The development of clinically applicable portable sensors and multiplex protein biomarker assays is one of the most important goals of laboratory medicine today. Sensing strategies based on electrochemical devices are discussed in this overview, with special emphasis on detection principles derived from voltammetry, electrogenerated chemiluminescence, bipolar electrochemistry and impedance-based measurements. Up-to-date examples of electrochemical methods in biomedical research and development are highlighted here, including critical evaluation and future directions of the analysis, development and validation of new protein biomarkers.
- MeSH
- biologické markery analýza MeSH
- biosenzitivní techniky metody MeSH
- elektrochemické techniky metody MeSH
- lidé MeSH
- mikročipová analýza metody MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- časopisecké články MeSH
AIM: To demonstrate and discuss the pros and cons of various conventional and innovative analytical approaches. Methodology & results: Matrix-assisted laser desorption/ionization mass spectrometry imaging (MSI) of tissue sections as well as the extraction of tissue homogenates, blood plasma and dried blood spots coupled with LC-MS were employed to monitor the pharmacokinetics of metformin in mice. The time profile of metformin measured by matrix-assisted laser desorption/ionization MSI correlated well with the results found by LC-MS. Repeatability of the preparation of tissue sections for MSI was very good. CONCLUSION: MSI provided valuable information on the spatial distribution and relative concentration of the analyte within tissue sections. The analysis of the extracts of tissue homogenates, blood plasma and blood spots provided quantitative data on metformin. The dried blood spot approach is a progressive method of sampling, especially in studies where the amount of available blood is limited.
- MeSH
- chromatografie kapalinová metody MeSH
- lidé MeSH
- metformin farmakokinetika MeSH
- myši MeSH
- spektrometrie hmotnostní - ionizace laserem za účasti matrice metody MeSH
- tandemová hmotnostní spektrometrie metody MeSH
- zvířata MeSH
- Check Tag
- lidé MeSH
- myši MeSH
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
AIM: Novel compounds for obesity treatment are currently being studied employing lipidized analogs of anorexigenic neuropeptides. Various analogs of prolactin-releasing peptide have demonstrated their ability to decrease food intake. Adequate analytical tools are required to support corresponding research. Methodology & results: An analytical method was developed that includes simple dilution of plasma samples prior to liquid chromatography-mass spectrometry and employs a monolithic column for the determination of lipidized analogs of prolactin-releasing peptide in complex biological samples. A multiple reaction monitoring approach was applied that included matrix calibration and an internal standard and produced a linear calibration range 20-200 ng ml-1 in rat and macaque plasma samples. CONCLUSION: A straightforward, simple and reliable analytical method was developed satisfying major validation criteria.
- MeSH
- biochemická analýza krve metody MeSH
- chromatografie kapalinová metody MeSH
- hormon uvolňující prolaktin krev chemie MeSH
- kalibrace MeSH
- krysa rodu rattus MeSH
- lipidy chemie MeSH
- metody pro přípravu analytických vzorků * MeSH
- sekvence aminokyselin MeSH
- tandemová hmotnostní spektrometrie metody MeSH
- zvířata MeSH
- Check Tag
- krysa rodu rattus MeSH
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
AIM: Micro-SPE in pipette tips (μ-SPE-PT) with particle sorbent has never been used in small-molecule drug analysis. Methodology & results: μ-SPE-PT was used for the extraction of statins from biological materials followed by UHPLC-MS/MS. The commercial and homemade μ-SPE-PT tips filled with particle sorbent were compared. While the homemade tips enabled direct serum sample loading into the sorbent, protein precipitation (PP) had to be implemented before μ-SPE-PT procedure using commercial tips. Three μ-SPE-PT methods were developed and validated: method A: μ-SPE-PT with homemade tips; method B: PP + μ-SPE-PT with homemade tips; and method C: PP + μ-SPE-PT with commercial tips. Method A enabled a simple high-throughput approach (48 samples in 90 min) compared with methods B and C that required three-times longer time. However, PP increased the recoveries of protein-bound analytes and extracts purity in methods B and C. The matrix effects without internal standards correction for method C were significantly higher than those for the methods A and B. CONCLUSION: Compared with commercial tips, homemade tips filled with particles were found to be more suitable for drug analysis. Commercial tips tested in this study were found challenging but the conditions under which they could be applicable were also defined.
- MeSH
- design vybavení MeSH
- léčivé přípravky krev MeSH
- lidé MeSH
- limita detekce MeSH
- mikroextrakce na pevné fázi přístrojové vybavení metody MeSH
- tandemová hmotnostní spektrometrie metody MeSH
- vysokoúčinná kapalinová chromatografie metody MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- časopisecké články MeSH
- validační studie MeSH
A number of novel lipopeptides have been studied for their possible therapeutic potential. These studies should be supported by the appropriate analytical tools not only for novel potential drugs but also for their metabolites, precursors and side products. Lipopeptides have specific physicochemical properties that make them successful in medical applications. However, there are some difficulties with their qualitative and quantitative analyses in biological samples. Therefore, reliable, sensitive and robust analytical methods are in high demand. The main interest of our review is to describe a selection of specific and important properties of lipopeptides, and the analytical methods currently utilized for their characterization and determination in biological samples. A comparison of the pros and cons of immunomethods versus LC-MS methods is discussed in detail.
- MeSH
- extrakce na pevné fázi MeSH
- ghrelin analýza izolace a purifikace MeSH
- hmotnostní spektrometrie * MeSH
- imunoanalýza * MeSH
- lidé MeSH
- lipopeptidy analýza izolace a purifikace MeSH
- vazba proteinů MeSH
- vysokoúčinná kapalinová chromatografie MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- časopisecké články MeSH
- přehledy MeSH
Jana Zemenová talks to Sankeetha Nadarajah, Commissioning Editor: Jana is a PhD student of analytical chemistry in her final year at the University of Chemistry and Technology, Prague. She also works at the Institute of Organic Chemistry and Biochemistry of Czech Academy of Sciences, in the group led by Lenka Maletínská. She has obtained her MSc in Analysis of Drugs and continues working at University of Chemistry and Technology Prague under the supervision of David Sýkora.
This article reflects our observations of recent accomplishments made using selected ion flow tube MS (SIFT-MS). Only brief descriptions are given of SIFT-MS as an analytical method and of the recent extensions to the underpinning analytical ion chemistry required to realize more robust analyses. The challenge of breath analysis is given special attention because, when achieved, it renders analysis of other air media relatively straightforward. Brief overviews are given of recent SIFT-MS breath analyses by leading research groups, noting the desirability of detection and quantification of single volatile biomarkers rather than reliance on statistical analyses, if breath analysis is to be accepted into clinical practice. A 'strengths, weaknesses, opportunities and threats' analysis of SIFT-MS is made, which should help to increase its utility for trace gas analysis.
- MeSH
- acetonitrily analýza MeSH
- biologické markery analýza MeSH
- dechové testy přístrojové vybavení MeSH
- design vybavení MeSH
- feces chemie MeSH
- hmotnostní spektrometrie přístrojové vybavení MeSH
- idiopatické střevní záněty diagnóza MeSH
- kolorektální nádory diagnóza MeSH
- lidé MeSH
- malondialdehyd analýza MeSH
- těkavé organické sloučeniny analýza MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- časopisecké články MeSH
BACKGROUND: Statins are the microsomal 3-hydroxy-3methylglutaryl-coenzyme A reductase inhibitors used for the treatment of hypercholesterolemia. Some recent studies revealed also the extra-lipid effects and anticancer activities. Due to the wide incidence of cancer diseases, the number of studies dealing with anticancer statin activities has grown in recent years. Development of one universal multistatin method will be a very convenient way of providing practical and economical multiple statin analysis. Results/methodology: Fast and sensitive methods for determination of seven clinically relevant statins, their interconversion products and metabolites (17 analytes in total) in biological samples using microextraction by packed sorbent for sample preparation and UHPLC-MS/MS for subsequent analysis were developed and validated. Three MS platforms with different ion sources, transfer optics, collision cell technologies and scan speed parameters were compared. CONCLUSION: Significant differences among the methods were observed in terms of selectivity and sensitivity. Microextraction by packed sorbent was successful in the extraction of all 17 analytes from biological matrix.
- MeSH
- biochemická analýza krve metody MeSH
- chemická precipitace MeSH
- lidé MeSH
- limita detekce MeSH
- mikroextrakce na pevné fázi metody MeSH
- reprodukovatelnost výsledků MeSH
- statiny krev chemie izolace a purifikace MeSH
- tandemová hmotnostní spektrometrie metody MeSH
- vysokoúčinná kapalinová chromatografie metody MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- přehledy MeSH
AIM: A new HPLC method for the determination of neopterin, kynurenine and tryptophan using a second-generation monolith stationary phase and high-throughput sample preparation procedure based on microplates was developed and fully validated. MATERIALS & METHODS: As the stationary phase a monolithic C18 Chromolith high-resolution column with dimensions of 4.6 × 100 mm connected to a monolithic 4.6 × 10-mm security guard was used. Separation was achieved using 15 mM phosphate buffer (KH2PO4 +K2HPO4·3H2O at pH 3) and acetonitrile in gradient mode. RESULTS: Target analytes were determined in 5.5 minutes in amniotic fluid, effusions and wound exudates with a limit of quantification (LOQ) of 1.25 nM for neopterin, 2.5 µM for tryptophan and 0.25 µM for kynurenine. DISCUSSION: The method was applied to real clinical sample measurements, and it will be used to monitor neopterin, kynurenine and tryptophan levels in biological fluids to assess the patient response to therapy and clinical status.
- MeSH
- exsudáty a transsudáty metabolismus MeSH
- hojení ran * MeSH
- kynurenin analýza MeSH
- lidé MeSH
- maligní pleurální výpotek metabolismus MeSH
- neopterin analýza MeSH
- plodová voda metabolismus MeSH
- spektrofotometrie ultrafialová MeSH
- tryptofan analýza MeSH
- vysokoúčinná kapalinová chromatografie metody MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- MeSH
- chromatografie kapalinová metody MeSH
- hmotnostní spektrometrie metody MeSH
- lidé MeSH
- monitorování léčiv metody MeSH
- superkritická fluidní chromatografie metody MeSH
- Check Tag
- lidé MeSH
- Publikační typ
- úvodníky MeSH
