of emerging pollutants in the environment, including chromatographic techniques coupled to mass spectrometry, and bio analytical approaches (biosensors).

Highlights

► Overview of new trends for the analysis of emerging pollutants in the environment. ► Online sample pre-treatments are presented and discussed. ► New clean up tendencies are discussed. ► Advanced LC separation and tandem mass spectrometric detection are revised. ► Biosensing technologies are also presented as complementary tools.

Comprehensive impurity profiling of nutritional infusion solutions by multidimensional off-line reversed-phase liquid chromatography×hydrophilic interaction chromatography–ion trap mass-spectrometry and charged aerosol detection with universal calibration

19 September 2012, 08:44:59
Publication year: 2012
Source:Journal of Chromatography A, Volume 1259
Simone Schiesel, Michael Lämmerhofer, Wolfgang Lindner
A new analysis strategy was employed for the establishment of a comprehensive qualitative and quantitative impurity profile of a stressed multi-constituent pharmaceutical drug formulation, namely a nutritional infusion solution composed of amino acids and dipeptides. To deal with the highly complex samples a multidimensional analysis approach was developed which made use of an off-line two-dimensional reversed-phase liquid chromatography (RPLC)×hydrophilic interaction chromatography (HILIC) separation and combination of complementary detection involving ion trap mass spectrometry (IT-MS) and a charged aerosol detector (CAD). The CAD is a mass-sensitive universal detector for non-volatile compounds with relatively consistent detector response. A universal calibration function was set up with a set of standards. This universal calibration function was then employed to quantify unknown impurities allowing their classification into those that need to be reported (>0.05% relative to the precursor compound), identified (>0.1%), and quantified (>0.15%). The dilemma of unavailability of authentic standards at this stage of research for quantification could thereby be circumvented. Relevant impurities above the reporting threshold were identified by IT-MS. Impurities detected comprised di-, tri- and tetrapeptides, cyclic dipeptides (diketopiperazines), pyroglutamic acid derivatives and their condensation products. Cross-validation with HPLC–MS/MS methods using synthesized authentic standards confirmed the results obtained by the presented multidimensional analysis assay.

Highlights

► Comprehensive analysis of complex drug formulation. ► Orthogonal separation methods and complementary detection. ► Universal detection by CAD for preliminary quantitation. ► HPLC hyphenated with ESI-ion-trap-MS for qualitative analysis. ► Rapid classification of impurities according to their relevance.

Quantitative high-performance liquid chromatography–tandem mass spectrometry impurity profiling methods for the analysis of parenteral infusion solutions for amino acid supplementation containing l-alanyl-l-glutamine

19 September 2012, 08:44:59
Publication year: 2012
Source:Journal of Chromatography A, Volume 1259
Simone Schiesel, Michael Lämmerhofer, Alexander Leitner, Wolfgang Lindner
Potential impurities in a parenteral infusion solution for amino acid supplementation containing alanylglutamine (AlaGln) and glycyltyrosine (GlyTyr) as peptide constituents have been determined. Such complex multicomponent pharmaceutical formulations with reactive ingredients may yield a multitude of impurities in stress testing samples. Thus, three stability indicating LC–ESI-MS/MS methods were developed for the establishment of quantitative impurity profiles employing a Chiralpak QN-AX and a Polysulfoethyl A stationary phase in HILIC mode as well as a Gemini C18 stationary phase in gradient RPLC mode. The primary goal was to separate isobaric compounds (stereoisomers, constitutional isomers, retro-peptides) and to provide quantitative data of impurities identified in stressed nutritional infusion solutions. The optimized methods were calibrated by standard addition in the samples and validated according to ICH guidelines. The methods were then applied for the analysis of stressed sample solutions stored under different conditions. Major peptide impurities found in concentrations above the qualification threshold in stressed solutions stored at 40°C for 6 months comprised cyclo(AlaGln) 808μg/mL, pyroGluAla 122μg/mL, AlaGlu 117μg/mL, cycloGlyTyr 60μg/mL, AlaGln epimers (DL+LD) 38μg/mL, and TyrGly 27μg/mL. A number of impurities above the reporting threshold were also detected including AlaAlaGln 18μg/mL, cyclo(AlaGlu) 16μg/mL, AlaGlu(AlaGln) 17μg/mL, and AlaGlu(His) 12μg/mL. The study showed that bioactive peptides may be formed in amino acid infusion solutions by condensation of amino acids and a careful control of these impurities is mandatory.

Highlights

► Separation of stereoisomeric peptides. ► Accurate analysis of constitutional isomers indistinguishable by MRM transitions. ► Detection of peptides formed during processing of amino acid formulation.

Quantitative profiling of polar primary metabolites using hydrophilic interaction ultrahigh performance liquid chromatography–tandem mass spectrometry

19 September 2012, 08:44:59
Publication year: 2012
Source:Journal of Chromatography A, Volume 1259
Helen G. Gika, Georgios A. Theodoridis, Urska Vrhovsek, Fulvio Mattivi
A hydrophilic interaction liquid chromatography (HILIC)-MS/MS profiling method was developed for the efficient separation and quantification of small polar molecules, mostly primary metabolites. The method was based on an ultrahigh performance liquid chromatography (UHPLC) separation system coupled with ESI mass spectrometry on a triple quadrupole mass spectrometer, operating in both positive and negative ionisation mode using rapid polarity switching. With the developed method quantitation of 135 compounds belonging in four major classes of polar compounds (sugars, aminoacids, organic acids and amines) was achieved in a single run of 30min. The method was applied to grape extracts from different varieties and provided information on primary metabolite content. Multivariate statistical analysis was applied using the concentrations found, with the aim of investigating the differences in metabolite profiles. Classification of grapes according to their skin colour was carried out using principle component analysis based on the concentration variation of a number of the metabolites studied.

Highlights

► A new HILIC–MS/MS method for the determination of 124 polar metabolites. ► ESI (positive/negative) ionisation of aminoacids, amines, organic acids, saccharides. ► Utilisation of new sub-3μm stationary phase material (HILIC Amide). ► Provides quantitative results that complement untargeted metabolomics studies. ► Applicability in different fields: biochemistry, food science, clinical chemistry.

Investigation of chronic alcohol consumption in rodents via ultra-high-performance liquid chromatography–mass spectrometry based metabolite profiling

19 September 2012, 08:44:59
Publication year: 2012
Source:Journal of Chromatography A, Volume 1259
Helen G. Gika, Cheng Ji, Georgios A. Theodoridis, Filippos Michopoulos, Neil Kaplowitz, Ian D. Wilson
Alcohol consumption in man, when seen in its extreme form of alcoholism, is a complex and socially disruptive disorder that can result in significant levels of liver injury. Here the rodent “intragastric feeding model” was used together with UHPLC–TOFMS analysis to determine changes in global metabolite profiles for plasma and urine from alcohol treated rats and mice compared to control animals. Multivariate statistical analysis (using principal components analysis, PCA) revealed robust differences between profiles from control and alcohol-treated animals from both species. A large number of metabolites were seen to differ between control and alcohol-treated animals, for both biofluids.

Highlights

► Urine and Plasma from Rodent “intragastric alcohol feeding model” metabolically profiled with UPLC-TOF–MS. ► Scope was to determine changes in the metabolite profiles due to alcohol treatment. ► PCA revealed robust differences between profiles from control and alcohol-treated animals from both species. ► A large number of metabolites were seen to differ between control and alcohol-treated animals, for both biofluids.


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